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Reference handbook
DL50/DL53/DL55/DL58 Titrators
1. Introduction 2. Setup 3. Methods 4. Sample data memory 5. Analysis 6. Auxiliary functions 7. DL58 8. Symbols and explanations 9. Error messages and malfunctions 10. Installation and maintenance 11. Accessories 12. Technical data 13. Index 14. Data sheet 15. ISO certificate, System validation
Introduction
1.
Introduction
In contrast to the Quick Guide, this Reference Handbook provides a complete description of the operating principles of the DL50, DL53, DL55 and DL58 Titrators. Its layout has been kept modular to ensure future supplementation or replacement of individual sections or pages; new texts carry the date of issue in the footer on every page. Safety notes Measures for your personal protection and for operational safety are described in Section 2 of the Quick Guide. We strongly advise you to read these. The symbols listed there also appear for texts in this Reference Handbook which require safety measures. Keywords used appears before all texts which refer to an error in the measured value acquiNOTICE sition, data storage etc. Note appears before all texts which contain additional explanations.
Index The index in Section 13 comprises key words from the Quick Guide and the Reference Handbook. Software version The Reference Handbook applies to software version 2.x for all four titrators. Note: All information concerning automation in this titrator's Reference Handbook relates to the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear in some places. Operation of other METTLER TOLEDO sample changers via your titrator is described in the corresonding Operating Instructions.
The following pages provide an overview of the menus and commands which are available under the menu and auxiliary function keys.
FCC rules
This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is like to cause harmful interference in which case the user will be required to correct the interference at his own expense. 08/2004
METTLER TOLEDO DL50/DL53/DL55/DL58
1-1
Menus: Overview
Setup
Method
Resources Titrants Sensors Temperature sensors Print Titrants NaOH HCl HClO4 Esc 0.1 mol/L 0.1 mol/L 0.1 mol/L Delete
SETUP
Methods Method ID Standard methods User methods METTLER methods Print
METHOD
Modify SETUP Standard methods
OK
METHOD
Add
Modify
OK SETUP
Equivalence point titr'n End point titration (EP) Titer by EQP titration Esc Print Method: Title Sample Stir Esc Title
Modify METHOD
Titrant parameters Name NaOH Concentration [mol/L] 0.1 Titer 1 Esc Modify
OK
Modify
OK METHOD
Titrant names HCl HClO4 AgNO3 EDTA Esc Titrant parameters Name HClO4 Concentration [mol/L] 0.1 Titer 1 Esc Modify
SETUP
OK SETUP
Method ID 00001 Title Equivalence point titr'n Date/time 00-00-0000 00:00 Esc Method: 00001 Title Sample Stir Esc Methods Method ID 00001 Standard methods User methods Delete Print
OK METHOD
OK
Modify
OK METHOD
Modify
1-2
08/2004
Menus: Overview
Sample
Run
No.
Status
Wt/vol.
Meth.
ID
Samples to be analyzed Number of samples Method ID User Add 1 00001
RUN
Start
Add New sample series
SAMPLE
Defined are Stirrer 1: Stand 1 Sensor 1: DM141 Drive 2: 0.1 mol/L AgNO3 Esc Print Sample No. 1 Sample ID Weight [g] 1.23452 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance1)
RUN
Esc Sample entry Number of samples Method ID

User
OK SAMPLE 2 00001 OK
OK RUN
Esc
OK
Sample No. 1 SAMPLE Sample ID Weight [g] 1.19831 Limits [g] 0.02 2.0 Correction factor f Esc Balance1) OK
Current sample
RUN
No. 1 of 1
Sample ID Method ID 00001 OK Stir function Wait time [s] Speed [%] 30 80 Hold2)
mV
Sample No. 2 SAMPLE Sample ID Weight [g] 1.36712 Limits [g] 0.02 2.0 Correction factor f Esc Balance1) OK No. 1 2 Status ready ready Wt/Vol. 1.19831 1.36712 Meth. 00001 00001 ID
RUN
E V curve
mL
Delete
Print
Modify
Add
Table Result list Method: 00001 Sample 1 R1 = 29.26 %
Values
Curve2)
Hold2) RUN
1) 2)
appears only if a balance has been defined appears only with DL55 and DL58
OK
08/2004
1-3
Auxiliary functions: Overview
Sensor
Stirrer
Sensor Measure potential Measure temperature Calibrate temperature sensors
SENSOR
Stirrer Titration stand Speed [%] Stand 1 50 Modify Stirrer Titration stand Speed [%] Stand 1 50
STIRRER
OK Measure potential Sensor Unit of meas. Titration stand Esc Measured values DG111 mV Stand 1 Modify SENSOR
Start STIRRER
Start SENSOR
Stop
43.7 mV
Stop
Changer
Burette
Sample changer Change lift position Rotate turntable Dispense/rinse
CHANGER
Burette Rinse burette Rinse tip Dispense
BURETTE
OK Change lift position Lift position bottom CHANGER Rinse burette Burette drive Drive 2
OK BURETTE
Esc Change lift position Lift position
Modify
Start CHANGER
Esc Rinse burette Burette drive
Modify1)
Start BURETTE
bottom
Drive 2
Stop
1)
Stop appears only with DL55 and DL58
1-4
08/2004
Auxiliary functions: Overview
Results
Results2) Display result list Perform calculations Display measured values
Result list Method: 00001 Sample 1 R1 = 29.26 % Sample 2

2)
The parameters appear only when results of a sample determination are available
Misc.
...
MISC. Data transfer Memory card Computer4) Remote control4)
Miscellaneous Define titrator settings Adjust measuring inputs Shorten analysis sequence
Titrator settings Date/time format Date/time Language Esc Formats Date format Time format Esc 17-OCT-1995 17:04 (24 h) Modify
08/2004
*
RESULTS Report3) Output Printer Results All results
Report
REPORT
OK RESULTS
No Yes Modify
Start REPORT
Report Output unit writing report
OK
3)
The parameters appear only when curves, results or sample data of a sample determination are available
Data Transfer
DATA TRANSFER
OK MISC. Memory card5) Display directory Copy from titrator to card Copy from card to titrator Esc Directory User methods Resources Memory copies Esc
4) 5)
OK DATA TRANSFER
Modify
OK MISC.
OK DATA TRANSFER
OK
Print
OK
appears only if a computer has been defined appears only if memory card is formatted
1-5
Setup
Setup
Contents
Page 2. 2.1 2.1.1 2.1.2 2.1.3 2.2 2.2.1 2.2.2 2.2.3 2.3 2.4 2.4.1 2.4.2 2.5 2.6 2.7 2.7.1 2.7.1.1 2.7.1.2 2.7.2 2.7.3 2.7.4 2.7.5 2.8 2.8.1 2.8.2 2.8.3 Setup .......................................................................................................... Titrants ....................................................................................................... Delete ....................................................................................................... Modify ....................................................................................................... Add ........................................................................................................... 2-3 2-4 2-4 2-4 2-6
Sensors ...................................................................................................... 2-7 Delete ....................................................................................................... 2-7 Modify ....................................................................................................... 2-7 Add ........................................................................................................... 2-10 Temperature sensors ................................................................................ 2-11 Polarized sensors ..................................................................................... 2-13 Modify ....................................................................................................... 2-13 Add ........................................................................................................... 2-14 Auxiliary values ......................................................................................... 2-15 Titration stands ......................................................................................... 2-17 Peripherals ................................................................................................. Printer ....................................................................................................... Centronics interface: Settings for an EPSON printer ............................... RS232 interface: Settings for an EPSON printer ..................................... Balance .................................................................................................... System ..................................................................................................... Sample changer ....................................................................................... External keyboard .................................................................................... Solvents (with sample changer only) ...................................................... Delete ....................................................................................................... Modify ....................................................................................................... Add ........................................................................................................... 2-18 2-18 2-19 2-20 2-21 2-23 2-25 2-26 2-27 2-27 2-27 2-28
08/2004
2-1
Setup
2-2
08/2004
Setup
Setup
2.
Setup
In order to perform titrations, the titrator must be acquainted with the titrants and their concentrations and the sensors with a feasible unit of measurement. It must know the burette drive on which the burette is located and the input to which the sensor is connected. It must also be familiar with the settings of the attached devices such as a balance or printer in order to transfer data. In this menu you define all these chemical and mechanical resources and store them: you set up your titrator. When you press the Setup key, the list of resources appears: Titrants Sensors Temperature sensors Polarized sensors Auxiliary values Titration stands Peripherals Solvents (only with ST20A) The titrants and METTLER TOLEDO sensors in most frequent use are already stored in the titrator. You can not only delete these resources and modify their parameters, but also define new ones. Note: All information concerning automation in this titrator's Reference Handbook relates to the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear in some places. Operation of other METTLER TOLEDO sample changers via your titrator is described in the corresonding Operating Instructions.
NOTICE
All resources needed for the METTLER methods are stored! If you delete one of these, the titrator will wait until the start of a titration of the method before displaying the error message that the resource is not installed.
Print Depending on your choice of resource, its list with the corresponding parameters will be printed out. Modify The list of the selected resources appears.
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2-3
Titrants
Setup
2.1
Titrants
When you select this menu and press <F4>, the stored titrants appear with their concentration data: Titrants NaOH HCl HCl04 Esc 0.1 mol/L 0.1 mol/L 0.1 mol/L Delete SETUP
Add
Modify
OK
2.1.1
Delete
If you press <F2>, "Delete", the titrant NaOH will be deleted from the list. 2.1.2 Modify
If you press <F4>, "Modify", the parameters of the titrants appear and you can change their names and values. Name Concentration [mol/L] Titer Burette volume Burette drive Titer Date/time NaOH 0.1 1.0 10 mL Drive 2 do not check 00-00-0000 00:00
Name
You can change the name by pressing <F4> and selecting a different name from the list of "Titrant names" which appears: Scroll the menu with the key so that the selector bar is positioned on, e.g. "HClO4" and confirm with OK: the name of the titrant is now HClO4. Enter the concentration of the titrant in mol/L. Change the titer only if you know its value. If you determine the titer of the titrant with the titrator, its value will be entered here automatically together with the date (see Titer function, Section 3.3.14).
Concentration Titer
2-4
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Setup
Titrants
Burette volume
Select the volume of the burettes you wish to use with <F4>: 1, 5, 10 or 20 mL. Press <F4> to select: Drive 1. DL50/DL53: These titrators do not have the "Modify" command.
Burette drive
Titer
You can choose whether to enter a date when you should check the titer of the titrant: Press <F4>, select "check on" in the mask which appears and then press <F4> again: Check on Day Month Year Esc 1 1 1997 OK SETUP
If you select "check after" and then press <F4>, the following mask appears: Check after No. of days 10 SETUP
Esc
OK
When the date has lapsed, you will receive an appropriate message during an ongoing titration method which uses this titer. Date/time You can neither enter nor delete the date. It refers to the titer determination of the titrant using the method function Titer and is thus entered here automatically together with the time (see Titer function, Section 3.3.14) As soon as you modify a parameter of the titrant, the date/time entry will be deleted. The expiry date of the titer is an exception: If you modify this, date and time will not be deleted.
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2-5
Titrants
Setup
Storage procedure The titrant with its modified parameters is stored when you confirm both the parameter mask and the list of titrants with OK. If you quit the list with Esc, the following message appears: Save changes? No Yes OK Any change to a parameter is always stored without a message if you press a Menu or Auxiliary function key. 2.1.3 Add SETUP
With this command you add a titrant to the titrants list, e.g. NaOH of concentration 1.0 mol/L or with a different burette volume or a titrant not yet on the list. The following parameters always appear: Name Concentration [mol/L] Titer Burette volume Burette drive Titer Date/time NaOH 0.1 1.0 10 mL Drive 2 do not check 00-00-0000 00:00
You can modify the parameters by the procedure described in Section 2.1.2. If you define, e.g. several NaOH solutions with the same concentration, you must also flag the names so that the titrator can distinguish these, e.g. NaOH/1. If you do not, the following message appears: Resource exists Modify name Overwrite parameters OK Modify: The parameter mask for modification of the name appears. Overwrite: The modified parameters are adopted. SETUP
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Setup
Sensors
2.2
Sensors
When you select this menu and press <F4>, the stored METTLER TOLEDO sensors with their measurement unit appear: Sensors DG111 DG101 DG113 Esc pH pH mV Delete SETUP
Add
Modify
OK
You can attach the listed sensors only to a pH option (see Sections 2.4 and 10.4). 2.2.1 Delete
If you press <F2>, "Delete", the sensor DG111 will be deleted from the list.
2.2.2
Modify
If you press <F4>, "Modify", the parameters of the sensors whose names and values you can change appear. Name Unit of meas. Sensor input Zero point [unit] Slope [mV/unit] Temperature [C] Date/time DG111 pH Sensor 1 7.0 59.16 25.0 00000000
00:00
Name
You can change the name by pressing <F4> and selecting a different name from the list of "Sensor names" that appears. Note: You do not need to define a reference electrode as it is part of the sensing electrode at the corresponding sensor option (see Section 10.4).
Unit of measurement
You select possible measurement units for the sensor from the selection menu.
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2-7
Sensors
Setup
Unit of measurement
mV:
Either there is no other suitable measurement unit with calibration parameters for the sensor or you need only mV. If you select the unit mV for a sensor, the calibration parameters zero point, slope and temperature are ignored by the titrator. If you select pH, next enter the calibration parameters for a pH electrode or have them entered by the titrator (see page 2-9: Notes 1 and 2). M represents any cation. If you select pM, next enter the calibration parameters for a pM electrode or have them entered by the titrator (see page 2-9: Notes 1 and 2). X represents any anion. If you select pX, next enter the calibration parameters for a pX electrode or have them entered by the titrator (see page 2-9; Notes 1 and 2). If you select %T, next enter the calibration parameters for a phototrode (measurement unit: transmission, see "Phototrode" Operating Instructions. If you select A, next enter the calibration parameters for a phototrode (measurement unit: transmission). The extinction [A = -log T] is calculated from this (see Section 8.4.1: Results).
pH:
pM:
pX:
%T:
A:
S/cm: If you select S/cm, next enter the calibration parameters of the conductivity cell. mS/cm: If you select mS/cm, next enter the calibration parameters for the conductivity cell. You can perform conductivity measurements and conductivity titrations with a conductometer fitted with an analog output. Sensor input Press <F4> to select: Sensor 1, 2, 3 or 4. The numbers refer to the slot of a pH option (see Section 10.4).
2-8
08/2004
Setup
Sensors
Zero point
The zero point is the measured value at which the sensor indicates 0 mV voltage (measuring chain zero point). For the zero point of a pH electrode this is pH0 with the unit pH. For the zero point of an ion selective electrode this is pM0 with the unit pM, or pX0 with the unit pX. The zero point of the phototrode is normally 0%T (100% T = 1000 mV). The zero point of a conductivity cell is normally 0 S/cm or 0 mS/cm. The slope of the sensor is the voltage change in mV per measurement unit. For the slope of a pH electrode this is the unit: mV/pH. For the slope of an ion selective electrode this is the unit: mV/pM or mV/pX. The slope of a phototrode is normally 10 mV/%T. For the slope of a conductivity cell this is the unit: mV/S*cm-1 or mV/mS*cm-1. Change the temperature if necessary: The current calibration temperature is either entered by you at the start of a calibration method (see Section 5.1) or measured automatically if you have attached and defined a temperature sensor (see Section 3.3.2). You can neither enter the date nor delete it. It refers to the calibration of the sensor using the method function Calibration and is entered here automatically together with the time (see Calibration function, Section 3.3.13).
Slope
Temperature
Date/time
Notes 1. When the titrator is delivered, the defined calibration data are theoretical values of a new sensor. You must perform a calibration of your sensor if you wish to determine accurate values (see Calibration function, Section 3.3.13). 2. With a calibration of pH, pM or pX sensors, the calibration data (zero point, slope, temperature) are entered here automatically together with the date. 3. As soon as you change a sensor parameter, the date/time entry is deleted.
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2-9
Sensors
Setup
NOTICE
You should never transfer the calibration data of glass electrodes which you obtain at sensor input 1 if you attach the electrode to, e.g. sensor input 2. To obtain correct values, recalibrate the electrode!
Storage procedure The sensor with the modified parameters is stored when you confirm both the parameter list and the list of the sensors with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see corresponding section at the end of Section 2.1.2).
2.2.3
Add
With this command you add a sensor to the sensor list, e.g. a DG111 sensor with different calibration parameters or a completely new sensor. The following parameters always appear: Name Unit of meas. Sensor input Zero point [unit] Slope [mV/unit] Temperature [C] Date/time DG mV Sensor 1 7.0 59.16 25.0 00000000
00:00
You change the parameters by the procedure described in Section 2.2.2. If you define, e.g. several DG111 sensors, you must also flag the name to ensure the titrator can distinguish these, e.g. DG111/2. If you do not, a message appears (see Section 2.1.3).
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08/2004
Setup
Temperature sensors
2.3
Temperature sensors
When you select this menu and press <F4>, the stored temperature sensors appear with the sensor type: Temperature sensors TEMP A Pt100 TEMP B Pt100 TEMP C Pt1000 Esc SETUP
Modify
OK
You can attach temperature sensors only to a pH option (see Section 10.4). You can neither delete a temperature sensor from the list nor add a new one to it. However, you can define, e.g. several Pt100s or Pt1000s at the same sensor input. Select, e.g. TEMP A, press <F4> and the following parameters appear: Name Sensor type Sensor input Zero point [C] Date/time TEMP A Pt100 Temp 1 0.0 00000000
00:00
Name Sensor type Sensor input
You can not change the sensor name. Press <F4> to select: Pt100 or Pt1000 (see Section 9.5). Press <F4> to select: Temp 1, 2, 3 or 4: The numbers refer to the slot of a pH option (see Section 10.4). The zero point of a Pt sensor is the difference between the measured value and a reference value, e.g. 0 C of an ice bath. You can neither enter nor delete the date. It refers to the calibration of the Pt sensor and is entered here automatically together with the time (see Section 6.1.3).
Zero point
Date/time
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2-11
Temperature sensors
Setup
Notes 1. The defined zero point is the theoretical value of a new Pt sensor. You must perform a calibration of your sensor if you wish to determine the exact value. With a calibration the zero point is entered here automatically with the date (see Section 6.1.3: Calibrate temperature sensors). 2. As soon as you modify a parameter of the temperature sensor, the date/time entry is deleted.
NOTICE
You should not transfer the zero point of temperature sensors which you obtain at input Temp 1 if you attach the sensors to, e.g. input Temp 2! To obtain correct values, recalibrate the sensor!
Storage procedure The Pt sensor with the modified parameters is stored when you confirm both the parameter mask and the list of the Pt sensors with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of Section 2.1.2).
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Setup
Polarized sensors
2.4
Polarized sensors
When you select this menu and press <F4>, "DM142" appears as the only polarized METTLER TOLEDO electrode stored in the titrator: Polarized sensors DM142 SETUP
Esc
Add
Modify
OK
You can attach this sensor only to a KF option (see Section 10.4). Note: If you have added polarized sensors to the list, the Delete command appears (<F2>).
2.4.1
Modify
If you press <F4>, "Modify", the name and sensor input of the DM142 appear: Sensor parameters Name Sensor input Esc Name DM142 Sensor 2 Modify OK SETUP
You can change the name by pressing <F4> and selecting a different name from the list of "Sensor names" that appears. Press <F4> to select: Sensor 1, 2, 3 or 4. The numbers refer to the slot of a KF option (see Section 10.4).
Sensor input
Storage procedure The sensor with the modified parameters is stored when you confirm both the parameter list and the list of the sensors with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of Section 2.1.2).
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Polarized sensors
Setup
2.4.2
Add
With this command you add a polarized sensor to the sensor list. The following parameters always appear: Sensor parameters Name Sensor input Esc DM Sensor 2 Modify OK SETUP
You change the parameters by the procedure described in Section 2.4.1. If you define, e.g. several DM142 sensors, you must also flag the name to ensure the titrator can distinguish these, e.g. DM142/2. If you do not, a message appears (see Section 2.1.3).
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Setup
Auxiliary values
2.5
Auxiliary values
When you select this menu and press <F4>, the 20 memory locations for auxiliary values appear: H1 - H20. You can use the Auxiliary value function to assign the results of a method, such as blank values, potentials or volume or amount of substance consumption to this memory. These values are then entered here automatically together with the date (see Section 3.3.15). You yourself can also enter numeric values as an auxiliary value here and call them up under the Calculation function. Auxiliary values H1 H2 H3 Esc 1.0 1.0 1.0 Modify OK SETUP
No auxiliary values are defined in the titrator on delivery. You can neither delete the memory locations nor add new ones. If you select, e.g. H1 and press <F4>, the following appears: Auxiliary value parameters Auxiliary value H1 ID Value 1.0 Date/time 00-00-0000 00:00 Esc Auxiliary value ID Value Date/time You can not change H1. Enter an identification if desired. Enter the value. You can neither enter nor delete the date. It refers to the determination of the auxiliary value using the method function Auxiliary value and is entered here automatically together with the time (see Section 3.3.15). SETUP
OK
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2-15
Auxiliary values
Setup
Notes 1. You can delete the data of an auxiliary value only by overwriting them yourself or have the titrator overwrite them using the Auxiliary value function. 2. The titrator does not tell you if you overwrite an auxiliary value. If you make frequent use of the auxiliary value memory, you should thus print out a list of its values from time to time (see page 2-3). 3. If you modify a parameter of the auxiliary value, the date/time entry is deleted.
Storage procedure The auxiliary value with the modified parameters is stored when you confirm both the parameter mask and the list of auxiliary values with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see appropriate paragraph at the end of Section 2.1.2).
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Setup
Titration stands
2.6
Titration stands
When you select this menu and press <F4>, the names of the five possible titration stands appear: Titration stands Stand 1 Stand 2 ST20A Esc Stand 1 Stand 2 ST20A Auto stand SETUP
Modify
OK
is the titration stand you receive with the basic version of the titrator. is the second titration stand of a dual titration stand. is the sample changer titration stand. is the name of the titration stand on which you can run a sample series without being prompted to insert the next sample (see Section 5.1). With this stand you can use, e.g. a robot to change the samples.
External stand is a titration stand you have set up in addition to the above-mentioned titration stands if you, e.g. attach a stirrer to a rod stand. You can neither delete a titration stand from the the list nor add a new one. If you select, e.g. Stand 1 and press <F4>, the following appears: Titration stand parameters Name Stand 1 Stirrer output Stirrer 1 SETUP
Esc
Modify
OK
Name Stirrer output
You can not change the name of the titration stand. Press <F4> to select the output for the stirrer: Stirrer 1, 2, 3, 4 or "Not at DL". 1, 2, 3, 4 refer to the position of the sensor option (see Section 10.4). Select "Not at DL" if you use a stirrer which is not attached to the titrator: The wait time specified under the Stir function is allowed to elapse within the method, but you yourself are responsible for arranging stirring (see Stir function, Section 3.3.3).
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Peripherals
Setup
2.7
Peripherals
When you select this menu and press <F4>, the names of the devices which you can attach to the titrator via the RS232C interfaces, the Centronics interface or the DIN socket appear. These devices are not defined by software in the factory. Printer Balance System Sample changer External keyboard Not Not Not Not Not defined defined defined defined defined
2.7.1
Printer
To define and set your printer, select Printer and press <F4>: Printer Status Printer type Esc Status Printer type Press <F4> to select "Defined". Select the type from the selection menu: Not defined EPSON ESC/P Modify OK SETUP
EPSON ESC/P HP PCL Level 3 IBM Proprinter ASCII GA42 You can change the settings for the selected printer in the parameter mask, which appears when you press <F4>. Note: On delivery of the titrator, the Centronics option is installed in slot 4 which has a parallel interface for the printer connection (see Section 10.4). An RS option with a serial printer interface has to be installed in slot 4 in order to use the METTLER TOLEDO Printer GA42.
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Setup
Peripherals
2.7.1.1
Centronics interface: Settings for an EPSON printer
Examples of default settings for an EPSON printer: Type Paper Paper format Automatic form feed Frame lines LX/SX Fanfold 81/2 * 11" No Straight
Type Paper
Press <F4> to select : "LX/SX" or "LQ/Stylus". Press <F4> to select : "Fanfold" or "Single sheet". Single sheet: - A form feed is effected at the end of a page. - If you select Yes for "Automatic form feed", a footer and a header will be printed out on every page.
NOTICE
You must not trigger a line or form feed at the printer if you have selected "Automatic form feed" for "Single sheet"! You can do this on the titrator with the following key combinations: <Shift + F1> triggers a line feed, <Shift + F2> triggers a form feed.
Paper format
Press <F4> to select: DIN A4 (width = 21 cm, length = 29.7 cm) 81/2 * 11" (width = 81/2 inches, length = 11 inches) 81/2 * 12" (width = 81/2 inches, length = 12 inches) Press <F4> to select: "Yes" or "No". Yes: The printer initiates a form feed after every document. No: The individual documents are separated by a distance of 2 lines. Press <F4> to select the frame for the report: Straight: The report is framed with straight lines. Dotted: The report is framed with dotted lines; this speeds up the printout by a factor of 2. None (no frame): Printing is fastest with this parameter. HP printers: Selection of the lines does not influence the speed.
Form feed
Frame lines
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Peripherals
Setup
2.7.1.2
RS232 interface: Settings for an EPSON printer
You can also attach printers to a serial interface if you have installed an RS option in slot 4 (see Section 10.4). You can use this interface to attach a GA42 Printer. While no software settings are necessary for the GA42 Printer, you must set its DIP switch 2 to the ON position (see GA42 Operating Instructions). Example of the default settings for an EPSON printer: Type Paper Paper format Automatic form feed Frame lines Baudrate Parity Number of data bits Number of stop bits LX/SX Fanfold 81/2 * 11" No Straight 2400 Even 8 Bits 1 Bit
The settings for the first 5 parameters are the same as those for the Centronics interface (see Section 2.7.1.1). Baud rate Parity Data bits Stop bits Press <F4> to select: 1200, 2400, 4800 or 9600. Press <F4> to select: "Even", "Odd" or "None". Press <F4> to select: 7 or 8 bits. Press <F4> to select: 1 or 2 bit(s).
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Setup
Peripherals
2.7.2
Balance
To define and set your balance, select Balance and press <F4>: Balance Status Transmn mode Esc Status Transmission mode Press <F4> to select "Defined". Press <F4> to select: "Unidirectional" or "Bidirectional". Not defined Unidirectional Modify OK SETUP
Unidirectional On inquiry of the weight, the balance continuously transfers the current weight value (without a stability check), which is displayed by the titrator. You must confirm this display with <F5> for the value to be accepted.
Data to titrator Titrator Balance Configuration: "Send Cont."
Bidirectional On inquiry of the weight, the balance transfers the current weight value when requested by the titrator, which then displays it (with stability check). Many METTLER TOLEDO balances show the weight limits in the balance display (see Section 4.2). The titrator accepts the stable weight value when you press either <F5> on the titrator or the transfer key of the balance.
Command from titrator Titrator Data to titrator Balance Configuration: "Send Stable" ("Send on Transfer")
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Peripherals
Setup
Notes 1. On delivery of the titrator, the Centronics option is installed which has a 9-pin RS232 interface for the attachment of a balance (see Section 10.4). If you install an RS option in slot 4, its balance interface is 8-pin. Depending on the installation, you must then have the right connection cable (see Section 11.2: Peripherals). RS232 9-pin: METTLER TOLEDO balances with RS interface: Order No. 59759, 229029 METTLER TOLEDO balances with LC interface: Order No. 229065 SARTORIUS balances with RS interface: Order No. 51190363 METTLER TOLEDO balances with RS interface: Order No. 51107195, 51107196 METTLER TOLEDO balances with LC interface: Order No. 229185 SARTORIUS balances with RS interface: Order No. 200495
RS232 8-pin:
2. The data output of the METTLER TOLEDO balance you wish to attach must be set as follows: Baud rate: 2400 Parity: even Mode: "Send Cont." for transmission mode Unidirectional "Send Stable" ("Send on Transfer") for transmission mode Bidirectional. 3. The following settings are important with AT balances: Unit: Prt on Print/Transfer command on g Weighing unit in g Int-FACE: SENd S.Stb Data transmission mode: Standby bd 2400 Baud rate: 2400 PAr -EParity: even HS OFF Handshake (XON/XOFF) off 4. With AG, PG, AB, PB and PR balances, the LC-RS8 cable must be set as follows: For bidirectional transfer For unidirectional transfer Left switch: Position 0 Left switch: Position 7 Middle switch: Position 3 Middle switch: Position 3 Right switch: Position 4 Right switch: Position 4 5. In case of SARTORIUS balances you must select Bidirectional as the transmission mode. The data output of the balance you wish to attach must be set as follows: Data output: Ext. print command/without stability Baud rate: 2400 Parity: even Stop bit: 1 Weight unit: g
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08/2004
Setup
Peripherals
2.7.3
System
To define and set your computer or terminal, select System and press <F4>: System Status Instrument type Esc Status Instrument type Press <F4> to select "Defined". Press <F4> to select from the selection menu: Not defined Computer Modify OK SETUP
Instrument type Computer Color terminal Monochrome term. Esc
SETUP
Modify
You can modify the settings for the Computer in the parameter mask, which appears when you press <F4>: Baud rate Parity Number data bits Number stop bits Bar code to computer Character set Send mode Communication protocol Start/end character 4800 Even 8 bits 1 bit No ASCII Spontaneous Normal '{'/ CR
Baud rate Parity
Press <F4> to select: 1200, 2400, 4800 or 9600. Press <F4> to select: "Even", "Odd" or "None".
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Peripherals
Setup
Data bits Stop bits Bar code
Press <F4> to select: 7 or 8 bits. Press <F4> to select: 1 or 2 bit(s). Press <F4> to select: "Yes" or "No". Yes: If you have attached a bar-code reader to the external keyboard, the read-in bar code will be sent directly to the computer. Depending on the program you have loaded, this bar code can be used to trigger commands from the computer. (See Section 6.8.4: Bar-code string and Section 10.8.1: Attaching a bar-code reader.) Press <F4> to select: "ASCII" or "DL" . ASCII: The standard character set (HEX 20 to HEX 7E) for the output of text to the computer is used. DL: The character set used in the titrator is used. Notice: If you select DL, you must specify 8 for the number of data bits! Press <F4> to select: "Spontaneous" or "On request". Spontaneous: The titrator sends the computer orders and data, as well as what has been generated (assuming that the computer is ready). On request: The titrator waits for the corresponding inquiry from the computer before it sends an order or data. Press <F4> to select: "Normal" or "Reduced". Normal: The data received by the titrator or computer are checked and any errors given with messages (safety mechanism active). Reduced: The received data are neither checked nor acknowledged so that no error messages are given (safety mechanism passive). Press <F4> to select: " '{' / CR " or " STX / ETX ". These start and end characters for the messages to be sent depend on the input possibility of your computer.
Character set
Send mode
Communication protocol
Start/end character
The computer needs an RS232C interface (DTE). The parameters baud rate, parity, number of data bits and number of stop bits are freely selectable. Connection cables are listed in Section 11.2. You will find additional information on the communication between titrator and computer in Section 6.8.2 and in the Operating Instructions for the computer interface (see Section 11.2).
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08/2004
Setup
Peripherals
You can change the settings for the selected Terminal in the parameter mask which appears when you press <F4>: Baud rate Parity Number data bits Number stop bits Baud rate Parity Data bits Stop bits 9600 Even 8 bits 1 bit
Press <F4> to select: 1200, 2400, 4800 or 9600. Press <F4> to select: "Even", "Odd" or "None". Press <F4> to select: 7 or 8 bits. Press <F4> to select: 1 or 2 bit(s).
You can use a terminal of the type DEC VT340 or DEC VT241 as a color terminal and either a DEC VT330 or DEC VT240 type as a monochrome terminal. The connection cable is listed in Section 11.2. You will find additional information on the configuration of the terminals and their operation in Section 10.9.
2.7.4
Sample changer
Note: All information concerning automation in this titrator's Reference Handbook relates to the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear in some places. To define the sample changer, select Sample changer and press <F4>: Sample changer Status Not defined SETUP
Esc Status Press <F4> to select "Defined".
Modify
OK
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Peripherals
Setup
2.7.5
External keyboard
You can attach a PC keyboard which has a DIN socket using a DIN cable (see Section 10.8: Attaching a keyboard). To define the keyboard, select External keyboard and press <F4>: External keyboard Status Layout Esc Not defined US International Modify OK SETUP
Status Layout
Press <F4> to select "Defined". Press <F4> to select: "US International", "Swiss (German)", "French", "German" or "Polish".
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Setup
Solvents
2.8
Solvents (with sample changer only)
The parameters of this resource are needed only if you have defined and attached a sample changer. You can connect time-controlled pumps, electromagnetic valves or dispensers to the sample changer to dispense solvents. When you select this menu and press <F4>, the stored solvents appear: Solvents (only with ST20A) H2O CH3OH CHCl3 Esc SETUP
Delete
Add
Modify
OK
2.8.1
Delete
If you press <F2>, "Delete", H2O will be deleted from the list. 2.8.2 Modify
If you press <F4>, "Modify", the following appears: Solvent parameters Name H2O Pump rate [mL/min] 200.0 ST20A output RINSE Esc Name SETUP
Modify
OK
You can modify the name by pressing <F4> and choosing a different name from the list of "Solvent names" that appears. The titrator uses the pump rate to calculate the volume to be dispensed for time-controlled pumps or electromagnetic valves. You must determine the pump rate of each metering device beforehand for every solvent: Add the solvent using the metering device to a measuring cylinder for 1 minute (stopwatch) and note the volume. Repeat this procedure for, e.g. 20, 30 and 40 seconds. Calculate the mean value per minute for the different volumes and enter this value.
Pump rate
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Solvents
Setup
Output
Press <F4> to select the ST20A output to which you will attach the metering device: "DOSE", "RINSE" or "DISPENSER".
Storage procedure The solvent with the modified parameters is stored when you confirm both the parameter mask and the list of solvents with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see appropriate paragraph at the end of Section 2.1.2).
2.8.3
Add
You can use this command to add a solvent to the list of solvents. The following mask always appears: Solvent parameters Name H2O Pump rate [mL/min] 200.0 ST20A output RINSE Esc SETUP
Modify
OK
You can modify the parameters by the procedure described in Section 2.8.2. If you define, e.g. several solvents with the same name, you must also flag these to ensure the titrator can distinguish them, e.g. H2O/2. If you do not, a message appears (see Section 2.1.3).
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Method
Method
Contents
Page 3. 3.1 3.1.1 3.1.2 3.1.3 3.1.4 3.2 3.2.1 3.3 3.3.1 3.3.2 3.3.3 3.3.4 3.3.5 3.3.6 3.3.6.1 3.3.6.2 3.3.6.3 3.3.6.4 3.3.6.5 3.3.6.6 3.3.6.7 3.3.7 3.3.7.1 3.3.7.2 3.3.7.3 3.3.7.4 3.3.7.5 3.3.7.6 3.3.8 Methods ..................................................................................................... Selecting methods .................................................................................... Method ID .................................................................................................... Standard methods ....................................................................................... User methods .............................................................................................. METTLER methods ..................................................................................... Modifying a method .................................................................................. Storage procedure ...................................................................................... 3-3 3-4 3-4 3-5 3-6 3-6 3-7 3-7
Functions ................................................................................................... 3-10 Title.............................................................................................................. 3-11 Sample ........................................................................................................ 3-12 Stir ............................................................................................................... 3-16 Measure ...................................................................................................... 3-17 Dispense ..................................................................................................... 3-19 EQP titration (equivalence point titration) .................................................... Titrant/Sensor .............................................................................................. Predispensing ............................................................................................. Titrant addition............................................................................................. Measure mode ............................................................................................ Recognition ................................................................................................. Termination .................................................................................................. Evaluation ................................................................................................... EP titration (end point titration) .................................................................... Titrant/Sensor .............................................................................................. Predispensing ............................................................................................. Titrant addition............................................................................................. End point ..................................................................................................... Tendency ..................................................................................................... Termination .................................................................................................. 3-20 3-20 3-21 3-22 3-25 3-28 3-33 3-34 3-37 3-37 3-38 3-39 3-41 3-42 3-42
Learn titration .............................................................................................. 3-43
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Method
Method
Page 3.3.9 3.3.9.1 3.3.9.2 3.3.9.3 3.3.9.4 3.3.9.5 3.3.9.6 3.3.9.7 3.3.9.8 3.3.10 3.3.10.1 3.3.10.2 3.3.10.3 3.3.10.4 3.3.10.5 3.3.10.6 3.3.10.7 3.3.11 3.3.12 3.3.13 3.3.14 3.3.15 3.3.16 EQP titration (Ipol/Upol) .............................................................................. Titrant/Sensor .............................................................................................. Indication ..................................................................................................... Predispensing ............................................................................................. Titrant addition............................................................................................. Measure mode ............................................................................................ Recognition ................................................................................................. Termination .................................................................................................. Evaluation ................................................................................................... EP titration (Ipol/Upol) ................................................................................. Titrant/Sensor .............................................................................................. Indication ..................................................................................................... Predispensing ............................................................................................. Titrant addition............................................................................................. End point ..................................................................................................... Tendency ..................................................................................................... Termination .................................................................................................. 3-45 3-45 3-46 3-48 3-48 3-49 3-50 3-52 3-53 3-56 3-56 3-57 3-59 3-60 3-60 3-61 3-61
pH/mV-stat .................................................................................................. 3-62 Calculation .................................................................................................. 3-66 Calibration ................................................................................................... 3-69 Titer ............................................................................................................. 3-72 Auxiliary value ............................................................................................. 3-73 Report ......................................................................................................... 3-74
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Method
Method
3.
Methods
The titrator performs analyses automatically with the aid of predefined methods. When the titrator is delivered, the Method menu already holds standard methods and methods developed by METTLER. You can modify these methods to suit your requirements and save them as User methods. A complete titration method comprises sample preparation, dispensing of auxiliary solutions, stirring and wait times, the actual titration, result calculation and a report. These sub-steps are defined as Functions in the titrator and they are executed in succession in an analysis. The individual functions comprise Parameters, whose values or names you can modify. You modify a method by changing the parameters of the preset functions.
Method
Functions
Parameters
modify
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Selecting methods
Method
3.1
Selecting methods
When you press the Method key, the following appears in the display: Method ID Standard methods User methods METTLER methods _____
Under Method ID you can call up a method stored with an identification number; these are the user and METTLER methods. Standard methods are methods we have entered in the factory without a method identification. User methods are the methods you have defined and saved (they are stored in the user data memory). METTLER methods are applications we have developed and stored for you. Print Method ID: The recalled method is printed out with its functions and parameters. Method groups: The list of methods of the selected group is printed out.
3.1.1
Method ID
The method identification is the 5-place, numeric identifier of a method (see Title function, Section 3.3.1). If you are familiar with the identification, enter it and press <F4>: The list of the functions of this method appears (see Section 3.2). Methods Method ID Standard methods User methods Delete 00001
METHOD
Print
Modify
Note: With user methods, you can enter an asterisk (*) after the first, second or third digit of the method ID: This replaces the remaining digits, e.g. 1*: All methods whose ID starts with 1 appear in the display. When you confirm the desired ID with OK, the function list of the selected method appears immediately.
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Method
Selecting methods
Delete When you press <F2>, the selection menu "Delete method?" appears in which you can confirm or cancel the command: Yes: The method will be deleted. No: The method remains stored. If you wish to delete a METTLER method or a user method that is stored in the sample data memory, an error message appears. You can not delete these methods (see Section 3.1.4 and 4.1).
3.1.2
Standard methods
If you select this group, the list of 21 methods entered in the factory appears with titles (see Section 5.2 of the Quick Guide). The standard methods are used as basic methods for the development of your own methods and can not be called up to perform an analysis as they have no method identification. As soon as you allocate an identification to a standard method, it is automatically stored as a user method with a method ID when saved and can be called up by you for the analysis. The parameters of the other functions are defined with default values or names for all methods; you can accept or modify these (see Sections 3.2 and 3.3).
Print The selected method with its functions and parameters is printed.
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Selecting methods
Method
3.1.3
User methods
If you select this group, a list of methods with the identification (and the name) first appears if you have stored modified standard or METTLER methods, e.g.: User methods 61 11152 00001 Esc METHOD
Delete
Print
Modify
Delete When you press <F2>, the selection menu "Delete method?" appears in which you can confirm or cancel the command: Yes: The method will be deleted. No: The method remains stored. Note: The "Delete" command is not available when the method is stored in the sample data memory (see Section 4.1). Print The selected method with its functions and parameters is printed.
3.1.4
METTLER methods
If you select this group, a list of applications developed by us with the identification and the name of the method appears: METTLER methods 90001 90002 90003 Esc Acid content Calibration pH electrode Calibration F- electrode Print Modify METHOD
You can modify METTLER methods to suit your requirements, but you must then give them a new method identification under the Title function in order to save them (see Section 3.3.1). Print The selected method with its functions and parameters is printed.
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Method
Modifying a method
3.2
Modifying a method
You have selected, e.g. the "Equivalence point titration" under standard methods and then press <F4>: The list of the functions of this method appears. Title Sample Stir EQP titration Calculation Calculation Calculation Report You can modify the parameters of all functions: Select the function and press <F4>: The mask with the Parameters defined for the function appears and you can then change their values and names (see Section 3.3).
3.2.1
Storage procedure
1. Every modified method is stored when you confirm the corresponding parameter masks of the individual functions and the list of the functions with OK. If you switch off the titrator before doing this, your changes will be discarded: all parameters are first written to the RAM (volatile memory) of the titrator and are not stored until the function list has been confirmed. After modification of the parameters of a function, you can save the method. The following sequence is an example of the standard method "Equivalence point titration": Method: Title Sample Stir Esc METHOD
Modify
OK
You modify the Title function by entering, e.g. the method identification 00001 and confirming it with OK (see also Section 3.3.1):
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Modifying a method
Method
Method: 00001 Title Sample Stir Esc
METHOD
Modify
OK
If you now press <F5>, the mask of the method groups reappears: the method is stored. Methods Method ID Standard methods User methods Delete 00001
METHOD
Print
Modify
As method 00001 is selected automatically, the list of the functions reappears immediately when <F4> is pressed to allow modification of other functions.
2. If you quit the list of the functions with Esc after you have modified parameters of functions, the following appears: Save method? No Yes OK No: Changes are not stored. Yes: The titrator stores all modified parameter values. The same message appears if you press a Menu or Auxiliary function key. METHOD
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Method
Modifying a method
3. Several functions such as "EQP titration" have a list of parameters which have subparameters. If you quit their mask with Esc after modifications, the following appears: Save changes? No Yes OK No: Changes are not stored. Yes: The titrator stores the modified parameter values. METHOD
4. On storage, the titrator checks the method and, if it has found several errors, draws your attention to the first of them. a. When you have confirmed the error message, the list of method functions appears with the selection bar on the first faulty function. After you have corrected its parameters and saved the method again, the next faulty function appears etc. b. If you have entered an existing method identification under the Title function, the following appears: Method ID exists Modify ID Overwrite method OK Modify ID The list of method functions appears; under the Title function you can modify the method ID and then save the method. Overwrite method The new or modified method is stored, that with the same identification deleted. METHOD
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Functions
Method
3.3
Functions
You select all functions whose parameters you wish to modify by the procedure described in Sections 3.1 and 3.2. The following explanations of all functions of the standard and METTLER methods as well as their parameters thus pertain to the Modify command. The order of the following sections corresponds to the below list of functions.
Title Sample Stir Measure Dispense EQP titration EP titration Learn titration EQP titration (Ipol/Upol) EP titration (Ipol/Upol) pH/mV-stat Calculation Calibration Titer Auxiliary value Report
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Method
Title
3.3.1
Title
This function is used for recognition of the titration method. You must enter its method ID parameter. You use this identification to call up the stored methods. The function has no meaning in the sequence of the method. The following example shows the title mask of the standard method "Equivalence point titration" (see Sections 3.2. and 3.2.1). Title _ _ _ _ _ Method ID Title Equivalence point titr'n Date/time 00-00-0000 00:00 Esc Method ID METHOD
OK
Enter a number with max. 5 characters (letters also admissible). You can not enter identifications in the range 90000 to 99999: they are reserved for METTLER methods. Asterisks (*) are not allowed for the method ID! Enter a title for the method. Date and time are entered here automatically when you save a modified method. You can neither delete not overwrite this information.
Title Date/time
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3-11
Sample
Method
3.3.2
Sample
Here you define the parameters needed for the entry of the sample data such as weight or volume, the titration stand on which the sample should be titrated and whether the temperature of the sample solution should be measured. Sample ID Entry type Molar mass M Equivalent number z Titration stand Temperature sensor
Weight 100 1 Stand 1 Manual
Note: If samples which are determined with this method are stored in the sample data memory as "ready", you can not modify the sample ID and the entry type (see Section 4.1). During a sample series, you can modify only the numeric parameter values for the ST20A titration stand (see following page and Section 5.2.3). Sample ID Enter the identification of the sample if required. This is adopted for all samples of a sample series. You can also enter and modify the ID in the Sample menu (see Section 4.1). Select from the selection menu: "Weight", "Volume" or "Fixed volume". Weight: Press <F4> to show the mask in which you can define the range which the sample weight should not violate: Lower limit [g] Upper limit [g] Volume: Press <F4> to show the mask in which you can define the range which the added volume should not violate: Lower limit [mL] Upper limit [mL] You do not enter the actual weight or volume until the sample preparation or when the titrator requests this information after the start of the method (see Section 5.1). If you violate the defined range, you receive an appropriate message. Fixed volume: Press <F4> to show the mask in which you can enter the volume. You can not modify this entry in the sample preparation!
Entry type
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08/2004
Method
Sample
Molar mass M Equivalent number z Titration stand
You can enter only one molar mass and one equivalent number for the calculation. If your sample contains several substances which have to be determined by equivalence points in the titration, you must enter their molar mass and equivalent number in constant C under the Calculation function (see Section 3.3.12). Select the titration stand at which you wish to determine the sample from the selection menu: "Stand 1", "Stand 2", "ST20A", "Auto stand" or "External stand" (see Section 2.6). Press <F4> to select the sensor if you have attached one; if not, select "Manual": the temperature entered before starting the method will then be adopted in the processing of the method (see Section 5.1). This parameter is used for the automatic measurement or adoption of the temperature of the sample solution before the start of the Measure, EQP/EP/Learn titration and pH/mV-stat functions. Thus the slope of the pH electrode is temperature-corrected and incorporated in the calculation of the pH value (see Section 2.3: Temperature sensors).
Temperature sensor
ST20A titration stand If you are working with a sample changer, here you define whether you wish to pump solvent, rinse the sensor and/or condition. Press <F4> to display: Pump Pump Rinse Conditioning No No No No
Pump (1)
You have attached a pump to the sample changer that should pump solvent into the titration vessel before every titration. Press <F4> to activate the parameter, in the mask that appears select "Yes" and then press <F4> again: Pump Solvent Volume [mL] Stir Esc H2O 10 No Modify OK METHOD
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Sample
Method
Pump (1)
Select the solvent from the list (press <F4>) which contains the solvents you have defined in the Setup menu. This solvent also defines the ST20A output to which you must attach the pump (see Section 2.8). Enter the volume that should be dispensed. You have defined the pump rate of the device in the Setup menu. Select whether the dispensing operation should be stirred (Yes) or not (No). If you have attached a second pump to the sample changer, this will be activated as soon as the first dispensing operation is at an end. To activate the parameters, press <F4>, select Yes in the mask that appears and then press <F4> again: The same mask as described under Pump (1) appears. Selecting the solvent also defines the ST20A output to which you must attach the second pump (see Section 2.8). You have installed a rinsing unit in the titration head and attached a pump to the sample changer to rinse the sensor and burette tip after every titration. Press <F4> to activate the parameter, select "Yes" in the mask that appears and press <F4> again: Rinse Solvent Volume [mL] Esc H2O 10 Modify OK METHOD
Pump (2)
Rinse
Select the solvent from the list (press <F4>) which contains the solvents you have defined in the Setup menu. Selecting this solvent also defines the ST20A output to which you must attach the pump (see Section 2.8). Enter the volume which should be dispensed. Note: If you run sample series in succession on the sample changer (possible only with DL55/DL58) and the titrator has titrated the last sample of the last method, the sensor and burette tip are rinsed in the middle beaker position. The sample beaker is then raised to ensure the sensor does not dry out, in other words it remains in the sample solution. To prevent this, you must insert a conditioning beaker after the last sample beaker.
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Method
Sample
Conditioning
You must activate this parameter if you wish to condition the sensor: Press <F4>, select "Yes" in the mask that appears then press <F4> again: Conditioning Time [s] Interval Rinse Esc 10 1 No OK METHOD
Enter the time for conditioning. Enter the Interval (number of samples), e.g. 3, in other words, conditioning must be performed after every third sample. If the sensor and burette tip have to be rinsed after the conditioning, select Rinse and define the solvent and volume for this rinsing operation (see page 3-14). Notes The following are defined (example): 10 s, 3 as interval and rinse 10 s with H2O: 1. The ST20A conditions with the defined parameters if you place a conditioning beaker after every 3rd sample beaker (always mark conditioning beakers with red stopper plugs!)
S1 S2 S3
S4
S5
S6
S7
S8
S9
2. The ST20A conditions and rinses with the defined parameters if it detects a conditioning beaker after a sample beaker.
S1 S2
S3
S4
S5
S6
S7
S8
S9
3. If the ST20A does not detect a conditioning beaker after the 3rd sample beaker, it searches for one by rotating backward. It then conditions for 10 s, but does not perform rinsing to avoid overflow of the beaker contents.
C C
S1
S2
S3
S4
S5
S6
S7
S8
S9
4. After the last sample of a series, the time and rinse parameters are not executed anymore.
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3-15
Stir
Method
3.3.3
Stir
You can modify the stirring speed and stirring and wait times. Stir Speed [%] Time [s] Esc Speed 50 10 OK METHOD
0 % The stirrer is at a standstill; 100% The stirrer stirs at maximum speed. The speed you define applies to all following functions up to the next Stir function. However, you can also change the speed during a titration (see Section 6.2). "0" means that the titrator does not wait at all, "10" means that it waits 10 s before it starts the next function: It then stirs at the defined speed. The remaining stirring time appears in the display.
Time
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Method
Measure
3.3.4
Measure
You measure the potential of a solution under defined conditions. The titrator determines the measured value as raw result E (see note 2 at the end of this section). Sensor Unit of meas. E [mV] t [s] t(min) mode t(max) [s] DG111 mV 0.5 1.0 Fix 30
Sensor Unit of measurement
Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. The defined measurement unit is entered automatically. If you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu, otherwise you will receive an error message when the method is started. The drift of the electrode potential must be less than E/t (0.5 mV/s) during the period t (1 s) for the measured value to be acquired. This happens within a defined time span t(min) and t(max). (See diagram in Section 3.3.6.4: Equilibrium controlled measure mode). t(min) is the earliest time for measured value acquisition. Select t(min) from the selection menu: t(min) mode Fix E > set value E < set value Esc METHOD
E [mV] t [s]
t(min) mode
Modify
Fix: Press <F4> to show the mask in which you can modify t(min). E greater than set value: Instead of a fixed time, you can enter a condition: The measured value must be greater or less than a certain set value: Press <F4> to E less than set value: show the mask in which you enter the set value [mV, pH, ...].
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Measure
Method
t(max) [s]
t(max) is the latest time for measured value acquisition. If you have selected one of the conditions for t(min), the titrator starts the next function only when the measured potential E is greater or less than the set value and the drift condition is met, but at the latest after t(max).
Notes 1. If you have selected a temperature sensor under the Sample function, the temperature of the sample solution is measured automatically before the titrator executes this function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature entered at the start of the method. The slope of the pH electrode is temperature-corrected by this measured or entered value and incorporated in the calculation of the pH value. 2. The Measure, Dispense, EQP/EP/EQP (Ipol/Upol)/EP (Ipol/Upol)/EP/Learn titration and pH/mV-stat functions generate Raw results (see Section 8.1: List of symbols). These you can print out as such on the attached printer (see Sections 3.3.16 and 8.1.1 for exceptions). incorporate in the calculation (see Examples of formulas: Section 8.4). obtain as a result if you assign them to the result R: e.g. R = E (see Section 3.3.12). At the end of a titration, you obtain only the final results in the display of the titrator, the raw results you can only print out. The titrator stores raw results up to the determination of the next sample within a sample series (see Section 8.5.6).
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Method
Dispense
3.3.5
Dispense
You dispense a certain volume of a titrant with a METTLER TOLEDO burette. The titrator determines the dispensed volume as the raw result VDISP [mL] or QDISP [mmol] (see Section 8.1: List of symbols and Section 3.3.4: Measure function). Dispense Titrant Concentration [mol/L] Volume [mL] 1.0 Esc Titrant Concentration Volume NaOH 0.1 Modify OK METHOD
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Enter the volume to be dispensed. Instead of a number, you can enter a formula.
Note: If you do not need the Dispense function in the method, enter 0 for the volume: The function will then be skipped during the analysis.
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EQP titration
Method
3.3.6
EQP titration (equivalence point titration)
Here you define the control and evaluation of an equivalence point titration. The equivalence point is that point at which exactly the same number of equivalents of titrant and analyte have reacted. In most cases, it is virtually identical to the inflection point of the titration curve. This inflection point is recognized and the equivalence point calculated. Titrant/Sensor Predispensing Titrant addition Measure mode Recognition Termination Evaluation The titrator determines several measured values and volumes as raw results including the half neutralization value EHNV (see Section 8.1: List of symbols and Section 3.3.4: Measure function). Note: If you have selected a temperature sensor under the Sample function, the temperature of the sample solution is measured automatically before the titrator executes this function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature entered at the start of the method. The slope of the pH electrode is temperature-corrected by this measured or entered value and incorporated in the calculation of the pH value.
3.3.6.1
Titrant/Sensor
To modify the titrant or sensor, press <F4>: Titrant Concentration [mol/L] Sensor Unit of meas. Titrant Concentration NaOH 0.1 DG111 mV
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically.
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Method
EQP titration: Predispensing
Sensor Unit of measurement
Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2.). Confirm the one you want with OK. The defined measurement unit is entered automatically. If you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu, otherwise you will receive an error message when the method is started.
3.3.6.2
Predispensing
Predispensing shortens the titration time. You can select one of four predispensing modes when you press <F4>. to to to to No volume potential slope (factor x sample size)
Volume
You dispense a specified volume [mL] which you can enter when you press <F4>. Instead of a number, you can enter a formula. You can also enter a wait time: After the predispensing, the titrator waits for this time to elapse before it adds the titrant in a controlled manner. You dispense to a specified potential [mV, pH, ....] that you can enter when you press <F4>. You dispense to a specified slope [mV, pH, ..../mL] of the titration curve; this you can enter when you press <F4>. You dispense to a specified volume that is calculated from the product of the sample weight or volume and a factor; you can enter this factor when you press <F4>. You can also enter a wait time (see Volume). You do not wish to predispense.
Potential
Slope
Factor x sample size
No
In predispensing to volumes or (sample size x factor), the titrator adds the titrant in three steps (4/7, 2/7, 1/7 of the defined volume), which allows optimum calculation of the addition increment in the subsequent dynamic titration. In the predispensing to potential or slope, the titrant addition follows the selected parameters of the main titration, but the increments are larger.
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EQP titration: Titrant addition
Method
The titrator acquires the potential values ET1 and ET2 in the predispensing.
ET1: Potential at the start of predispensing or the titration ET2: Potential after predispensing Predispensing to a: Volume or (factor x sample size) b: Potential c: Slope
3.3.6.3
Titrant addition
You select the dynamic or incremental addition mode: Titrant addition Dynamic Incremental Esc Info Modify METHOD
You can not decide what addition mode is optimum for your method until you know the titration curve. You can obtain general information by pressing <F3>: You generally select the dynamic addition mode for acid/base titrations in aqueous media or for argentometric and redox titrations, the incremental for acid/base titrations in nonaqueous media or for complexometric, redox and surfactant titrations. Dynamic The volume increment added by the titrator changes within the defined smallest and largest increment: V(min) and V(max). This should lead to a constant potential difference E per increment. Dynamic E(set) [mV] V(min) [mL] V(max) [mL] Esc
3-22
METHOD 8.0 0.02 0.15 Help
OK
08/2004
Method
Dynamic
E [mV]
E~~ E(set) E E(soll)
E5 E4 E3 V3 V4 V [mL]
If no predispensing takes place, the titrator dispenses the first two volume increments with V(min). Help If you press <F3>, you can adopt the values for all three parameters from the mask that appears. With the proposed value groups, sufficient measured points in the vicinity of the equivalence point should be generated to optimize its evaluation: For steep titration curves, a value for E must be selected which is smaller than for flat titration curves, e.g. 8 mV. For titration curves which show a sudden potential change, small values for E and V(max) should be selected, e.g. 4 mV.
E [mV]
steep curve flat curve
curve with sudden potential jump

V [mL]
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Method
Dynamic
Note: The smallest increment that the titrator can dispense is 1/5000 of the burette volume: 1 mL burette 0.0002 mL 5 mL burette 0.001 mL 10 mL burette 0.002 mL 20 mL burette 0.004 mL The volume increment added by the titrator is constant. Incremental V [mL] 0.3 METHOD
Incremental
Esc
E [mV]
Help
OK
E14
E13
E12
V [mL] V12 V14
Help If you press <F3>, you can adopt a value for V from the mask that appears. The proposed values are intended to achieve the same goal as in the dynamic titrant addition: sufficient measured points in the vicinity of the equivalence point to optimize its evaluation: For steep titration curves, a smaller V must be selected than for flat curves to ensure there are sufficient measured points at the equivalence point. For titration curves which exhibit a sudden potential change, a small V should be selected.
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Method
EQP titration: Measure mode
3.3.6.4
Measure mode
You select the equilibrium controlled or timed increment measured value acquisition: Measure mode Equilibrium controlled Timed increment Esc Info Modify METHOD
These parameters are used to define the wait time up to measured value acquisition following an incremental addition. In the equilibrium controlled measure mode, the wait time is variable, in the timed increment it is constant. You can not decide the optimum measure mode for your method until you know the reaction time of the components and the response time of the sensor used. General information is available under <F3>: Select the equilibrium controlled measure mode for, e.g. acid/base titrations in aqueous media, argentometric, complexometric, surfactant and redox titrations. the timed increment mode for acid/base titrations in nonaqueous media. Equilibrium controlled E [mV] t [s] t(min) [s] t(max) [s] 0.5 1.0 3.0 30.0
Before the titrator adds the next increment, an equilibrium must be established in the solution; the measured value must stabilize. The following are responsible for the equilibrium the potential change E measured in the solution within the defined time t. The wait time up to the next increment addition also depends on the definition of the minimum time t(min) and the maximum time t(max) As soon as the potential change of the solution is less than the defined equilibrium (E/t), the titrator acquires the measured value and adds the next increment. This can be at t(min) at the earliest and should be at t(max) at the latest. At t(max) the measured value is in any case acquired, even if the equilibrium condition is not yet met.
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Method
Equilibrium controlled
164 163 162 161 160 159
E [mV]
t = 2 s a E = 1 mV
t = 2 s 158 157 156 155 154 t(min) 153 b 152 151 Increment addition t [s] 0 1 t(min) 5 0 1 t(min) 5 7 Increment addtion b a E = 1 mV t(min)
a: The defined equilibrium condition is not yet met. t(min): The equilibrium condition is not met after 3 s. b: The equilibrium condition is met for the first time after 5.4 or 6.9 s.
This measure mode results in fast increment addition in the flat part of the titration curve and slow addition in the steep part. In addition to the potential, the titrator acquires the time and the titrant volume. You can print out these measured values after the titration of a sample (see Section 3.3.16: Report). Help When you press <F3>, you can adopt suggested values for all four parameters from the mask that appears: Fast titrations are, e.g. acid/base titrations in aqueous media, slow titrations, e.g. precipitation titrations in nonaqueous media.
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Method
Timed increment
After every increment addition, the titrator allows the time you have defined to elapse before it acquires the measured value. Timed increment t [s] 3.0 METHOD
Esc
Help
OK
Help When you press <F3>, you can adopt suggested values for the time interval from the mask that appears: Enter small time intervals for, e.g. acid/base titrations in aqueous media, large intervals for, e.g. precipitation titrations in nonaqueous media, 90 seconds for, e.g. TAN/TBN titrations of oils.
E [mV]
Measured value
Increment addition Increment addtion Increment addition
Measured values
t [s] t 1 = 3 s t 2 = 3 s t 3 = 3 s
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EQP titration: Recognition
Method
3.3.6.5
Recognition
Recognition of the equivalence point of a titration curve depends on the type of reaction of the components and hence on the evaluation procedure (see Section 3.3.6.7): 1. With the evaluation procedures Maximum and Minimum, an equivalence point is recognized when the greatest (smallest) potential value of the titration curve is greater (less) than two preceding and two subsequent values. 2. With the evaluation procedures Standard and Asymmetric, an equivalence point is recognized when the maximum of the absolute values of the 1st derivative of the titration curve is greater than two preceding and two subsequent values. 3. With the evaluation procedure Segmented, an equivalence point is recognized when the maximum of the absolute values of the 2nd derivative of the titration curve is greater than two preceding and two subsequent values. Note: For the first recognition of a possible equivalence point, the titrator needs a certain number of measured points. The number depends on the evaluation procedure. Measured points of a predispensing are not taken into account! Evaluation procedure Minimum/Maximum Standard Asymmetric Segmented First possible EQP at 4th measured point 4th measured point 4th measured point 5th measured point Required number of measured points 6 6 10 8
Example illustrating the evaluation procedure Minimum: If the lowest potential value is found at the third measured point, it is not recognized as an equivalence point. You must or can support the equivalence point recognition using four parameters: Threshold Steepest jump only Range Tendency 10.0 No No None
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Method
Threshold
To ensure that minor disturbances in the curve profile are not recognized as equivalence points, you must determine a threshold value: +/-E, E/V or 2E/V2. This must be exceeded. Notes 1. The threshold value should be maximum half as large as the expected maximum value of the first or second derivative at the equivalence point. 2. The threshold value depends on so many factors (solvent, concentration, sensor, type of reaction, etc.) that you can not define the "correct" threshold value until you have performed the first titration. Info You can obtain general information on threshold values in the standard evaluation if you press <F3>: For steep, normal and flat titration curves, ranges of threshold values are given for the first derivative in "pH/mL" and "mV/mL". With the other evaluation procedures, you can enter one of the following values for the first titration: Evaluation procedure Minimum/Maximum Asymmetric Segmented mV 0 10 10 pH/pM/pX 0 0.2 0.2 %T 0 1 1
Using the corresponding titration curve or the table of measured values (there is no table for the 2nd derivative), you can read off the potential value, the values for E/V or the values for 2E/V2 and then enter the threshold value.
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Method
Threshold
Example of threshold value of a titration curve for the evaluation procedure Minimum
E [mV]
+100
The minimum of this titration curve lies at -150 mV. You can enter, for example, -30 as the threshold value. The sign for the mV value must be entered.
Threshold value
0 -30 -100
Minimum V [mL]
Example of threshold value of a titration curve for the evaluation procedures Standard and Asymmetric
E [mV] Titration curve
V [mL] E/ V [mV/mL] 1st derivative Maximum (absolute)
Measured value
Threshold value V [mL]
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Method
EQ titration: Recognition
Threshold
Example of threshold value of a titration curve for the evaluation procedure Segmented
Titration curve
E [mV]
V [mL] 1st derivative E/V [mV/mL]
V [mL]
2nd derivative
2E/ V2 [mV/mL2]
Maximum (absolute) Measured value
Threshold value
V [mL]
Steepest jump only
You can also select this parameter for recognition of the equivalence point (press <F4>): The titrator then recognizes only the steepest jump of the titration curve.
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Method
Range
You can also define a potential range for recognition of the equivalence point. Equivalence points which lie outside this range are not recognized. Press <F4>, select "Yes" in the mask that appears and then press <F4> again: Range Limit A [mV,pH,..] Limit B [mV,pH,..] Esc 100 -100 OK METHOD
Instead of a number, you can also enter a potential stored as an auxiliary value or a formula. The equivalence point range always refers to the titration curve, in other words it is independent of the evaluation procedure. Tendency As a further aid in recognition of the equivalence point, you can define the tendency, namely in what part of the titration curve descending or ascending the equivalence point should be located (see diagram). Use <F4> to select the tendency: "None", "Positive" or "Negative".
Example illustrating selection of a range and positive tendency. Equivalence points which lie outside this range and which do not have the right tendency are ignored. Notice: A positive mV change means a negative pH change!
E [mV]
Limit A = +200 EQP Limit B = +100
Tendenz: positiv Tendency: positive
0 V [mL]
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Method
EQP titration: Termination
3.3.6.6
Termination
You can define how a titration should be terminated by selection of five different parameters. The titrator can terminate the titration either when the first of the selected conditions is met, or when all the selected conditions are met. An exception is the maximum volume: when this is reached, the titration is immediately terminated! at maximum volume [mL] at potential at slope after number EQPs comb. termination conditions 10.0 No No No No
Maximum volume You must enter the maximum volume. It is intended as a safety precaution: if the titration is faulty, an excessive amount of titrant is not dispensed unnecessarily as the titration is always terminated. Potential The titrator terminates the titration at the defined potential. Press <F4>, select "Yes" in the mask that appears then press <F4> again: At potential Potential [mV,pH,..] 0.0 METHOD
Esc
OK
Instead of a number, you can also enter a potential stored as an auxiliary value or a formula. Slope The titrator terminates the titration when the slope of the titration curve is less than a certain value. The measured slope must exceed this absolute value once and drop below it twice to terminate the titration. Press <F4>, select "Yes" and press <F4> again: Enter the slope [mV, pH,.../mL] in the mask that appears.
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EQP titration: Evaluation
Method
Number EQPs
The titrator terminates the titration after a certain number n of equivalence points has been found. Press <F4>, select "Yes" and press <F4> again: Enter the number in the mask that appears.
Comb. terminate- The titrator does not terminate the titration until all defined termination conditions are met (exception: maximum volume, see above). tion criteria Select "Yes" with <F4>.
3.3.6.7
Evaluation
You determine which evaluation procedure is used to calculate the equivalence points found and select potential values you wish to have evaluated. Procedure Potential 1 Potential 2 Stop for reevaluation Procedure Standard No No No
Use <F4> to select the procedure among several calculation modes which matches the titration curve (see Section 8.3). Standard Evaluation procedure for all S-shaped titration curves Minimum Determination of the minimum of a titration curve Maximum Determination of the maximum of a titration curve Segmented Evaluation procedure for titration curves with segments (segmented curve) Asymmetric Evaluation procedure for S-shaped, highly asymmetric titration curves. Note: If an evaluation is not possible with the standard procedure, the equivalence point is calculated by interpolation (see Section 8.3.1). If an evaluation is not possible with the asymmetric procedure, the equivalence point is calculated by the standard procedure or by interpolation (see Section 8.3.4). In both cases, the evaluation procedure will be documented for each sample in the raw results report if it differs from the defined procedure. If you have to work according to GLP guidelines, you should therefore always record the raw results (see Section 3.3.16).
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Method
EQP titration: Evaluation
Potential 1
In the selection of potentials, the titrator evaluates not only the equivalence points, but also the titrant consumption in mmol or mL required for attainment of these potential values (see Section 8.1: List of symbols). Press <F4>, select "Yes" and press <F4> again: Enter the first potential [mV, pH,...] in the mask that appears. Instead of a number, you can also enter a potential stored as an auxiliary value or a formula (see Section 2.5: Auxiliary values). If you wish to have a second potential evaluated, proceed as described for potential 1. Notes for Potential 1/2 1. If you have selected potential 1 and/or 2, the titrator does not test all termination conditions except maximum volume until the potentials are reached (see Section 3.3.6.6). 2. When you select the two potentials, you also define the tendency (from P1 to P2) and the order: If the titrator finds P2 first, it will no longer search for P1.
Potential 2
Stop for reevaluation
The EQP titration function is interrupted immediately before its completion if the termination conditions and the condition defined here are met. This allows you to modify parameters of the equivalence point recognition (all) and the evaluation (potential 1 and 2). All evaluations are performed again using the modified parameters (see Section 5.2.2). Press <F4>, select "Yes" in the mask that appears then press <F4> again: Reevaluation Condition neq=0 METHOD
Esc
Symbol
Modify
OK
The condition "neq = 0" means that the EQP titration function is interrupted immediately before its completion if no equivalence point has been found.
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Method
Modify Use <F4> to select a different condition in the list that appears: neq > 1: If more than one, neq < 2: less than two, or 3 > neq > 0: one or two equivalence points are found, the titration will always be interrupted. Symbol Press <F3> to show the list of symbols (see Section 8.1). You can select symbols from this list to define your own condition, e.g. VEQ > 0.6: - Select "neq > 1" (under "Modify" command) - delete "neq" - select "VEQ" from the symbol list - then position cursor on "1" and replace by "0.6".
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Method
EP titration
3.3.7
EP titration (end point titration)
Here you define the control and evaluation of an end point titration and thus titrate to a particular value of the selected measurement unit.
NOTICE
Before an end point titration to a particular pH value, you should calibrate the pH electrode used! Titrant/Sensor Predispensing Titrant addition End point Tendency Termination
The titrator determines several measured values and volumes as raw results (see Section 8.1: List of symbols and Section 3.3.4: Measure function). Note: If you have selected a temperature sensor under the Sample function, the temperature of the sample solution is measured automatically before the titrator executes this function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature entered at the start of the method. The slope of the pH electrode is temperature-corrected by this measured or entered value and incorporated in the calculation of the pH value.
3.3.7.1
Titrant/Sensor
To modify the titrant or sensor, press <F4>: Titrant Concentration [mol/L] Sensor Unit of meas. Titrant Concentration Sensor NaOH 0.1 DG111 mV
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK.
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EP titration: Predispensing
Method
Unit of measurement
The defined unit of measurement is entered automatically. When you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu, otherwise you will receive an error message when the method is started.
3.3.7.2
Predispensing
Predispensing shortens the titration time. You can select one or two predispensing modes when you press <F4>. Predispensing to volume to (factor x sample size) No Esc Volume METHOD
Modify
You dispense to a specified volume [mL] that you can enter when you press <F4>. Instead of a number, you can enter a formula. You can also enter a wait time: After the predispensing, the titrator waits for this time to elapse before it adds the titrant in a controlled manner. You dispense to a specified volume that is calculated from the product of the sample weight or volume and a factor; you can enter this factor if you press <F4>. You can also enter a wait time (see Volume). You do not wish to predispense.
No
In the subsequent continuous titrant addition, the titrator dispenses the volume in one step. It acquires the potential values ET1 and ET2 (see Section 3.3.6.2). In the subsequent dynamic titrant addition, it dispenses the volume in three steps (4/ 7, 2/ 7, 1/ 7 of the defined volume), which allows optimum calculation of the addition increment. It acquires the potential values ET1 and ET2.
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Method
EP titration: Titrant addition
3.3.7.3
Titrant addition
You can select a dynamic or continuous addition mode: Titrant addition Dynamic Continuous Esc Info Modify METHOD
Press <F3> for general information on what addition mode you should select: In general, select the dynamic addition mode for acid/base titrations in aqueous media, argentometric and redox titrations, the continuous mode for acid/base titrations in nonaqueous media. Dynamic For dynamic titrant addition in the EP titration, the same conditions apply as in dynamic addition in the EQP titration (see Section 3.3.6.3). The measured values are acquired with equilibrium control as in the EQP titration (see Section 3.3.6.4). E(set) [mV] V(min) [mL] V(max) [mL] E [mV] t [s] t(min) [s] t(max) [s] 8.0 0.02 0.15 1.0 1.0 2.0 10.0
dynamic titrant addition
equilibrium controlled measured value acquisition
Help (titrant addition) If you have selected the first three parameters and press <F3>, you can adopt suggested values for the dynamic addition from the mask that appears. For steep titration curves, a smaller value of E must be selected than for flat titration curves. For titration curves that exhibit a sudden jump, small values for E and V(max) should be selected. In the absence of predispensing, the titrator dispenses the first two volume increments with V(min).
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EP titration: Titrant addition
Method
Dynamic
Help (measured value acquisition) If you have selected one of the last four parameters and press <F3>, you can adopt suggested values for the equilibrium condition from the mask that appears: Fast titrations are, e.g. acid/base titrations in aqueous media, slow titrations are, e.g. precipitation titrations in nonaqueous media. The equilibrium conditions apply only in the end point range defined by the following formula: EP range = EP {1.5 * E(set)}. Example: If the end point is -30 mV, the condition holds for above values of -15 to -45 mV. Outside this range: E (outside) = 4 * E holds. If the end point is reached: E = E/2 holds.
Continuous
Continuous Control band [mV, pH,...] V(min) [mL] 0.01 Esc Help 100.0
METHOD
OK
The titrator dispenses the titrant slowly at the start then at the maximum rate until the defined control band. Within the control range, the dispensing rate decreases exponentially. In the vicinity of the end point, the titrator adds the increment V(min) (the smallest increment that the titrator can dispense is 1/5 000 of the burette volume).
E [mV, pH] Start of the control range +200 4 5 6 0 7 8 -100 End point V [mL] Control band = 250 mV (4.3 pH)
+100
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Method
EP titration: End point
Continuous
Help When you press <F3> you can adopt suggested values for the continuous addition from the mask that appears (confirm with OK). For titration curves with a steep control range, the control band must be larger than that for the flat control range. For V(min) you can enter a formula instead of a number. The titrator measures the initial potential ET1 after 1 - 3 seconds and for the table of measured values it acquires a measured value every 5 seconds.
3.3.7.4
End point
You have a choice between two end point titrations. End point EP absolute EP relative Esc EP absolute Modify METHOD
The absolute end point is the value on the electrode signal scale referred to zero. Press <F4> and enter the potential [mV, pH, ...] in the mask that appears. Instead of a number, you can enter a formula or call up a potential stored as an auxiliary value. Example: You have stored the value of "EPOT" of H3PO4 for the 1st equivalence point as H4. If you wish to titrate to this potential, enter H4. The relative end point is the difference between the electrode signal at the start of the titration and that at the end. Press <F4> and enter the potential [mV, pH, ...] in the mask that appears.
EP relative
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EP titration: Tendency/Termination
Method
3.3.7.5
Tendency
A titration exhibits a positive or negative mV or pH change (see diagram). You have to define this. Press <F4> and select "Positive" or "Negative" in the mask that appears (press <F4>).
NOTICE
A positive mV change means a negative pH change!

E [mV pH] Start potential 3 + 200 4 5 6 0 7 8 End potential EP relative = 310 mV (pH 5.2) Tendency positive (mV) negative (pH) Tendency negative (mV) positive (pH)
+ 300
+ 100
EP absolute = - 30 mV (pH 7.5) V [mL]
3.3.7.6
Termination
You define the termination of a titration by selecting two parameters. Termination Maximum volume [mL] Delay [s] Esc 10.0 10 OK METHOD
Maximum volume You must define the volume. It is intended as a safety precaution: if the titration is faulty, an excess amount of titrant is not added unnecessarily. Delay is the time from attainment of the end point up to definitive termination of the titration. If the measured value of the end point decreases within the specified time, the titrator adds additional increments.
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Method
Learn titration
3.3.8
Learn titration
If you are not sure what parameters you should enter for the titration function, select the standard method Learn titration and define the parameters for the titrant and sensor under the Learn titration function. Note: The titrator always titrates the entire volume of the burette used. You thus have to select weight/volume of your sample in accordance with the burette volume. Learn titration Titrant/Sensor METHOD
Esc To modify the titrant or sensor, press <F4>: Titrant Concentration [mol/L] Sensor Unit of meas. Titrant Concentration Sensor Unit of measurement NaOH 0.1 DG111 mV
Modify
OK
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. The defined measurement unit is entered automatically. If you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu. Otherwise you will receive an error message when the method is started.
When you start the method, the titrator executes one function after another. As soon as it has completed the Learn titration function, it calculates the parameters from the response behavior of the sensor, the shape of the titration curve and with consideration of the burette volume. It stores these as an EQP titration function and sends the data to the printer. While the data are being printed, the titrator executes the remaining functions: The "Learn titration" has given rise to an equivalence point titration!
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Learn titration
Method
Printout of a learned EQP titration (example: acid determination with NaOH)

LEARN TITRATION Method 12 Version Learn titration 28-Oct-1996 14:36
EQP titration Titrant/Sensor Titrant ............................... Concentration [mol/L] ................. Sensor ................................ Unit of meas. ......................... Predispensing ............................. Volume [mL] ........................... Wait time [s] ......................... Titrant addition .......................... E(set) [mV] .......................... V(min) [mL] .......................... V(max [mL] ........................... Measure mode .............................. E [mV] ............................... t [s] ............................... t(min) [s] ............................ t(max) [s] ............................ Recognition Threshold ............................. Steepest jump only .................... Range ............................... Tendency .............................. Termination at maximum volume [mL] ................ at potential .......................... at slope .............................. after number EQPs ..................... n = ................................ comb. termination conditions .......... Evaluation Procedure ............................. Potential 1 ........................... Potential 2 ........................... Stop for reevaluation .................
NaOH 0.1 DG111 pH to volume 1.0 0 Dynamic 12.0 0.08 0.4 Equilibrium controlled 1.0 1.0 2.0 20.0 2.0 No No None 10.0 No No Yes 1 No Standard No No No
If the titrator finds more than one equivalence point, it calculates the parameters for the one with the steepest jump. If the titrator does not find any equivalence points, it interrupts the method and an error message appears (see Section 5.2.2). The titrator first recognizes a possible equivalence point when this lies at the sixth measured point (see Section 3.3.6.5). As an EQP titration emerges immediately from the Learn titration function, you can titrate a series of samples with the same content. If you have selected "Statistics" under the Calculation function, the result of the first sample will then be discarded!
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Method
EQP titration (Ipol/Upol)
3.3.9
EQP titration (Ipol/Upol)
Here you define the control and evaluation of a voltametric or amperometric equivalence point titration. The equivalence point is that point at which exactly the same number of equivalents of titrant and analyte have reacted. In most cases, it is virtually identical to the inflection point of the titration curve. This inflection point is recognized and the equivalence point calculated. Titrant/Sensor Indication Predispensing Titrant addition Measure mode Recognition Termination Evaluation The titrator determines several measured values and volumes as raw results (see Section 8.1: List of symbols and Section 3.3.4: Measure function).
3.3.9.1
Titrant/Sensor
To modify the titrant or sensor, press <F4>: Titrant/Sensor

1/ I Titrant 2 2 Concentration [mol/L] 0.1 Sensor DM142 Esc
METHOD
Modify
OK
Titrant Concentration Sensor
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.4.). Confirm the one you want with OK.
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EQP titration (Ipol/Upol): Indication
Method
3.3.9.2
Indication
To select the voltametric or amperometric indication, press <F4>: Indication Voltametric Amperometric Esc Voltametric Modify METHOD
The potential difference between two metal electrodes is measured by polarizing them with a constant current (in the case of the DM142 electrode, the two pins of the platinum electrode are polarized). Press <F4> to enter the current Ipol. Its value depends among other things on: the electrode itself (e.g. distance between the platinum pins in the case of the DM142 electrode) the dissolved substance to be determined and its concentration the solvent the reaction with the titrant. You can obtain an initial starting point for the current intensity to be selected by measuring the corresponding solutions with different current intensities (see Section 6.1.4) and recording the voltage value. This should lie within the measurement range 1500 mV for both the initial and the equivalence point potential (see Section 12.1: Technical Data).
Example of a vitamin C determination in a multivitamin drink with DPI [0.01 mol/L]
E [mV]
V [mL]
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Method
EQP titration (Ipol/Upol): Indication
Amperometric
The potential difference between two metal electrodes is measured by polarizing them with a constant voltage (in the case of the DM142 electrode, the two pins of the platinum electrode are polarized). Press <F4> to enter the voltage Upol. Its value depends on the same factors mentioned under the parameter "Voltametric". You can obtain an initial starting point for the voltage to be selected by measuring the corresponding solutions with different voltage values (see Section 6.1.4) and recording the current intensity. This should lie within the measurement range 150 A for both the initial and the equivalence point potential (see Section 12.1: Technical Data).
E [A]
Example of a vitamin C determination in a multivitamin drink with DPI [0.01 mol/L]
V [mL]
Note: Higher current or voltage values result in higher jumps (a steeper curve) in the equivalence point region, however the platinum pins of the electrode become contaminated quicker.
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EQP titration (Ipol/Upol): Predispensing/Titrant addition
Method
3.3.9.3
Predispensing
Predispensing shortens the titration time. You can select one of two predispensing modes when you press <F4>. Predispensing to E volume ~ E(set) to (factor x sample size) No Esc Volume METHOD
Change
You dispense a specified volume [mL] which you can enter when you press <F4>. Instead of a number, you can enter a formula. You can also enter a wait time: After the predispensing, the titrator waits for this time to elapse before it adds the titrant in a controlled manner. You dispense to a specified volume that is calculated from the product of the sample weight or volume and a factor; you can enter this factor when you press <F4>. You can also enter a wait time (see Volume). You do not wish to predispense.
No
In predispensing to volumes or (sample size x factor), the titrator adds the titrant in three steps (4/7, 2/7, 1/7 of the defined volume).
3.3.9.4
Titrant addition
You can enter only a constant increment for the volume (see Section 3.3.6.3: Incremental titrant addition): Titrant addition V [mL] 0.05 METHOD
Esc
OK
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Method
EQP titration (Ipol/Upol): Measure mode
3.3.9.5
Measure mode
You select the equilibrium controlled or timed increment measured value acquisition: Measure mode Equilibrium controlled Timed increment Esc Modify METHOD
These parameters are used to define the wait time up to measured value acquisition following an incremental addition. In the equilibrium controlled measure mode, the wait time is variable, in the timed increment it is constant. You can not decide the optimum measure mode for your method until you know the reaction time of the components and the response time of the sensor used. Equilibrium controlled E [mV, A] t [s] t(min) [s] t(max) [s] 0.5 1.0 3.0 30.0
Before the titrator adds the next increment, an equilibrium must be established in the solution; the measured value must stabilize. The following are responsible for the equilibrium the potential change E measured in the solution within the defined time t. The wait time up to the next increment addition also depends on the definition of the minimum time t(min) and the maximum time t(max) As soon as the potential change of the solution is less than the defined equilibrium (E/t), the titrator acquires the measured value and adds the next increment. This can be at t(min) at the earliest and should be at t(max) at the latest. At t(max) the measured value is in any case acquired, even if the equilibrium condition is not yet met (see diagram in Section 3.3.6.4). This measure mode results in fast increment addition in the flat part of the titration curve and slow addition in the steep part.
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EQP titration (Ipol/Upol): Recognition
Method
Timed increment
After every increment addition, the titrator allows the time you have defined to elapse before it acquires the measured value (see diagram in Section 3.3.6.4). Timed increment t [s] 3.0 METHOD
Esc
OK
For both measure modes, the titrator acquires the potential, the time and the titrant volume. You can print out these measured values after the titration of a sample (see Section 3.3.16: Report).
3.3.9.6
Recognition
Recognition of the equivalence point of a titration curve depends on the type of reaction of the components and hence on the evaluation procedure (see Section 3.3.9.8): 1. With the evaluation procedures Maximum and Minimum, an equivalence point is recognized when the greatest (smallest) potential value of the titration curve is greater (less) than two preceding and two subsequent values. 2. With the evaluation procedures Standard and Asymmetric an equivalence point is recognized when the maximum of the absolute values of the 1st derivative of the titration curve is greater than two preceding and two subsequent values. 3. With the evaluation procedure Segmented, an equivalence point is recognized when the maximum of the absolute values of the 2nd derivative of the titration curve is greater than two preceding and two subsequent values. Note: For the first recognition of a possible equivalence point, the titrator needs a certain number of measured points (see Section 3.3.6.5). You must or can support the equivalence point recognition using four parameters: Threshold Steepest jump only Range Tendency 10.0 No No None
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Method
EQP titration (Ipol/Upol): Recognition
Threshold
To ensure that minor disturbances in the curve profile are not recognized as equivalence points, you must determine a threshold value: +/-E, E/V oder 2E/V2. This must be exceeded. Notes 1. The threshold value should be maximum half as large as the expected maximum value of the first or second derivative at the equivalence point. 2. The threshold value depends on so many factors (solvent, concentration, sensor, type of reaction, etc.) that you can not define the "correct" threshold value until you have performed the first titration. 3. You will find examples of the threshold value for the different evaluation procedures in Section 3.3.6.5.
Steepest jump only
You can also select this parameter for recognition of the equivalence point (press <F4>): The titrator then recognizes only the steepest jump of the titration curve. You can also define a potential range for recognition of the equivalence point. Equivalence points which lie outside this range are not recognized. Press <F4>, select "Yes" in the mask that appears and then press <F4> again: Range Limit A [mV, A] Limit B [mV, A] Esc 100 200 OK METHOD
Range
Instead of a number, you can also enter a potential stored as an auxiliary value or a formula. The equivalence point range always refers to the titration curve, in other words it is independent of the evaluation procedure. Tendency As a further aid in recognition of the equivalence point, you can define the tendency, namely in what part of the titration curve descending or ascending the equivalence point should be located (see diagram on page 3-32). Use <F4> to select the tendency: "None", "Positive" or "Negative".
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EQP titration (Ipol/Upol): Termination
Method
3.3.9.7
Termination
You can define how a titration should be terminated by selection of five different parameters. The titrator can terminate the titration either when the first of the selected conditions is met, or when all the selected conditions are met. An exception is the maximum volume: when this is reached, the titration is immediately terminated! at maximum volume [mL] at potential at slope after number EQPs comb. termination conditions 10.0 No No No No
Maximum volume You must enter the maximum volume. It is intended as a safety precaution: if the titration is faulty, an excessive amount of titrant is not dispensed unnecessarily as the titration is always terminated. Potential The titrator terminates the titration at the defined potential. Press <F4>, select "Yes" in the mask that appears then press <F4> again: At potential Potential [mV, A] 0.0 METHOD
Esc
OK
Instead of a number, you can also enter a potential stored as an auxiliary value or a formula. Slope The titrator terminates the titration when the slope of the titration curve is less than a certain value. The measured slope must exceed this absolute value once and drop below it twice to terminate the titration. Press <F4>, select "Yes" and press <F4> again: Enter the slope [mV/mL] or [A/mL] in the mask that appears.
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Method
EQP titration (Ipol/Upol): Evaluation
Number EQPs
The titrator terminates the titration after a certain number n of equivalence points has been found. Press <F4>, select "Yes" and press <F4> again: Enter the number in the mask that appears. The titrator does not terminate the titration until all defined termination conditions are met (exception: maximum volume, see above). Select "Yes" with <F4>.
Comb. termination criteria
3.3.9.8
Evaluation
You determine which evaluation procedure is used to calculate the equivalence points found and select potential values you wish to have evaluated. Procedure Potential 1 Potential 2 Stop for reevaluation Procedure Standard No No No
Use <F4> to select the procedure among several calculation modes which matches the titration curve (see Section 8.3). Standard Evaluation procedure for all S-shaped titration curves; can be used for curves with steep jumps in titrations with voltametric and amperometric indication. Minimum Determination of the minimum of a titration curve Maximum Determination of the maximum of a titration curve Segmented Evaluation procedure for titration curves with segments (segmented curve); can be used for titrations with amperometric indication. Asymmetric Evaluation procedure for S-shaped, highly asymmetric titration curves.
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Method
Procedure
Notes 1. In an evaluation with the standard procedure is not possible, the equivalence point is calculated by interpolation (see Section 8.3.1). If an evaluation is not possible with the asymmetric procedure, the equivalence point is calculated by the standard procedure or by interpolation (see Section 8.3.4). In both cases, the evaluation procedure will be documented for each sample in the "raw results" report if it differs from the defined procedure. If you have to work according to GLP guidelines, you should therefore always record the raw results (see Section 3.3.16). 2. If you determine the same sample with a voltametric and amperometric EQP titration, in many cases you must change not only the parameters of the indication, measured value acquisition and recognition, but also the evaluation procedure. An example is the vitamin C determination in a multivitamin drink with DPI [0.01mol/L]:
Voltametric titration: Standard
E [mV]
Amperometric titration: Segmented

E [A]
E-V curve
E-V curve
E/V-V curve
E/V-V curve
2E/V2-V curve
2E/V2-V curve
V [mL]
V [mL]
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Method
Procedure
3. If you obtain a so-called Z curve in an equivalence point determination (see diagram), we recommend performing an end point titration.
E [mV]
Example of a titer determination of iodine solution [0.1 mol/L] with L-ascorbic acid (vitamin C)
V [mL]
Potential 1
In the selection of potentials, the titrator evaluates not only the equivalence points, but also the titrant consumption in mmol or mL required for attainment of these potential values (see Section 8.1: List of symbols). Press <F4>, select "Yes" and press <F4> again: Enter the first potential [mV, A] in the mask that appears. Instead of a number, you can also enter a potential stored as an auxiliary value or a formula (see Section 2.5: Auxiliary values). If you wish to have a second potential evaluated, proceed as described for potential 1. Notes for Potential 1/2 1. If you have selected potential 1 and/or 2, the titrator does not test all termination conditions except maximum volume until the potentials are reached (see Section 3.3.9.7). 2. When you select the two potentials, you also define the tendency (from P1 to P2) and the order: If the titrator finds P2 first, it will no longer search for P1.
Potential 2
The EQP titration (Ipol/Upol) function is interrupted immediately before its completion if the termination conditions and the condition defined here are met (see Section 3.3.6.7).
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EP titration (Ipol/Upol)
Method
3.3.10
EP titration (Ipol/Upol)
Here you define the control and evaluation of an end point titration with voltametric or amperometric indication. Titrant/Sensor Indication Predispensing Titrant addition End point Tendency Termination The titrator determines several measured values and volumes as raw results (see Section 8.1: List of symbols and Section 3.3.4: Measure function).
3.3.10.1
Titrant/Sensor
To modify the titrant or sensor, press <F4>: Titrant/Sensor

1/ I Titrant 2 2 Concentration [mol/L] 0.1 Sensor DM142 Esc
METHOD
Modify
OK
Titrant Concentration Sensor
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.4). Confirm the one you want with OK.
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Method
EP titration (Ipol/Upol): Indication
3.3.10.2
Indication
Press <F4> to select the voltametric or amperometric titration : Indication Voltametric Amperometric Esc Voltametric Modify METHOD
The potential difference between two metal electrodes is measured by polarizing them with a constant current (in the case of the DM142 electrode, the two pins of the platinum electrode are polarized). Press <F4> to enter the current Ipol. Its value depends among other things on: the electrode itself (e.g. distance between the platinum pins in the case of the DM142 electrode) the dissolved substance to be determined and its concentration the solvent the reaction with the titrant. You can obtain an initial starting point for the current intensity to be selected by measuring the corresponding solutions with different current intensities (see Section 6.1.4) and recording the voltage value. This should lie within the measurement range 1500 mV for both the initial and the end point potential (see Section 12.1: Technical Data).
E [mV]
Example of a Karl Fischer titration with Hydranal (2-component system)
V [mL]
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EP titration (Ipol/Upol): Indication
Method
Amperometric
The potential difference between two metal electrodes is measured by polarizing them with a constant voltage (in the case of the DM142 electrode, the two pins of the platinum electrode are polarized). Press <F4> to enter the voltage Upol. Its value depends on the same factors mentioned under the parameter "Voltametric". You can obtain an initial starting point for the voltage to be selected by measuring the corresponding solutions with different voltage values (see Section 6.1.4) and recording the current intensity. This should lie within the measurement range 150 A for both the initial and the end point potential (see Setion 12.1: Technical Data).
E [A]
Example of a Karl Fischer titration with Hydranal (2-component system)
V [mL]
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Method
EP titration (Ipol/Upol): Predispensing
3.3.10.3
Predispensing
Predispensing shortens the titration time. You can select one or two predispensing modes when you press <F4>. Predispensing to volume to (factor x sample size) No Esc Volume METHOD
Modify
You dispense to a specified volume [mL] that you can enter when you press <F4>. Instead of a number, you can enter a formula. You can also enter a wait time: After the predispensing, the titrator waits for this time to elapse before it adds the titrant in a controlled manner. You dispense to a specified volume that is calculated from the product of the sample weight or volume and a factor; you can enter this factor if you press <F4>. You can also enter a wait time (see "Volume"). You do not wish to predispense.
No
With the predispensing, the titrator dispenses the volume in one step.
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EP titration (Ipol/Upol): Titrant addition/End point
Method
3.3.10.4
Titrant addition
The addition can only be continuous (see Section 3.3.7.3: Continuous titrant addition): Titrant addition Control band [mV, A] V(min) [mL] 0.01 Esc 500.0 METHOD
OK
The titrator dispenses the titrant slowly at the start then at the maximum rate until the defined control band. Within the control range, the dispensing rate decreases exponentially. In the vicinity of the end point, the titrator adds the increment V(min) (see diagram in Section 3.3.7.3); the smallest increment that the titrator can dispense is 1/5 000 of the burette volume. For V(min) you can enter a formula instead of a number. The titrator measures the initial potential ET1 after 1 - 3 seconds and for the table of measured values it acquires a measured value every 5 seconds. The titrator can store maximum 300 measured values. If this limit is exceeded, it reduces the number of measured values by half by leaving only every second measured value in the memory. The new measured values continue to be acquired every 5 seconds. Note: The control band determines the control and the speed of the end point titration. To enter a "reasonable" value, you should perform an equivalence point titration with timedincrement measured value acquisition. Using the table of measured values of this titration, you can determine both the end point potential and the control band exactly.
3.3.10.5
End point
You enter the end point for the titration. End point Potential [mV, A] 100.0 METHOD
Esc
OK
Instead of a number, you can enter a formula or call up a potential stored as an auxiliary value.
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Method
EP titration (Ipol/Upol): Tendency/Termination
3.3.10.6
Tendency
A titration exhibits a positive or negative mV or A change. You have to define this. Tendency Tendency Negative METHOD
Esc
Modify
OK
Note: The tendency of a voltametric titration with a positive current intensity is negative, with a negative current intensity it is positive. The tendency of an amperometric titration with a positive voltage is positive, with a negative voltage it is negative.
3.3.10.7
Termination
You define the termination of a titration by selecting two resp. three parameters. Termination Maximum volume [mL] Delay [s] Maximum time [s] Esc 10.0 Yes No OK METHOD
Maximum volume You must define the volume. It is intended as a safety precaution: if the titration is faulty, an excess amount of titrant is not added unnecessarily. Delay is the time from attainment of the end point up to definitive termination of the titration. If the measured value of the end point decreases within the specified time, the titrator adds additional increments. Instead of or in addition to the delay time, you can also enter a time when the titration should be stopped. Enter a maximum time when, e.g. you perform a stating (see METTLER method 90016: Drift determination for KF titrations). If you define a value for both termination parameters, the titration will be terminated when one of the two values is reached. Note: If the titration is terminated because the maximum time has been reached, no end point will be calculated. VEND (VEX) is recorded as the raw result.
Maximum time
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pH/mV-stat
Method
3.3.11
pH/mV-stat
With the aid of this function you can perform a pH-stating. You determine the parameters which assure the constancy of a potential value, which lead to termination of the pH-stating and which are used for the evaluation. Titrant/Sensor Pretitration End point Tendency Termination Storage interval Evaluation The titrator determines the following raw results (see also 8.1: List of symbols): the titrant consumption in mL or mmol up to termination of the pH-stating. the titrant consumption in mL or mmol up to attainment of defined time limits. the mean titrant consumption in mL/min or mmol/min within the defined time limits. the correlation coefficient CSTAT, which results from calculation of the mean titrant consumption through linear regression. Notes 1. If you have selected a temperature sensor under the Sample function, the temperature of the sample solution is measured automatically before the titrator executes this function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature entered at the start of the method. The slope of the pH electrode is temperature-corrected by this measured or entered value and incorporated in the calculation of the pH value. 2. In the recording of a titration curve, you obtain only the actual pH-stating. You can follow the graphical plot of the pretitration only on the display. Titrant/Sensor To modify the titrant or the sensor, press <F4>: Titrant Concentration [mol/L] Sensor Unit of meas. NaOH 0.1 DG111 mV
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Method
pH/mV-stat
Titrant Concentration Sensor Unit of measurement
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. The defined measurement unit is entered automatically. If you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu, otherwise you will receive an error message when the method is started.
Pretitration Select the pretitration if the potential value of your solution differs from the value you need for the pH-stating: Press <F4> and select "Yes" in the mask that appears. Press <F4> and enter the control band [mV, pH, ...] in the mask that appears (see Section 3.3.7.3: EP titration, Titrant addition). End point End point Potential [mV, pH,...] Control band [mV, pH,...] Esc Potential 8 0.7 OK METHOD
The value you enter here is kept constant during the pH-stating. Instead of a number, you can enter a formula or call up a potential stored as an auxiliary value (see example in Section 3.3.7.4). The defined value controls the end point range: The lower the value, the faster the titrator reacts to a deviation from the potential of the defined end point. Help You can accept suggested values for the value of the control band: Press <F3> and confirm a value in the mask that appears with OK. For pH-statings whose end point lies in a steep control range, the control band must be larger than for statings whose end point lies in a flat control range.
Control band
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pH/mV-stat
Method
Tendency The tendency you have to define refers to the titrant which is added. The kinetics of the reaction determined by pH-stating are always in the opposite direction! Press <F4> and select "Positive" or "Negative" in the mask that appears. Termination You define the termination of the pH-stating by the following parameters: Maximum volume [mL] t(min) [s] t(max) [s] Minimum consumption [mL] Time span [s] 10 60 600 0.1 10
Maximum volume The entry is intended as a safety precaution: if the titration is faulty, an excess amount of titrant is not added unnecessarily. t(min) is the earliest time a termination can take place; it depends on the minimum consumption within the defined time range. is the time when the pH-stating should be terminated.
t(max)
Min. consumption The stating is terminated when not more than 0.1 mL titrant are consumed within 10 seconds (example of default parameters). Time span This condition can be effective at the earliest after 60 seconds [t(min)]. After 600 seconds [t(max)], the stating is terminated even if the condition is not met. Storage interval You define a time interval for storage of the measurement data. Press <F4> and enter the interval in the mask that appears. With the default value, the current measured value and the associated volume are stored after 10 s. The titrator can store and print out maximum 300 measured values. If the defined interval is too small, after 300 measured values the titrator first eliminates the values of the pretitration. If the limit of 300 measured values is then again exceeded, it reduces their number by half by leaving only every second measured value in the memory. The measured values continue to be stored at the defined interval.
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Method
pH/mV-stat
Evaluation The following parameters define the evaluation of the pH-stating: Evaluation Time limit t1 [s] Time limit t2 [s] Esc Time limit t1 Time limit t2 100.0 200.0 OK METHOD
The titrant consumption is calculated up to the defined times t1 and t2 (see Section 8.1: List of symbols). The time limits are not restricted to the values t1 and t2 entered here. In one of the additional Calculation functions, you can calculate, e.g. the mean titrant consumption within different time limits with R = QSTAT (100, 200). the titrant consumption up to a different time limit with R = VT (200). the correlation coefficient within a different time limit with R = CSTAT (300, 600). In this manner you can also define additional results with new time limits following a pH-stating (see Section 6.5.3: Perform calculations).
Example of the progress of a pH-stating with time
V/t [mL/s]
3 2
1: Pretitration 2: When the end point is reached, the titrator waits 5 s before sending an audio signal and the message "Pretitration complete: Please add sample!". The titrator continues to exert control and stir. 3: You enter your sample and confirm the message with OK: The titration starts. If you have to remove the titration vessel for addition, you can stop the stirrer during this time (see Section 6.2) 4: The termination condition of V/t is met, the pH-stating is terminated.
4 t [s] 1 t(min) t(max)
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Calculation
Method
3.3.12
Calculation
You can use this function to calculate one result R for every sample. Formula Constant Decimal places Result unit Result name Statistics Formula R=Q*C/m C=M/(10*z) 3 % No
Press <F4> to open the "List of formulas" and select a different formula or enter the one you need for your calculation (see also Section 8.4: Examples of formulas). Press <F4> to open the "List of constants" and select a different constant or enter the one you need for your calculation. Symbol You can select the symbols you need for your calculation from the list that appears by pressing <F3>. It contains all symbols possible for the individual functions (see also Section 8.1: List of symbols). You can link together all available parameters and numeric values. Example illustrating the entry of the formula "R=QSTAT(120,180)": - Press <F4> and accept "R=VSTAT(100,200)", - position the cursor on "V", delete it and select "Q" from the list, - replace "100" by "120", - skip the comma with the cursor and - replace "200" by "180". The following operations are available for calculations: on the keypad Addition: Subtraction: + in "List of formulas" Logarithmic function to base 10: Logarithmic function to base e: Exponential function to base 10: Exponential function to base e: Squaring function: Square root function: lg(x) ln(x) pw(x) ex(x) sq(x) sr(x)
Constant
Multiplication: * Division: /
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Method
Calculation
Decimal places Result unit Result name Statistics
Enter the number of decimal places you require in the result. Press <F4> to select the unit from the selection menu. You can enter the name with an attached keyboard. Use <F4> to select whether a statistical calculation should be performed. "Yes": in the analysis of a sample series the mean value x, the standard deviation s and the relative standard deviation srel are calculated and recorded.
Notes 1. Some standard methods include three Calculation functions. If you need only one result, delete the formula "Rn = ..." with CE. This skips the function when the method is processed. 2. For the calculation of a titration curve with 3 equivalence points (acidic mixture of 3 substances), you must define the parameters of the three Calculation functions.
E
R3
R2
R1
Q1
Q2
Q3
Formula 1st Calculation function: 2nd Calculation function: 3rd Calculation function: R1 = Q1 C1 / m R2 = Q2 C2 / m R3 = Q3 C3 / m
Constant C1 = M / (10 z) C2 = (60.01 1000) / 1 C3 = 53.5 / 1
Unit [%] [ppm] [mg/g]
Another example is the METTLER method 90001: In addition to the NaOH consumption in mL as a result, the acid content of HCl in mol/L and in g/L are calculated. 3. R and C are indexed according to the preset sequence. If you delete, e.g. the formula "R2 =...", 3 remains as the index for the third calculation if you do not change it yourself (see Section 8.2: Use of indices).
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Calculation
Method
4. You must enter the molar mass M and the equivalent number z of the 2nd and 3rd Calculation function as numeric values or insert as Hj if you have stored them as auxiliary values (see Section 2.5): M and z are defined in the Sample function for the calculation of the first equivalence point (see Section 3.3.2). 5. If you do not know the number of equivalence points, you can have Q recognized by a condition instead of defining indices for Q (see "List of formulas"). Example: R = Q (200 < EPOT < 300) means that the Q used for the calculation is that whose equivalence point potential lies between 200 and 300 mV. If the titrator detects more than one equivalence point in this range, it calculates the first (see also Section 8.4.3). 6. The titrator checks your entries when you quit the parameter mask with OK. If you have entered wrong formulas or constants, you immediately receive an appropriate error message, e.g. Error No. 3 Wrong formula Modify Terminate METHOD
OK Modify: You can change the entry. Terminate: The entry last stored reappears. If you have used raw results (e.g. R = QDISP) which the titrator can not determine as the method does not include the Dispense function, you do not receive an error message until the method is stored. 7. The titrator stores results until you start a new sample series or switch off the titrator (see also Section 8.5.6). 8. If you abort the method with Reset, an evaluation of the data obtained to date follows. If you were to abort the titration sequence (see point 2), e.g. shortly before the second equivalence point, you would receive result R1 but not R2 and R3 (see Section 5.2.4). 9. Under the auxiliary function Results, you can perform additional calculations after the titration of a sample (see Section 6.5.3) eliminate results (outliers) on completion of a sample series and thus modify the statistical evaluation (see Section 6.5.5).
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Method
Calibration
3.3.13
Calibration
You can use this function to calibrate an electrode: its zero point and its slope are calculated. You determine the buffers which you use for calibration of the sensor. The potential of the buffer solutions is acquired using the Measure function (see example in the Quick Guide). Notes 1. As the slope of an electrode depends on the temperature, it is important to incorporate the temperature in the calibration. Before the Measure function, the temperature of the buffer solution is measured automatically if you have attached a temperature sensor; otherwise, the temperature you entered before the start of the calibration is used (see Sample function, Sections 3.3.2 and 5.1). If you later measure the pH value of a solution at a different temperature, the slope of the sensor is temperature-corrected by the titrator. 2. The calibration data (zero point, slope and calibration temperature) are entered automatically with the date in the parameter mask of the sensor (see Section 2.2.2). 3. Depending on the number of buffer solutions measured, the titrator performs the following calibration: With one buffer solution, it calculates the zero point of the sensor. The slope remains unchanged. With several buffer samples, it calculates the zero point and the slope of the sensor by means of a linear regression through the measured points. You can modify the following parameters: Sensor DG111 Buffer type pH (DIN/NIST) Result R 1 Minimum slope [mV/unit] -55.0 Maximum slope [mV/unit] -65.0 Sensor Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. Press <F4> and select the type in the mask that appears: pH (DIN/NIST), pH (MERCK), pH (METTLER TOLEDO) or pH, pM, pX.
Buffer type
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Calibration
Method
Buffer type
The titrator has 8 values each for DIN/NIST, MERCK Titrisol and METTLER TOLEDO buffer solutions stored which you can select to calibrate pH electrodes. Under "pH, pM, pX (free selection)" enter values of userselected buffer solutions to calibrate pH or ion-selective electrodes (see Note 2). Example illustrating selection of pH values of a MERCK buffer. Press <F4> to display the selection menu: pH (MERCK Titrisol) First buffer Second buffer Third buffer Esc pH 4 pH 4 pH 4 Modify OK METHOD
If your first buffer solution does not have a pH value of 4, press <F4> (otherwise, select 2nd buffer): MERCK buffers pH 3 pH 4 pH 5 pH 6 Esc METHOD
OK
Select a different buffer value from this list, e.g. pH 3 and confirm with OK. In the "pH (MERCK Titrisol)" mask select the 2nd buffer and again press <F4> to select its pH value, e.g. pH 7 etc. Notes 1. The buffer values apply to a temperature of 25 C for DIN/NIST buffers 20 C for MERCK Titrisol buffers 25 C for METTLER TOLEDO buffers. If you calibrate at a different temperature, these buffer values are automatically temperature-corrected and recorded on the printout. If you calibrate at a temperature that lies outside the defined range for the corresponding buffer, "Temperature outside limits" appears in the report; however, the calibration data will be recorded.
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Method
Calibration
Buffer type
2. For the pH, pM, pX buffer values you can also enter formulas. 3. Positive ions result in a negative slope, negative ions in a positive slope.
Result R
"1" (result index): The measured values E of the buffer solutions used are stored under the first Calculation function: R1 = E (see Section 8.2: Use of indices). The titrator calculates the zero point and the slope of the electrode by linear regression by assigning the measured values to the standard concentrations of the buffer solutions. The index must thus be the same as under the Calculation function. Enter the minimum and maximum slope; the slope of an electrode is a measure of its quality. If you obtain a slope, e.g. with the pH buffer types in a pH calibration which lies outside the limits you have defined, the calibration data are not entered for the corresponding sensor. The error message "Data not transferred" appears on the report.
Minimum slope Maximum slope
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Titer
Method
3.3.14
Titer
Titer is an assignment function: The result R or its calculated mean value x of the titration of a titrant is assigned to the titer by t = R or t = x and automatically entered in the parameter mask of the titrant with the date (see Section 2.1.2 and the example in the Quick Guide). Titer Titrant NaOH Concentration [mol/L] Formula t = x Esc Titrant Concentration Formula t = METHOD
0.1 Modify OK
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to select from the selection menu: "x", if you determine the titer with more than one sample so that the calculated mean value is assigned to the titer. The statistical calculation must be selected in the Calculation function for this. "R" only if you determine the titer with a single sample.
Note: If you delete, e.g. one result of these titer determinations under the auxiliary function Results, the new calculated mean value will not be entered in the parameter mask of the titrant!
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Method
Auxiliary value
3.3.15
Auxiliary value
Auxiliary value is an assignment function. The result (R or Ri) or its calculated mean value (x or x [k]) or a raw result of the titration function is assigned to the auxiliary value Hj and entered automatically with the date in the parameter mask of the auxiliary value (see Section 2.5 and Section 8.2: Use of indices). 20 auxiliary value memories are available: H1 - H20. You can store, e.g. the following as auxiliary values: the blank value of a titration (example of the standard method: "Blank by EQP titration") a raw result that you obtain under the EQP or EP titration function, e.g. "H6 = VEQ". You can call up these auxiliary values in the Calculation function. Auxiliary value ID Formula Esc ID Formula Enter an identification if desired. Enter "H = R" or "Hj = Ri" if you determine the auxiliary value with a single sample. Enter "H = x " or "Hj = x [k]" only if you determine the auxiliary value with more than one sample so that the calculated mean value is assigned to the auxiliary value. The Statistics calculation must be selected in the Calculation function for this. You can also enter, e.g. "H (Hj) = VEND * 1.5" as a formula. Symbol If "Formula" is selected, you can open the list of symbols with <F3> (see also Section 8.1). Select the symbol from this list which should be assigned to the auxiliary value, e.g. for the formula "H6 = VEQ": - Position the cursor on "2", - replace "20" by "6", - position the cursor on "R" and delete "R1", - select "VEQ" from the symbol list. METHOD
H20=R1 OK
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Report
Method
3.3.16
Report
You use this function to determine what data should be recorded. Note: If your method contains two Titration functions, e.g. standard method "2 Step titrations (EQP)", a Report function also follows the first Titration function so that you can record, e.g. the table of measured values and titration curve of the first function. The reason for this is that the titrator stores only the measured values of the last Titration function. The titrator stores the raw results of all functions up to the determination of the next sample within a series (see Section 8.5.6). Report Output Printer Results All results Esc Output METHOD
Yes No Modify
OK
Use <F4> to select the unit(s) or card to which the data should be sent: Printer, Memory card (not with DL50), Computer, Printer + memory card (not with DL50) or Printer + computer. Printer is stored as the default parameter (for the printer you have defined, see Section 2.7.1). If you have not defined a printer and/or computer, the function can not be executed. This case neither initiates an error message nor does it influence the titration. If you have defined and switched on a printer, but this is set to "offline", the titrator waits until you switch the printer to "online" and then starts to transfer its data. If you have defined and attached a computer, but have not switched it on, an appropriate error message appears. If you have selected memory card but have not inserted one, an appropriate error message appears.
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Method
Report
Results
All results defined in the Calculation function are recorded for the current sample after every titration. Use <F4> to select "No" if you do not want a report. After the last titration of a sample series, the results of all samples are recorded if you select "Yes" with <F4>. These include the statistics, calibration, titer and auxiliary value data if the parameter or the functions have been defined in the method. After every titration the raw results such as VEQ or VDISP of the current sample are recorded if you select "Yes" with <F4>. After every titration the table of measured values of the current sample is recorded if you select "Yes" with <F4>. After the last titration of a sample series the sample data of all samples are recorded if you select "Yes" with <F4> (ID, molar mass, equivalent number, weight/volume, correction factor). After every titration the titration curve Potential vs Volume of the current sample is printed out if you select "Yes" with <F4>. After every titration the 1st derivative of the titration curve Potential vs Volume of the current sample is recorded if you select "Yes" with <F4>. The ordinate representation is linear. After every titration the 1st derivative of the titration curve Potential vs Volume of the current sample is recorded if you select "Yes" with <F4>. The ordinate representation is logarithmic. After every titration the 2nd derivative of the titration curve Potential vs Volume of the current sample is recorded if you select "Yes" with <F4>. The ordinate representation is linear. After every titration the titration curve Potential vs Time of the current sample is recorded if you select "Yes" with <F4>. After every titration the titration curve Volume vs Time of the current sample is recorded if you select "Yes" with <F4>. After every titration the 1st derivative of the titration curve Volume vs Time of the current sample is recorded if you select "Yes" with <F4>.
All results
Raw results
Table of measured values Sample data
E V curve
E/V V curve
log E/V V curve 2E/V2 V curve E t curve
V t curve
V/t t curve
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Sample
Contents
Page 4. 4.1 4.1.1 4.1.2 4.1.3 4.1.4 4.1.4.1 4.1.4.2 4.2 4.3 Sample data memory ................................................................................ Entering sample data ................................................................................ Deleting sample data ............................................................................... Printing sample data ................................................................................ Modifying sample data ............................................................................. Adding sample data ................................................................................. DL50/DL53 ............................................................................................... DL55/DL58 ............................................................................................... 4-3 4-4 4-6 4-7 4-7 4-8 4-8 4-8
Weight transfer from a balance ............................................................... 4-12 Requesting sample data from a computer ............................................. 4-13
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4-1
Sample
4.
Sample data memory
This menu is used for the entry and storage of sample data. You can enter weight or volume, identification, correction factor and temperature for maximum 60 samples. The data remain stored even if you switch off the titrator; data of analyzed samples, on the other hand, are deleted. The menu is always accessible during the analysis to allow the user to see which samples have already been titrated to modify or delete data of samples not yet analyzed to enter data for additional samples. The performance of the four titrators differs in this menu as follows:
DL50/DL53: You can enter data for only one sample series. DL55/DL58: You can enter data for three sample series; these series can be run with the same method or with three different methods. You can enter the data of a so-called urgent sample.
With the Run key, method(s) and sample data are called up automatically and analyzed in succession by the titrator (see Section 5).
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Sample
4.1
Entering sample data
When you press the Sample key, the (blank) sample data list appears: No. Status Wt/vol. Meth. ID
Add Add New sample series New sample series (data: computer)1) Esc
1)
SAMPLE
OK
appears if you have defined and attached a computer (see Section 4.3).
Sample entry Number of samples Method ID User Esc Number samples Enter, e.g. 3. Method ID 1 00001
SAMPLE
OK
Enter, e.g. 00001 (example for the standard method "Equivalence point titration", see Section 5.1): This calls up the method to be used for analysis of the samples. If you do not know the identification of the method, press <F4> "Modify": The method groups appear. Confirm either user or METTLER methods: The list of these methods appears. Confirm the method you need for the analysis. Enter your name if a keyboard is attached to the titrator.
User
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Sample
Note: The titrator also accepts methods stored on an inserted memory card or in an attached computer: When you enter an identification whose method is not stored in the titrator, the method is first searched for on the memory card and entered (not possible with the DL50). If the method is not stored on the card, it is requested from the computer and entered (see Operating Instructions: Computer Interface Description). Press <F5> to show the sample data mask (weight entry as example): Sample No. 1 Sample ID Weight [g] 0.0 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Esc SAMPLE
Balance* OK
* "Balance" appears if you have defined a balance in the Setup menu.
Sample ID
Enter or modify or delete if you have already defined the identification in the Sample function (Section 3.3.2). Enter or transfer from an attached balance (see Section 4.2). If you can not enter the weight or volume until during the titration, e.g. as you do not wish to lose time through back weighing, do not enter anything: As the titrator does not need the sample data until it starts to calculate, the sample data mask appears again in the display during the titration (see Section 5.1). You can also enter the weight during the titration in the sample data memory (see Section 5.2: Sequence of a pH-stat titration). If you have defined a fixed volume in the Sample function, no change is possible. If you have violated the lower or upper limits of the weight/volume, but still confirm this entry, the following appears: Entry outside limits Modify entry Save entry OK Modify: The sample data mask reappears. Save: The weight is transferred. The sample data mask for the next sample or the sample data list appears. SAMPLE
Weight (Volume)
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Sample
Limits
You can not change the limits. These data do not appear if you have defined a fixed volume in the Sample function. You can enter a value for every sample that is reconciled in the calculations if you enter f in the formula of the Calculation function. Example: Each substance has a different, known moisture content whose value you can insert for f: 1st sample: Moisture content = 4% f = 0.96 R = Q * C/(m * f) 2nd sample: Moisture content = 3% f = 0.97 R = Q * C/(m * f) Enter the temperature of the solution to be titrated. You can not change the value if you have defined a temperature sensor in the Sample function.
Correction factor
Temperature
When you confirm the entries, the sample data mask for the second and the third sample appears, followed by the sample data list: No. 2 3 Status ready ready Wt/vol. 1.23454 1.67115 Meth. 00001 00001 ID 45321 45322
Delete
Print
Modify
Add
4.1.1
Deleting sample data
When you press <F2>, the following appears: Delete sample(s) Selected sample Sample series Esc Selected sample OK SAMPLE
The sample highlighted by the selection bar when you confirmed "Delete" is deleted. DL50/DL53: All entered data are deleted. DL55/DL58: All data of the sample series which contains the sample highlighted by the selection bar when you confirmed "Delete" are deleted.
Sample series
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Sample
Notes 1. You can not delete sample data of a series which are done until all defined samples have been analyzed. When you then press <F2>, you can delete only the series. 2. If the titrator is controlled by a computer, you can not delete the sample data (see Section 6.8.3).
4.1.2
Printing sample data
A list of all sample data contained in the sample data memory is printed out.
4.1.3
Modifying sample data
The sample data mask of the selected sample appears. As long as the sample is ready, you can modify all parameters. If the sample is being titrated, in other words is active, you can modify the parameters as long as the weight/volume of the sample has not yet been used for the calculation. When the sample is titrated, in other words ready, you can not modify any parameters.
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Sample
4.1.4 4.1.4.1
Adding sample data DL50/DL53
You add data of a new sample to the existing data of a sample series: Add Sample to series1) SAMPLE
Esc
1)
OK
If you have transferred the existing data from a computer, "Sample to series (data: computer)" appears, see Section 4.. If the series has been processed, "New sample series" also appears.
Sample to series
The sample data mask for sample No. 4 of method 00001 appears (example in Section 4.1.1). As long as you do not delete the data of a series classed as done, you can add data for a new sample to the series. The data of a processed series are deleted when you switch off the titrator select "New sample series" in place of "Sample to series" modify the method used to run the series.
4.1.4.2
DL55/DL58
You either add the data of an additional sample or that of a new series to the existing data of a series. The series are processed by the titrator in the defined sequence. Add New sample series New sample series (data: computer)1) Sample to series Esc
1)
SAMPLE
1) OK
appears when you have defined and attached a computer (see Section 4.3). If you have transferred existing data from the computer. "Sample to series (data: computer)" also appears scroll display
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Sample
New sample series
You can add maximum two additional series to an existing series. Before the first sample series (possible only if its method has not yet been started): No. Status Wt/vol. Meth. ID
1 2
ready ready
1.36182 1.23454
00001 00001
45320 45321 Add
Select the blank line above the first sample and press <F5>: The "Add" mask appears (see above and the sequence in Section 4.1). Between two sample series No. 2 3 1 2 Status ready ready ready ready Wt/vol. 1.23454 1.67115 5 5 Meth. 00001 00001 2 2 ID 45321 45322
Add
Select a sample data line of the first series and press <F5> : The "Add" mask appears (see above and sequence in Section 4.1). After the last sample series Select a sample data line of the last series and press <F5>: The "Add" mask appears. Sample to series The sample data mask for sample No. 4 of method 00001 appears (example in Section 4.1.1). You can add samples to a completed series before the titrator starts to process the next series, in other words before you confirm the result list of the last sample with OK. As soon as you have confirmed the result list of the last sample of a series, all its data are deleted when the next series is defined. You can then enter the data for a new sample series.
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Sample
Urgent sample If you have to analyze one sample immediately while a sample series is being processed by the DL55/DL58, you can insert this after the active series sample. The sample series is interrupted and then continued after the determination. Example: The titrator is processing sample 2 of method 00001. Press the Sample key and select the active sample: No. 1 2 3 1 Status done active ready ready Wt/vol. 1.36181 1.23454 1.67115 5 Meth. 00001 00001 00001 2 ID 45320 45321 45322 Add Add New sample series1) Sample to series Urgent sample Esc
1)
SAMPLE
OK
appears if three series have not yet been defined.
Confirm "Urgent sample" with OK. Sample entry Number of samples Method ID User Esc 1 00001 OK SAMPLE
Number samples You can not modify these: You can determine only one urgent sample at a time! Method ID Enter the identification of the method which should be used to determine the sample. Enter your name if a keyboard is attached to the titrator.
User
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Sample
After entry and confirmation of the sample data, the following appears: No. 1 2 EX 3 Status Wt/vol. Meth. ID done 1.36181 00001 45320 active 1.23452 00001 45321 ready 0.41894 8 ready 1.67115 00001 45322 Delete Print Modify
Add
When sample 2 is done, method 8 for the urgent sample is called up (see Section 5.4: Running sample series). When the urgent sample is done, method 00001 for sample 3 is called up. The data of the urgent sample are deleted. Note: When a defined sample series has been analyzed and you confirm the Add command to add a sample to the series, "Urgent sample" is also available in the mask that appears (see previous page).
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Sample
4.2
Weight transfer from a balance
If you have attached a balance to the titrator, you must have defined this in the Setup menu. If not, "Balance" does not appear in the sample data mask. Sample No. 1 Sample ID Weight [g] 0.0 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Esc SAMPLE
Balance OK
When you press <F4>, the value displayed on the balance appears, e.g. Weight: > 1.36181 SAMPLE
Esc
OK
The weight is transferred with OK. If the weight violates the lower limit, three minus signs ( ) always appear after "Weight", if it exceeds the upper limit three plus signs (+ + +) appear. You can change or confirm the weight (see Section 4.1: Weight parameter). With METTLER TOLEDO balances which have a key to transfer the weight, you can enter the weight values for a sample series from the balance without pressing a key on the titrator. The setting "Bidirectional transmission mode" is required for this. Some balances show the sample number, others also show weight limits (DeltaTrac). With weight "0.0" in the first sample data mask, press <F4>. Press the TARE key of the balance to display the current weight. Activate the weight transfer with the appropriate key of the balance: The weight is entered in the sample data mask; at the same time, the titrator automatically starts the weight entry for the next sample.
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Sample
4.3
Requesting sample data from a computer
If you have loaded the DLWin or the LabX titration software or an appropriate program on the attached computer, you can request the sample data stored on it. With the "Add" command, the following appears automatically: Add New sample series New sample series (data: computer) SAMPLE
Esc Series entry ID User Esc ID
OK SAMPLE
OK
You enter the identification of the sample series stored in the computer. This is transferred to the sample data memory with OK. These sample data can only be printed out or displayed ("Modify" command). Enter your name if a keyboard is attached to the titrator. Note: For reports which are sent to the printer, the computer and the memory card, the name entered in the titrator is always adopted, the name entered in the computer is adopted if you do not enter a name in the titrator.
User
If you wish to add the data of a new sample to a series transferred from the computer, confirm "Sample to series (data: computer)" in the "Add" mask with OK. The sample data are added to the sample data list. You will find further information in the Operating Instructions for the computer interface or the DLWin or LabX titration software.
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Run
Run
Contents
Page 5. 5.1 5.2 5.2.1 5.2.2 5.2.3 5.2.4 5.3 5.4 Analysis ..................................................................................................... Menu sequence up to insertion of the sample ....................................... Analysis sequence of a sample ............................................................... Fading out analysis ..................................................................................... Analysis is interrupted ................................................................................. Modifying method of the current sample series .......................................... Aborting analysis ......................................................................................... 5-3 5-4 5-7 5-11 5-11 5-12 5-12
DL55/DL58: Modifying ongoing method ................................................ 5-13 DL55/DL58: Running sample series ........................................................ 5-15
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Run
Run
5.
Analysis
You perform titrations with a selected method. The data required for this are stored in the Method and Setup menus. You prepare your sample, titrate it and receive the result. You enter the sample data such as weight or volume directly before the start of each sample determination. These data are also entered in the sample data memory. To modify them during the titration or to add samples to a defined sample series, you can open the Sample menu. While a method is running, you can call up the auxiliary functions "Stirrer" and "Results"; all other auxiliary functions and the Setup and Method menus are blocked. In this menu, the functions of the Run and command key <F5> are identical, in other words you can press one or other key. The performance of the four titrators differs in this menu as follows:
DL50/DL53:
One titration curve is displayed (EQP/EP titration: Potential vs. Volume, pH/mV titration: Potential vs. Time). Seven titration curves for the display can be selected. You can interrupt the analysis of a sample to modify parameters of the ongoing method.
DL55/DL58:
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Menu sequence
Run
5.1
Menu sequence up to insertion of the sample
When you press the Run key, there are two possibilities for the display (as an example of the representation, the standard method "Equivalence point titration" is used. This has been changed for the determination of CaCl2 and stored with the identification 00001): No data in sample data memory: All sample data in sample data memory (see Section 4.1):
RUN Samples to be analyzed 3 samples, Method 00001 RUN
Samples to be analyzed Number of samples Method ID User 3 00001
Start
Delete
Start
Defined are Stirrer 1: Stand 1 Sensor 1: DM141 Drive 2: 0.1 mol/L AgNO3 Esc Print
RUN
Defined are Stirrer 1: Stand 1 Sensor 1: DM141 Drive 2: 0.1 mol/L AgNO3 Esc Print
RUN
OK
OK
Sample No. 1 Sample ID 45320 Weight [g] 1.23452 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance* * "Balance" appears, if you have defined a balance in the Setup menu Current sample
RUN
Current sample
RUN
No. 1 of 3
Sample ID Method ID
45320 00001 OK
OK
RUN
No. 1 of 3
Sample ID Method ID 45320 00001 OK
The Stir function is being processed
Notes 1. If you have defined an expiry date for the titrant and this has lapsed, an appropriate message follows the "Defined are" mask. In order to determine a titer before the sample analysis, you can confirm the message with Esc. 2. When the sample data mask or that of the "Current sample" appears, the sample is active in the sample data memory. The titrator executes the Sample function of the method and starts to acquire the time for every determination as the raw result TIME (see Section 5.2: Example of an analysis sequence and Section 8.1: List of symbols).
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Run
Menu sequence
3. The titrator also accepts methods which are stored on an inserted memory card or in an attached computer: When you enter an identification whose method is not stored in the titrator, the method is first sought on the memory card and entered (not possible with the DL50). If the method is not stored there, it is requested from the computer and entered (see Operating Instructions: Computer Interface Description). Mask: Samples to be analyzed Number samples Enter, e.g. 3; this enters a sample series. Method ID Enter, e.g. 00001: This calls up the method which should be used for analysis of the samples. If you do not know the identification of the method, press <F4> (Modify): The method groups appear. Confirm either user or METTLER methods: The list of these methods appears. Confirm the method you need for the analysis. Enter your name if a keyboard is attached.
User
Delete If, e.g. you have called up a method which you do not wish to use for the analysis, you can delete it. You have this possibility available with direct start if you confirm the "Defined are" mask with Esc (see page 5-4). Mask: Defined are This mask appears so that you can check whether you have attached the resources required by the method. You can exclude the mask from the sequence (see Section 6.7.3). If you have not defined a resource or there is no RS or sensor option available for the defined resource, an appropriate error message appears. Mask: Sample No. 1 (sample data mask) This mask does not appear if you have defined "Fixed volume" as entry type in the Sample function have not defined a predispensing to "factor x sample size" in the EQP/EP titration function have defined results such as "R = Q" in the Calculation function(s) which do not require the sample size m.
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Menu sequence
Run
If you still have to enter sample data such as the temperature for buffer solutions to be measured in a sensor calibration, you can do this for every sample in the Sample menu (see Section 4.1). Sample ID Enter or modify or delete if you have already defined the identification in the Sample function (see Section 3.3.2). Enter or transfer from an attached balance (see Section 4.2). If you can not enter the weight or volume until during the titration as, e.g. you do not wish to lose time through back weighing, do not enter anything. As the titrator does not need the sample size until it performs calculations, the sample data mask appears again in the display during the titration: either when the titrator reaches the EQP/EP titration function under which a predispensing to (factor x sample size) has been defined or when it reaches the Calculation function under which the sample size m is needed for the result. You can also enter weight/volume in the Sample menu (see Section 5.2: Example of a pH-stating). If you violate the upper or lower limits of the weight/volume but still confirm the entry, an appropriate message appears (see Section 4.1). You can not change the limits. This information does not appear if you have defined a fixed volume in the Sample function. You can enter a value for each sample which is reconciled in the calculations if you insert f in the formula of the Calculation function (see Section 4.1). Enter that of the solution to be titrated. You can not change the value if you have defined a temperature sensor in the Sample function.
Weight (Volume)
Limits
Correction factor
Temperature
Mask: Current sample If you work with a sample changer, in other words you have defined "ST20A" as a titration stand, the mask always appears, but is confirmed automatically (no OK command). If you have defined "Auto stand" as the titration stand, the mask does not appear as a system, e.g. a robot undertakes insertion or changing of the sample.
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Run
Analysis sequence
5.2
Analysis sequence of a sample
1st example: Method 00001 (see Section 5.1)

Sample No. 1 Sample ID 45320 Weight [g] 1.23452 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance Current sample RUN
OK RUN
The titrator starts to process the method with the Sample function. ( Enter ID.) Weigh in sample, enter the weight for the first sample or have it transferred from a balance. ( Enter correction factor and temperature.) Press <F5> or the Run key. Before you confirm this mask, fix the sample beaker to the titration stand.
No. 1 of 3
Sample ID Method ID 45320 00001 OK Stir function Wait time [s] Speed [%] 30 80 Hold1)
mV
RUN
The titrator stirs with 80% of the maximum speed for 30 seconds (CaCl2 dissolves during this time). The elapse of time is displayed.
1) appears only with the DL55/DL58 (see Section 5.3)
E V curve
The titrator executes the EQP titration function.
mL
Table Result list Method: 00001 Sample 1 R1 = 29.26 %
Values
Curve1)
Hold2) RUN
1) 2)
appears only with DL55/DL58 (see next page) appears only with DL55/DL58 (see Section 5.3)
After the last method function, in other words before the result list appears, the titrator ends the time acquisition for this sample determination (see Note 2, Section 5.1): The sample is present in the sample data memory as done.
OK Sample No. 2 Sample ID 45321 Weight [g] 1.08723 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance Current sample RUN
The sample data mask for the second sample appears: Procede as described under sample 1.
OK RUN
You are "prompted" to insert the second sample etc.
No. 2 of 3
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Analysis sequence
Run
At the end of the series, the results of all samples appear in the display. If you confirm this result list, the mask "Samples to be analyzed" again appears. The method used to perform the last titration is entered as method. In the sample data memory, all samples of this series are present as done. You can now add samples to this series here (see Section 4.1.4). As soon as you start a new series or an individual sample, all data of the executed series will be deleted.
Notes 1. Changing stirrer speed During a titration you can always activate the Stirrer key to change the stirrer speed (see Section 6.2). 2. Method with two different titrants/sensors If, e.g. you have to use two titrants for a back titration and have only one burette drive, the following message (example) appears: Change resources Drive 2: 0.1 mol/L HCl RUN
OK If you have to use two sensors to, e.g. set the pH before the actual determination with a phototrode and have only one sensor option, "Sensor 1: DP660" appears. The message always appears before the function in which the second resource is needed. 3. DL55/DL58: Curve display During the EQP/EP titration or EQP/EP titration (Ipol/Upol) or pH/mV-stat function, the command <F4> (Curve) remains active if the curve representation has been selected. You can select the following curves for the display: E V curve Potential vs. Volume E/V V curve 1st derivative (Potential vs. Volume) log E/V V curve 1st derivative (Potential vs. Volume, logarithmic) 2E/V2 V curve 2nd derivative (Potential vs. Volume) E t curve Potential vs. Time V t curve Volume vs. Time V/t t curve 1st derivative (Volume vs. Time)
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Run
Analysis sequence
4. Result list a. During a titration, you can always activate the Results key to view the results generated to date (see Section 6.5.1). b. All results of a learn titration are marked in the display by an exclamation mark(!). c. With a sample series, the titrator skips the list for each sample you have excluded from the analysis sequence (see Section 6.7.3). d. With a sample series, all menus and auxiliary functions between the individual determinations are again accessible if you do not confirm the result list of the sample. You can then, e.g. also modify the method used to analyze the samples of this series (see Section 5.2.3). This is no longer possible if you exclude the "Result list for each sample" from the sequence (see point c.).
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Analysis sequence
Run
2nd example: pH-stating This sequence of a pH-stating in which the titrator should start the titration immediately after sample addition shows the entry of the sample data in the Sample menu during the titration:
Sample No. 1 Sample ID 592 Weight [g] 0.0 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance RUN
The titrator executes the Sample function. Confirm the sample data mask without entering the weight.
OK
Current sample
RUN
Add the sample and immediately confirm with OK.
No. 1 of 5
mV
E t curve
Table
Values
Curve1)
Hold2)
The titrator starts the pH-stating (the Stir function does not appear as the stirring time is defined with 0 (zero). 1) appears only with DL55/DL58 (see page 5-8) 2) appears only with DL55/DL58 (see Section 5.3)
Press
No. 1 2 3
Sample
Status active ready ready Wt/Vol. 0.0 0.0 0.0 Meth. ID
The sample data list appears.
33 592 33 593 33 594 Print Modify
Add
Sample No. 1 Sample ID 592 Weight [g] 0.1456 Limits [g] 0.02 - 2.0 Correction factor f 1.0 Balance
SAMPLE
The sample data mask appears. Enter the weight.
OK
Press
mV
Run
E t curve
If the pH-stating is not yet complete, the E - t curve of the pH/mV-stat function is again displayed. Otherwise, the function executed by the titrator appears.
s
Table
Values
Curve
Hold
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Run
Analysis sequence
5.2.1
Fading out analysis
During the titration you can enter sample data: press the Sample key (see Section 4.1 and example on previous page) change the stirrer speed: press the Stirrer key (see Section 6.2) view all results generated to date: press the Results key (see Section 6.5.1). The titration continues to run in the background. To display it again, press the Run key: The display shows the method function which is currently being executed by the titrator.
5.2.2
Analysis is interrupted
The titrator immediately interrupts an analysis in the following situations: 1. After the Learn titration function if it has not found any equivalence points (see Section 3.3.8). Confirm the error message: The representation of the Titration function shown before the interruption appears in the display (see example below). If you wish the titrator to execute the remaining functions of the method, press <F5>, "Proceed": The titrator executes the remaining functions. 2. At the immediate end of an EQP titration or EQP titration (Ipol/Upol) function when the condition for the defined parameter Stop for reevaluation is met (see Sections 3.3.6.7 and 3.3.9.8). The following display appears: Reevaluation required EQP titr. [1] neq=0 Confirm with OK and perform reevaluation (RESULTS) OK
(Example)
RUN
Measured values
RUN
6.789 265.9
mL mV
Table Curve Proceed
You can now confirm "Proceed" (the analysis is continued) or press the Results key to perform the reevaluation, see Section 6.5.2.
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Analysis sequence
Run
Note: If a method is interrupted which is not stored in the titrator but has been requested from the computer or a memory card, a reevaluation is not possible (see Section 5.1: Note 3 and Section 6.5.2).
5.2.3
Modifying method of the current sample series
After every sample determination, you can modify the method used to perform the series. A requirement is that you do not exlude the "Result list for each sample" from the analysis sequence (see Section 6.7.3). If you wish to modify the functions of the method, all parameters of the Sample function are blocked with the exception of the numeric parameters you have defined for the ST20A titration stand. with all other functions you can change only the numeric parameter values. When you save the method, the printer automatically records the complete method with the modified values: these remain stored for the method. To continue the sample series, press the Run key twice: The prompt to insert the next sample appears. Note: You can not change a method which is not stored in the titrator but is requested from the computer or the memory card.
5.2.4
Aborting analysis
If you wish to abort the sample which is currently being titrated, press the Reset key. The mask "METTLER TOLEDO/DL5x/Version x.x" appears. If you abort the sample at a time at which a result has already been calculated this is displayed in the result list (auxiliary function "Results"). If no result has been calculated, only the sample number will be listed. Individual sample The sample is present in the sample data memory as done and is deleted as soon as you start the analysis of a new sample. Sample series A series is not aborted with Reset: The sample is present in the sample data memory as done. With Run the display for the remaining samples of the series appears (example): Samples to be analyzed 2 samples, Method 00001 RUN
Delete
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Start
08/2004
Run
DL55/DL58: Modifying ongoing method
5.3
If you confirm "Hold" during a sample determination, the titrator stops the function it is currently executing. You can then modify the method used to analyze the sample: - Press the Method key (example): Methods Method ID 00001 METHOD
Print Notice Parameters that you can not modify are blocked.
Modify METHOD
OK With OK the functions of the interrupted method appear. All parameters of the Sample function are blocked with the exception of the numeric parameter values you have defined for the ST20A titration stand. With all other functions you can modify only the numeric parameter values. If you save the method, the printer automatically records the complete method with the modified values; these remain stored for the method. To continue the sample series, press the Run key: The representation shown before the interruption appears in the display. Press the Run key or <F5>: The analysis sequence is continued. In the case of an interrupted sample determination, the modifications apply only to the functions which the titrator has not yet started to execute. Exceptions are the Stir, EQP/EP titration, EQP/EP titration (Ipol/Upol) and pH/mV-stat functions. 1st example: Stir function If you interrupt the method at this function, you can modify not only the stirring and wait times, but also the rotational speed. On continuation of the determination, the titrator adds the difference between the defined and modified times to the stirring time remaining: the entire stirring time corresponds to the modified time and stirs at the modified speed.
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Run
2nd example: Dispense function If you interrupt the method at this function, change the volume and then continue the determination, the new volume is not added until the next sample determination. 3rd example: EQP titration function If you interrupt the method at this function, you can modify, e.g. the value for the maximum volume or the potential value for termination of the titration if this termination parameter is defined within the method. On continuation of the method, the titrator executes the modified parameters of the EQP titration. 4th example: pH/mV-stat function If you interrupt the method at this function, you can modify, e.g. the value for the control band, the volume for the minimum consumption or the time for the defined termination criteria. On continuation of the method, the titrator executes the modified parameters of the pH-stat function. Note: You can not modify a method which is not stored in the titrator but is requested from the computer or the memory card (see Section 5.1: Note 3).
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Run
DL55/DL58: Running sample series
5.4
You can store three sample series in the sample data memory of the DL55/DL58. These are processed in this menu by the titrator in sequence with your help. An attached sample changer automates this procedure. You can check the ongoing method in the Sample menu (see Section 4). As soon as the next sample series is started, all data of the executed series are deleted. At the end of the processed sample series, only the data of the last series remain stored. They are deleted as soon as you start the determination of a new sample or series. With all titration stands, the sample data mask appears only if you have not entered the weight (volume) for the samples before the start of the method. If you work with titration stand 1, 2 or an external stand, you must confirm the mask "Current sample" for every sample. If you have attached a sample changer, the titrator titrates the samples of all measurement methods without the need for your intervention. A requirement is that you have entered all sample data you have excluded the mask "Defined are" from the analysis sequence (see Section 6.7.3) the methods use the same resources or their setup data are defined at the other drive (titrants), at a different sensor option (sensors) or at the other ST20A output (solvents) (see comparison of the titration sequences on the following page). If you work with the auto stand, the mask "Current sample" does not appear, in other words each sample determination is started without confirmation. As a result, you can attach a robot to handle sample changing. The same prerequisites hold for the automatic running of sample series as for the use of the sample changer. Note: All information concerning automation in this titrator's Reference Handbook relates to the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear in some places. Operation of other METTLER TOLEDO sample changers via your titrator is described in the corresonding Operating Instructions.
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Run
Comparison of the analysis sequences for three sample series at the ST20A titration stand or at stand 1, 2 or the external stand. (The masks "Defined are" and "Result list for each sample" are excluded from the sequence for stand 1/2/external.)
Samples to be analyzed 3 samples, Method 00001 6 samples, Method 2 10 samples, Method 8 Delete RUN RUN
ST20A
Current sample
Start
Stand 1/2/external
RUN
Current sample
No. 1 of 3
Sample ID Method ID 45320 00001
No. 1 of 3
The mask "Current sample" appears for every sample, but is confirmed automatically. The titrator titrates all samples of method 00001. It then starts to titrate the samples of method 2 (the setup data are the same as for method 00001). It then starts to titrate the samples of method 8 (the setup data are the same as for method 00001). At the end of all sample determinations of method 8, the following appears:
Result list Method: 8 Sample 1 R1 = 97.386 % Sample 2 RUN
The titrator titrates all samples of method 00001. At the end of the 3 determinations, the following appears:
Result list Method: 00001 Sample 1 R1 = 29.26 % Sample 2 RUN
OK
Current sample
RUN
No. 1 of 6
The titrator titrates all samples of method 2. At the end of the 6 determinations, the following appears:
OK Result list Method: 2 Sample 1 R1 = 4.234 mmol R2 = 2.31 g/L RUN
OK
Current sample
RUN
No. 1 of 10
The titrator titrates all samples of method 8. At the end of the 10 determinations, the result list with the results of all samples of this method appears (see mask in ST20A column). 5-16
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Run
If the titrator has to process methods which have the same burette drives or sensor inputs in succession on the sample changer, you have to intervene:
Samples to be analyzed 4 samples, 7 samples, Delete Method 00001 Method 111 Start RUN
Current sample
RUN
No. 1 of 4
Sample ID Method ID 45320 00001
The titrator titrates all samples of method 00001. It then starts to execute the functions of the first sample of method 111: a different titrant and a different sensor are required. The following message appears before the Titration function in which the titrant and the sensor are defined:
Change resources Drive 2: 0.1 mol/L EDTA Sensor 1: DP660 OK RUN
Place the burette with the EDTA solution on burette drive 2 and attach the DP660/DP5 Phototrode to sensor input 1 (pH option in slot 1) and plug into titration stand.
If you confirm the message, the titrator executes the remaining functions of the method, it then titrates the other samples. At the end of the 7 determinations, the result list with the results of all samples of this method appears. The mask "Current sample" appears for every sample, but is confirmed automatically.
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Auxiliary functions
Contents
Page 6. 6.1 6.1.1 6.1.2 6.1.3 6.1.4 6.2 6.3 6.3.1 6.3.2 6.3.3 6.4 6.4.1 6.4.2 6.4.3 6.4.4 6.4.5 6.4.4 6.4.6 6.5 6.5.1 6.5.2 6.5.3 6.5.4 6.5.5 6.6 Auxiliary functions .................................................................................... Sensor ........................................................................................................ Measure potential........................................................................................ Measure temperature .................................................................................. Calibrate temperature sensors .................................................................... Measure voltage/current (Ipol/Upol) ............................................................ Stirrer ......................................................................................................... 6-3 6-4 6-4 6-5 6-6 6-7 6-8
Sample changer ........................................................................................ 6-9 Change lift position ...................................................................................... 6-9 Rotate turntable ........................................................................................... 6-9 Dispense/rinse ............................................................................................ 6-10 Burette ........................................................................................................ Rinse burette ............................................................................................... Rinse tip ...................................................................................................... Dispense ..................................................................................................... Dispense continuously ................................................................................ Titrate manually ........................................................................................... Dispense continuously (Ipol/Upol) ............................................................... Titrate manually (Ipol/Upol) ......................................................................... Results ....................................................................................................... Display result list ......................................................................................... Perform reevaluation ................................................................................... Perform calculations .................................................................................... Display measured values ............................................................................ Modify statistics ........................................................................................... 6-11 6-11 6-12 6-12 6-13 6-14 6-15 6-16 6-18 6-18 6-18 6-20 6-21 6-22
Report ......................................................................................................... 6-24
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Auxiliary functions
Page 6.7 6.7.1 6.7.1.1 6.7.1.2 6.7.1.3 6.7.1.4 6.7.1.5 6.7.1.6 6.7.2 6.7.3 6.7.4 6.7.5 6.7.6 6.8 6.8.1 6.8.2 6.8.3 6.8.4 Miscellaneous ............................................................................................ Define titrator settings ................................................................................. Date/time format .......................................................................................... Date/time ..................................................................................................... Language .................................................................................................... Report header ............................................................................................. Titrator ID .................................................................................................... Audio signal ................................................................................................. Adjust measuring inputs .............................................................................. Shorten analysis sequence ......................................................................... Define user level ......................................................................................... Activate control input ................................................................................... Activate control output ................................................................................. Data transfer .............................................................................................. Memory card ............................................................................................... Computer .................................................................................................... Remote control ............................................................................................ Bar-code string ............................................................................................ 6-26 6-26 6-26 6-27 6-27 6-27 6-27 6-28 6-28 6-30 6-31 6-32 6-33 6-36 6-36 6-40 6-42 6-43
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Auxiliary functions
6.
Auxiliary functions
You can use these symbol keys to perform the activities mentioned below. These auxiliary functions are independent of a titration method, but they can support or supplement a method. While a titration is running, you can activate only the functions of the Stirrer and Results keys, all other keys are blocked. Measure potential or temperature of a solution Calibrate temperature sensors Measure voltage/current (Ipol/Upol) Switch stirrer on or off, change stirrer speed
Stirrer
Sensor
Operate sample changer manually

Changer
Burette
Rinse burette and burette tip Dispense a specified volume Dispense continuously Titrate manually Dispense continuously (Ipol/Upol) Titrate manually (Ipol/Upol) Display result list of all samples of a series Modify evaluation of an EQP titration Perform additional calculations of the sample last titrated Display measured values of the sample last titrated Modify statistical evaluation of the series last titrated
Results
Report
Misc.
...
Data Transfer
08/2004
Print out additional reports of the series last performed or sample last titrated Define date and language Enter calibration data of the measuring inputs Modify analysis sequence Change user level Activate control inputs and outputs
Copy data from titrator to the memory card and vice versa (not possible with DL50) Transfer data from the titrator to the computer Select whether titrator should be controlled by the computer Enter bar-code string (computer transfer)
6-3
Sensor
6.1
Sensor
When you press the Sensor key, the following auxiliary functions appear: Measure potential Measure temperature Calibrate temperature sensors Measure voltage/current (Ipol/Upol)
6.1.1
Measure potential
You can measure the potential of solutions (mV, pH, %T, etc.). Sensor Unit of meas. Titration stand Speed [%] Temperature [C] Temperature sensor Report t [s] Sensor Unit of measurement DG111 mV Stand 1 50 25.0 Manual No 5
Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. The defined measurement unit is entered automatically. You can select a different measurement unit from the selection menu (press <F4>). Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Enter the temperature of the solution to be measured if you have not attached a temperature sensor. Press <F4> to select: Manual, TEMP A, TEMP B, TEMP C or TEMP D. Use <F4> to select "Yes" if desired: A measured value will be recorded every 5 seconds if you accept the time interval of "5".
Titration stand
Speed
Temperature
Temp. sensor Report t [s]

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Sensor
You can start and stop the measurement with <F5>. Start: The titrator starts to measure the potential of the solution. The measured values are shown in the display and are recorded. During the measurement, all other keys are blocked.
6.1.2
Measure temperature
You can measure the temperature of solutions (C, F or K). Temperature sensor Unit of meas. Titration stand Speed [%] Report t [s] Temp. sensor Unit of meas. Titration stand TEMP A C Stand 1 50 No 5
Press <F4> to select: TEMP A, TEMP B, TEMP C or TEMP D. Press <F4> to select: C, F or K. Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Press <F4> to select "Yes" if desired: A measured value is recorded every 5 seconds if you accept a time interval of "5". Start and stop the measurement with <F5>. Start: The titrator starts to measure the temperature of the solution. The measured values are shown in the display and are recorded. During the measurement, all other keys are blocked.
Speed
Report t [s]
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Sensor
6.1.3
Calibrate temperature sensors
You can calibrate your Pt100 or Pt1000 sensors. The zero point determined by this procedure is entered together with the date in the parameter mask of the corresponding temperature sensor (see Section 2.3). Calibrate temperature sensors Temperature sensor TEMP A SENSOR
Esc Temp. sensor
Modify
Start
Press <F4> to select: TEMP A, TEMP B, TEMP C or TEMP D. Press <F5>: the mask with the prompt to immerse the sensor in ice water appears. (We advise you to use a Dewar vessel.) When you are certain that the sensor has cooled to 0 C, confirm this with OK: The calibration was successful if Modify and Start reappear in the display. You can calibrate the next Pt sensor. If the measured temperature value does not lie between -2 C and +2 C, an appropriate error message appears. Confirm this message and first "check" the temperature value given by the sensor using the auxiliary function Measure temperature (see Section 6.1.2).
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Sensor
6.1.4
Measure voltage/current (Ipol/Upol)
You can measure the voltage or the current of solutions with polarized sensors (mV, A). Sensor Indication Titration stand Speed [%] Report t [s] DM142 Voltametric Stand 1 50 No 5
Sensor
Press <F4> to open the list containing the polarized sensors you have defined in the Setup menu (see Section 2.4). Confirm the one you want with OK. Press <F4> to select: "Voltametric" or "Amperometric": Voltametric: Enter the current value which should be applied to the sensor to measure the voltage. Amperometric: Enter the voltage value which should be applied to the sensor to measure the current. Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Use <F4> to select "Yes" if desired: A measured value will be recorded every 5 seconds if you accept the time interval of "5". You can start and stop the measurement with <F5>. Start: The titrator starts to measure the voltage or current of the solution. The measured values are shown in the display and are recorded. During the measurement, all other keys are blocked.
Indication
Titration stand
Speed
Report t [s]
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Stirrer
6.2
Stirrer
You can start the stirrer and change its speed, e.g. to dissolve a substance. Stirrer Titration stand Speed [%] Stand 1 50 Modify Titration stand Start STIRRER
Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Start and stop the stirrer with <F5>. Start: The stirrer stirs at the specified speed.
Speed
Changing the speed during a titration To change the speed during a sample determination: press the Stirrer key (this does not interrupt the method): Stirrer Speed [%] 50 STIRRER
OK Change the speed and confirm with OK: the stirrer stirs at the new speed or is at a standstill if you have entered zero. To follow the analysis sequence in the display again, press the Run key.
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Changer
6.3
Sample changer
Note: All information concerning automation in this titrator's Reference Handbook relates to the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear in some places. Operation of other METTLER TOLEDO sample changers via your titrator is described in the corresonding Operating Instructions.
You can control the sample changer (titration stand: ST20A) and the attached pumps/ dispensers manually. For this you must define the sample changer in the Setup menu and have attached it (see Section 2.7.4). Sample changer Change lift position Rotate turntable Dispense/rinse OK CHANGER
6.3.1
Change lift position Change lift position Lift position bottom CHANGER
Esc Position
Modify
Start
Use <F4> to select: bottom, middle or top. Press <F5> to move the lift to the desired position.
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Changer
6.3.2
Rotate turntable Rotate turntable Direction Number of positions Esc forward 1 Modify Start CHANGER
Direction Number of positions
Press <F4> to select: forward or backward. Enter the number of positions the turntable should move forward or backward. Press <F5> to move the turntable the specified number of positions forward or backward.
6.3.3
Dispense/rinse
If you have attached a pump or a dispenser to an ST20A output, you can dispense or rinse the sensor in the titration vessel. Dispense/rinse ST20A output RINSE CHANGER
Esc ST20A output
Modify
Start
Use <F4> to select: DOSE, RINSE or DISPENSER. Start and stop the dispensing or rinsing process with <F5>. Note: The relay at the "DISPENSER" output closes for 0.5 s and triggers the dispensing.
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Burette
6.4
Burette
When you press the Burette key, the following auxiliary functions appear: Rinse burette Rinse tip Dispense Dispense continuously Titrate manually Dispense continuously (Ipol/Upol) Titrate manually (Ipol/Upol)
6.4.1
Rinse burette Rinse burette Burette drive Drive 2 BURETTE
Esc Burette drive
Modify
Start
Press <F4> to select : Drive 1 DL50/DL53: The Modify command is missing. Start and stop the rinsing process with <F5>. Start: The titrator discharges 1 burette volume. The piston of the burette moves below its zero position to ensure that air bubbles "hidden" in the stopcock are drawn in then expelled.
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Burette
6.4.2
Rinse tip Rinse tip Burette drive Drive 2 BURETTE
Esc Burette drive
Modify
Start
Press <F4> to select: Drive 1 DL50/DL53: The Modify command is missing. Start: 5% of the burette volume are discharged to eliminate any diffusion with solvent in the dispensing tube tip.
6.4.3
Dispense
You can dispense a defined volume. Dispense Burette drive Burette volume Volume [mL] Esc Burette drive Drive 2 10 mL 1.0 Modify Start BURETTE
Press <F4> to select: Drive 1 DL50/DL53: The Modify command is missing. Press <F4> to select: 20, 1, 5 or 10 mL. Enter the volume to be dispensed. Start: The titrator dispenses the specified volume.
Burette volume Volume
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Burette
6.4.4
Dispense continuously
You can dispense stepwise and follow the potential change as a function of the dispensing in the display. You must define the following parameters: Burette drive Burette volume Rate [mL/min] Sensor Titration stand Speed [%] Temperature [C] Temperature sensor Burette drive Drive 2 10 mL 1.0 DG111 Stand 1 50 25.0 Manual
Press <F4> to select: Drive 1 DL50/DL53: The Modify command is missing. Press <F4> to select: 20, 1, 5 or 10 mL. is the rate of dispensing. Press <F4> to open the list containing the sensors you have defined in the Setup menu. Confirm the one you want with OK. The sensor acquires the measured values in the measurement unit you have defined for this sensor (see Section 2.2.2). Use <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Enter the temperature of the solution to be measured if you have not attached a temperature sensor. Press <F4> to select: Manual, TEMP A, TEMP B, TEMP C or TEMP D. Start and stop the dispensing with <F5>. Start: The titrator dispenses continuously and acquires the potential values of the changing solution. The measured values "mL" and "mV, pH,..." are displayed.
Burette volume Rate Sensor
Titration stand
Speed
Temperature
Temp. sensor
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Burette
6.4.5
Titrate manually
You can titrate manually and follow the potential change as a function of the dispensed volume in the display. You must define the following parameters: Titrant Concentration [mol/L] Sensor Unit of meas. Titration stand Speed [%] Temperature [C] Temperature sensor Titrant Concentration Sensor Unit of measurement NaOH 0.1 DG111 mV Stand 1 50 25.0 Manual
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2). Confirm the one you want with OK. The defined measurement unit is entered automatically. You can select a different measurement unit from the selection menu (press <F4>). Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Enter the temperature of the solution to be measured if you have not attached a temperature sensor. Press <F4> to select: Manual, TEMP A, TEMP B, TEMP C or TEMP D.
Titration stand
Speed
Temperature
Temp. sensor
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Burette
Use <F5> to start, interrupt and continue the titration, use <F1> to terminate it. Start: The titrator starts to dispense and increases the dispensing rate continuously. The measured values "mL" and "mV, pH,..." are displayed. The dispensing is interrupted, but measurement of the potential value continues.
Hold:
Proceed: The titrator starts again to dispense at the smallest dispensing rate, in other words you control the addition in the vicinity of the desired end point with the <F5> key. End: The titration is terminated.
The results are displayed: the volume in "mL" and "mmol" and the potential in the selected measurement unit. You can print out these results.
6.4.6
Dispense continuously (Ipol/Upol)
You can dispense stepwise and follow the voltage and current change as a function of the dispensing in the display. You must define the following parameters: Burette drive Burette volume Rate [mL/min] Sensor Indication Titration stand Speed [%] Drive 2 10 mL 1.0 DM142 Voltametric Stand 1 50
Burette drive
Press <F4> to select: Drive 1 DL50/DL53: The Modify command is missing. Press <F4> to select: 20, 1, 5 or 10 mL. is the rate of dispensing. Press <F4> to open the list containing the polarized sensors you have defined in the Setup menu (see Section 2.4). Confirm the one you want with OK.
Burette volume Rate Sensor
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Burette
Indication
Use <F4> to select:"Voltametric" or "Amperometric": Voltametric: Enter the current value which should be applied to the sensor to measure the voltage. Amperometric: Enter the voltage value which should be applied to the sensor to measure the current. Use <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Start and stop the dispensing with <F5>. Start: The titrator dispenses continuously and acquires the voltage or current values of the changing solution. The measured values "mL" and "mV" or "A" are displayed.
Titration stand
Speed
6.4.5
Titrate manually (Ipol/Upol)
You can titrate manually and follow the voltage or current change as a function of the dispensed volume in the display. You must define the following parameters: Titrant Concentration [mol/L] Sensor Indication Titration stand Speed [%] Titrant Concentration Sensor
1/ 2
I2
0.1 DM142 Voltametric Stand 1 50
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the polarized sensors you have defined in the Setup menu (see Section 2.4). Confirm the one you want with OK.
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Burette
Indication
Use <F4> to select:"Voltametric" or "Amperometric": Voltametric: Enter the current value which should be applied to the sensor to measure the voltage. Amperometric: Enter the voltage value which should be applied to the sensor to measure the current. Press <F4> to select: Stand 1, Stand 2, ST20A, Auto stand or External stand; this tells the titrator what stirrer it has to control. 0% The stirrer is at a standstill. 100% The stirrer stirs at maximum speed. Use <F5> to start, interrupt and continue the titration, use <F1> to terminate it. Start: The titrator starts to dispense and increases the dispensing rate continuously. The measured values "mL" and "mV" or "A" are displayed. The dispensing is interrupted, but measurement of the voltage or current value continues.
Titration stand
Speed
Hold:
Proceed: The titrator starts again to dispense at the smallest dispensing rate, in other words you control the addition in the vicinity of the desired end point with the <F5> key. End: The titration is terminated.
The results are displayed: the volume in "mL" and "mmol" and the voltage value in "mV" or the current value in "A". You can print out these results.
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Results
6.5
You can also press the Results key during a titration. The following auxiliary functions can be executed: Display result list Perform reevaluation1) Perform calculations Display measured values Modify statistics
1) appears only when the titrator interrupts the analysis (see Section 6.5.2)
6.5.1
You can view the results generated in the titration of a sample or a sample series. The list is displayed at the earliest (press <F5>) during the first titration (only "Method ID" and "Sample 1" appear if no result is available).
6.5.2
The parameters for the reevaluation of an EQP titration are displayed when the titrator interrupts the current EQP titration or EQP titration (Ipol/Upol) function immediately before completion as the defined condition for the Stop for reevaluation parameter is met (see Sections 3.3.6.7 and 3.3.9.8). In such a case, the message "Reevaluation required" appears (see Section 5.2.2) and you can modify the following parameters under this auxiliary function (example): Threshold Steepest jump only Range Tendency Potential 1 Potential 2 Maximum volume 1000 No Yes Positive No No 5
Modify the appropriate parameters and press <F5>. A mask appears in which you can choose whether you wish to save the modifications of these method parameters for this sample or sample series permanently or only temporarily.
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*
Results
Display result list Perform reevaluation
08/2004
Results
The titrator then reevaluates the titration curve. At the same time, the printer records this EQP titration/ EQP titration (Ipol/Upol) function with the modified parameters. (If your changes still do not meet the defined condition, the message "Reevaluation required" reappears.) To continue the interrupted sample determination, press the Run key: The representation of the EQP titration/EQP titration (Ipol/Upol) function shown before the interruption appears in the display. Press <F5>: The titrator executes either the EQP titration/EQP titration (Ipol/Upol) function (if, e.g. dispensing must be continued owing to the modified parameters) or the next function. Notes 1. To evaluate the effects of your changes, you can view and print out the table of measured values or curve (see Sections 6.5.4 and 6.6). check the new raw results of the EQP titration/EQP titration (Ipol/Upol) function: select the auxiliary function Perform calculations (see Section 6.5.3) assign the raw results to Rx or Cx , e.g. Rx = VEQ or Cx = VP1. 2. "Perform reevaluation" does not appear if the interrupted method is not stored in the titrator but on the memory card or in the computer (see Section 5.1). 3. With the DL55/DL58, "Perform reevaluation" also appears if you interrupt the current EQP titration/EQP titration (Ipol/Upol) function of a user method after a possible predispensing. The auxiliary function does not appear if the interrupted method is a METTLER method.
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Results
6.5.3
At the end of a titration, you can perform additional calculations for these samples. The function appears when you press the Results key on completion of the titration. In the case of a sample series, this is possible only if the "Result list for each sample" is not excluded from the sequence of a series (see Section 6.7.3). DL55/DL58: The auxiliary function also appears if you interrupt the titration and then press the Results key. When you select the auxiliary function, the following parameters appear: Formula Rx = Constant Cx = Decimal places Result unit Result name Q*Cx/m M/(10*z) 3 %
Formula
Constant
Decimal places Result unit Result name
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*
Perform calculations Press <F4> to open the "List of formulas" and accept a different formula from the list or enter the one you need for your calculation (see also Section 8.4: Examples of formulas). Press <F4> to open the "List of constants" and accept a different constant from the list or enter the one you need for your calculation. Symbol You can take the symbols you need for your calculation from the list you obtain when you press <F3>. This includes all symbols possible for the individual functions (see Section 3.3.12: Calculation function and Section 8.1: List of symbols). Enter the number of decimal places you wish to have in your result. Press <F4> to select the unit from the selection menu. You can enter the name using an attached keyboard. Press <F5> to calculate and display the result(s), press <F3> to print it (them) out.
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Results
6.5.4
Display measured values
On completion of every titration, you can display the table of measured values or view the titration curve of this sample again. The function appears when you press the Results key at the end of the titration. With a sample series, this is possible only if the "Result list for each sample" is not excluded from the sequence of the series (see Section 6.7.3). When you select the auxiliary function, the following appears (example): Measured values RESULTS
5.621 mL -267.3 mV
Table Curve1) OK You can view either the table of measured values, the measured value pair Potential/Volume or the titration curve.
1)
DL50: DL53:
With the "(display) Curve" command, the E-V curve is shown in the case of an EQP/ EP titration and the E-t curve with a pH-stat titration. The "(display) Curve" command remains active when you have selected it. Press <F4> to show the selection menu from which you can select one of the possible curve representations: E V curve E/V V curve log E/V V curve 2E/V2 V curve E t curve V t curve V/t t curve Potential vs Volume 1st derivative (Potential vs Volume) 1st derivative (Potential vs Volume, logarithmic) 2nd derivative (Potential vs Volume) Potential vs Time Volume vs Time 1st derivative (Volume vs Time)
1) DL55:
DL58:
When you confirm one of the curves with OK, it is displayed.
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Results
6.5.5
If you have selected Statistics: Yes in the method under the Calculation function(s), the mean value is calculated with a sample series of 2 samples, with more than 2 samples you also obtain the standard deviation and the relative standard deviation. This auxiliary function is then accessible under the Results menu to modify the statistical evaluation, i.e. to allow elimination of outliers. The function appears when you press the Results key on completion of every titration. This is possible only if the "Result list for each sample" is not excluded from the sequence of the series (see Section 6.7.3). Modify statistics Display evaluation Delete result Undo deletion Esc Display evaluation Example of a statistical evaluation with 6 samples Statistical evaluation R1 n x s = 6 = 1.234 % = 0.01268 % OK Delete result Using the result list you decide what sample result is an outlier and then delete it. Delete result Sample No. Result R Esc 1 1 OK RESULTS RESULTS RESULTS
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*
Modify statistics OK Enter the number of the sample whose result should be deleted, e.g. 2. Enter the number (index) of the result defined by the Calculation function.
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Results
Delete result
If you confirm OK, the result is deleted and the statistical data are calculated with the new number of samples. You can delete several sample results and always view the final result in the mask "Statistical evaluation" (example): Statistical evaluation s = 0.00346 % srel = 0.112 % Outlier Sample No. 2 deleted RESULTS
OK You can use the parameter "All results" of the auxiliary function Report to print out the new evaluation (see Section 6.6). Undo deletion As long as the result list of this sample series remains stored, you can undo the deletion for all sample results: Undo deletion Sample No. Result R Esc 1 1 OK RESULTS
Enter the number of the sample and that of the corresponding result R: The result of this sample will be reincorporated in the statistical calculation.
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Report
6.6
Report
On completion of each sample series, you can print out additional reports or transfer them to a computer (see also Section 3.3.16: Report function). In the case of a sample series, this is possible only if you have not excluded the "Result list for each sample" from the sequence of the series (see Section 6.7.3). DL55/DL58: You can activate the auxiliary function if you interrupt the titration and then press the Report key. Report Output Printer Results All results REPORT
No No Modify
Start
Output
Press <F4> to select the output unit to which the data should be sent: Printer, Memory card (not with the DL50) Computer, Printer + memory card (not with the DL50) or Printer + computer. All results of the sample last determined defined in the Calculation functions are recorded when you select "Yes" with <F4> and press <F5>. Results of all samples generated to date are recorded when you select "Yes" with <F4> and press <F5>. They also include the statistical data if these have been calculated (see Section 6.5.5). The raw results of the sample last determined are recorded when you select "Yes" with <F4> and press <F5>.
Results
All results
Raw results
Table of The table of measured values of the sample last determined is recorded measured values when you select "Yes" with <F4> and press <F5>. Sample data The sample data of all samples of the current series are recorded when you select "Yes" with <F4> press <F5>. The titration curve Potential vs Volume of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>.
E V curve
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Report
E/V V curve
The 1st derivative of the titration curve Potential vs Volume of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>. The ordinate representation is linear. The 1st derivative of the titration curve Potential vs Volume of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>. The ordinate representation is logarithmic. The 2nd derivative of the titration curve Potential vs Volume of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>. The ordinate representation is linear. The titration curve Potential vs Time of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>. The titration curve Volume vs Time of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>. The 1st derivative of the titration curve Volume vs Time of the sample last determined is recorded when you select "Yes" with <F4> and press <F5>.
log E/V V curve 2E/V2 V curve
E t curve
V t curve
V/t t curve
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Misc.
...
Miscellaneous
6.7
When you press the Misc. key, the following appears Define titrator settings Adjust measuring inputs Shorten analysis sequence Define user level Activate control input Activate control output
6.7.1
Define titrator settings
You can or must select or define the following settings for the titrator: Date/time format Date/time Language Report header Titrator ID Audio signal
6.7.1.1
Date/time format
You have several possibilities for the date and time notation. If you wish to change the existing formats, select this menu line and press <F4>: Formats Date format Time format Esc Date format Time format 17-OCT-1995 17:04 (24 h) Modify OK MISC.
Press <F4> to select one of the four possible formats. Press <F4> to select the other format. If you change the formats, e.g. after a month they are transferred to all data stored at the time.
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Misc.
...
6.7.1.2
Date/time
To change the date or the time, select this menu line and press <F4>; the mask appears in which you can overwrite the date.
6.7.1.3
Language
In the titrator all texts are stored in English, German, French, Italian and Spanish. To change the active language, select this menu line and press <F4>: Language Active language English MISC.
Esc Active language
Modify
OK
Press <F4> to select one of the languages.
6.7.1.4
Report header
If you wish to enter an identifier or a text (with attached keyboard) which should appear in the header of every report of a titration method, select this menu line and press <F4>: Report header Text: Text: Esc OK MISC.
6.7.1.5
Titrator ID
If you wish to enter an identification for your titrator this is always recorded select this menu line and press <F4>; the mask appears in which you can enter an identification.
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Misc.
...
Audio signal
6.7.1.6
An audio signal confirms either every keystroke or draws your attention to instructions, notes and error messages. When the titrator is delivered, all these parameters are assigned a signal. To change this, press <F4>: Audio signal Keystroke Results Messages Esc Keystroke Yes Yes Yes Modify OK MISC.
Yes: A brief signal sounds after every keystroke. If you do not wish to hear this, press <F4>: "No. Yes: A brief signal sounds after every result that appears in the display. If you do not wish to hear this, press <F4>: "No. Yes: A signal draws your attention to error messages, notes and instructions. If you do not wish to hear this, press <F4>: "No.
Results Messages
6.7.2
Adjust measuring inputs
The measuring inputs for sensors and temperature sensors must be adjusted to ensure the titrator measures potential and temperature values correctly. The adjustment of the measuring inputs is performed by METTLER TOLEDO and the calibration data of the characteristic line of each input recorded on a data sheet, which is enclosed with every sensor option (see Section 10.5.1). The measuring inputs of the pH option installed in slot 1 of the titrator in the factory are adjusted; the calibration data are stored and can be printed out (see mask). Measuring inputs Option in slot 1 Option in slot 21) Esc
1)
MISC.
Print
Modify
OK
appears only if a sensor option is installed in the slot
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Misc.
...
Notes 1. If you receive a data sheet with a pH option which contains instructions for the entry of the calibration data, you must follow these: If, for example, you install this or an additional option in slot 2, you must enter the data of the data sheet for slot 2 (overwrite default values!). Calibration data Sensor 1: Temp 1 (Pt100): Esc Offset Slope Offset MISC. 0 30950 -15463 OK
2. If you receive a data sheet with a pH option which contains only calibration data, these are stored on the option itself. They are automatically adopted for every slot and can not be deleted. In this case you can only view the data: Calibration data Sensor 1: Temp 1 (Pt100): Esc Offset Slope Offset 0 30950 -15463 OK MISC.
3. You always receive a data sheet with a KF option which contains only calibration data, in other words the data are stored on the option and are automatically adopted for each slot; they can not be deleted: Calibration data Sensor 2 (Ipol): Sensor 2 (Upol): Esc Offset Slope Offset 0 26025 0 OK MISC.
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Misc.
...
Shorten analysis sequence
6.7.3
During the sequence of an analysis, information is shown in the display which you must confirm with OK to allow the titrator to continue working: the mask "Defined are" appears at the start (see Section 5.1), and on completion, the "Result list" for every titrated sample within a series (see Section 5.2). You can exclude these two masks from the analysis sequence to accelerate it. Shorten analysis sequence Defined resources Result list for each sample Esc Defined resources Result list for each sample Yes Yes Modify OK MISC.
Yes: The mask "Defined are" appears before the determination of a sample or sample series. If this is not required, select "No" with <F4>. Yes: Within a sample series the result list appears after the determination of each sample if you are working with titration stand 1, 2 or external. If this is not required, select "No" with <F4>. With series which you perform at a sample changer (titration stand: ST20A) or at an auto stand, the mask is skipped automatically (see Sections 5.1 and 5.4).
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Misc.
...
6.7.4
Define user level
You can decide if all people who work with the titrator should also have access to the Setup or Method menu, i.e. have the possibility to delete resources or modify methods. If you have, e.g. temporary staff who can perform only routine analyses, it is good practice to block their access to these menus. Define user level User level Expert MISC.
Esc Expert Routine
Modify
OK
In the factory setting of the titrator, you have access to all menus. To change this, select "Routine" with <F4>. In the Setup menu you can only print out the defined resources. In the Method menu you can only print out the methods. In the Data transfer menu, you can not - transfer data to the computer - remote-control the titrator - transfer data to and from the memory card - delete data on the memory card - format a memory card. In the Analysis menu you can not modify an ongoing method (DL55/ DL58: see Section 5.3). To switch to the expert level at a later date, open this mask, Define user level User level Routine MISC.
Expert
Esc
OK
and while holding down the Shift key, press key 1 three times: "Expert" and the "Modify" command reappear.
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Misc.
...
Activate control input
6.7.5
The RS option has a socket whose two TTL inputs you can activate (see Section 10.7). To do this, you must have installed the option in the third slot, attached the devices whose signal should be scanned. Activate control input Input In 3.1 MISC.
Esc Input
Modify
Start
Press <F4> to activate the other input: "In 3.2". Start: The input signal of the attached device is scanned until you press <F5> (Stop). The input signal Off corresponds to a voltage of 5 V, On to a voltage of 0 V. Example: A level sensor is attached via a TTL input to check the amount of liquid in a container. The setup is designed for a maximum level of 500 mL:
TTL socket
Level sensor
500 mL
If the container holds more than 500 mL, the sensor sends the input signal Off. If the container holds less than 500 mL, the sensor sends the input signal On to indicate that the container should be filled.
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Misc.
...
6.7.6
Activate control output
The RS option has a socket whose four TTL outputs you can control (see Section 10.7). To do this, you must have installed the option in the third slot attached the devices you intend to control. Note: TTL are signals which do not transfer power. To operate devices such as a pump, you must connect an amplifier in the circuit (see Section 10.7) Activate control output Output Control mode Esc Output Control mode Out 3.1 On/Off Modify Start MISC.
Press <F4> to select: "Out 3.2", "Out 3.3", "Out 3.4" or Out 3.1". The following modes are possible (press <F4>): On/Off Input controlled Sequential On/Off Start: The attached device is controlled until you press <F5> (Stop). The output signal On (Start) corresponds to a voltage of 0 V, Off (Stop) to a voltage of 5 V. Example: A pump is attached via a TTL output. The pump is switched on (it dispenses) with "Start" and switched off with "Stop". Input controlled Input controlled Input Output signal Esc In 3.1 Normal Modify OK MISC.
Press <F4> to select the other input: "In 3.2". Press <F4> to select the other signal possibility: "Inverted" (see following page).
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Misc.
...
Example: A pump is attached via a TTL output, a level sensor via a TTL input:
Control mode
TTL socket
Pump with supply vessel
Container with level sensor
The titrator checks at the start whether the signal of the selected input is in Section 6.7.5). With this voltage of 0 V the titrator controls the pump (normal output signal) so that it starts to pump liquid from the supply vessel into the container with the level sensor. As soon as this container holds more than 500 mL, the pump is switched off automatically. Inverted: The pump can be controlled only with the 5 V signal instead of the normal output signal of 0 V. When the pump is switched off, the voltage is 0 V. Sequential You can use this special mode to control, e.g. a dispenser.
Sequential Number of pulses Pulse duration [s] Interval [s] Esc 10 1.0 1.0
MISC.
OK
Each pulse causes the dispenser to dispense a quantity of liquid. This depends on the pulse duration, which you can find on the data sheet of the dispenser.
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Misc.
...
Control mode
1st pulse
Interval Off
3rd pulse
Pulse duration On
Start: The dispensing starts and is stopped automatically when the sequence has been processed. You can also terminate the dispensing with <F5> (Stop).
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Data Transfer
6.8
Data transfer
With the DL53, DL55 and DL58 you can back up your data on a memory card. You can also transfer the data to a computer or control the titrator from the computer; for this you can enter a bar-code string. Memory card Computer 1) Remote control1) Bar-code string
1) These
1)
parameters do not appear until you have defined the computer in the Setup menu (see Section 2.7.3)
6.8.1
Memory card
You can use a memory card with the DL53, DL55 and DL58 to 1. store user methods and resources when the user data memory is full back up all data of the user data memory, i.e. resources and user methods. You can reload these data when needed on the same or on another titrator of the same type. The cards you can use are listed in Section 12.8, insertion information in Section 10.6). 2. store reports of analyses. You can print these out from the card at any time. DL50: You can use only a memory card supplied by METTLER TOLEDO to load a new software version. Formatting a new card Remove the write protection of the card and insert card. Confirm "Memory card" with OK: The message "Card not readable" appears. If you confirm this with OK, the following appears: Format card All data will be deleted! DATA TRANSFER
Esc
Start
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Data Transfer
Start: The card is formatted and the end of the operation displayed. Note: Formatting of a 1 MB SRAM card takes approx. 30 seconds, that of a 2 MB Flash card approx. 4 minutes. The formatting generates a directory and commands. Confirm "Memory card" in the Data Transfer mask again: Display directory Copy from titrator to card Copy from card to titrator Format card
Directory
Directory User methods Resources Memory copies Reports Esc
DATA TRANSFER
Print
OK
Print: A list of the stored methods is printed out. OK: A list of the methods, resources or memory copies appears if they are on the card. You can then print out or delete an individual method, the list of selected resources or the list of the memory copies. Reports: If you have selected "Memory card" as output in the function or auxiliary function Report, the selected results or curves are stored under the method ID and the date, e.g. Reports (series) 90001 235 90002 Esc 18-Oct-1996 22-Oct-1996 22-Oct-1996 Delete 11:48 14:34 10:03 OK DATA TRANSFER
<F5> shows the list of the reports for each sample of the series (see following page):
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Data Transfer
Directory
Reports (samples) 1 [1] 18-Oct-1996 2 [1] 18-Oct-1996 3 [1] 18-Oct-1996 Esc Delete 11:48 12:01 12:23
DATA TRANSFER
Print
1, 2 and 3 refer to the sample No., [1] to the number of the Report function (index, relevant only with special methods). [*] appears if the report has been sent by the auxiliary function Report (Report key). <F4> prints out the results and/or curves defined in the function. From titrator... Copy to card User methods Resources Memory copy Esc User methods: With <F5> the following appears: Copy method Method ID DATA TRANSFER DATA TRANSFER
OK
Esc
Modify
Start
Enter the identification of the method; if you do not know this, press <F4>: The list of user methods appears from which you can select the one you wish to copy. If a method with the same ID is stored on the card, an appropriate message appears. Resources: <F5> is used to show the list of resources from which you can select those you wish to copy. Resources stored on the card will be overwritten.
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Data Transfer
From titrator...
Memory copy: With <F5> the following appears: Copy DATA TRANSFER
All data of the user data memory will be copied on the card. Esc Start
You use this procedure to generate a backup copy of the user data memory. Start: All stored resources and user methods are copied and stored as "memory copies" on the card with date and time (see following page). During the copying operation, the message "Data are transferred" appears. From card... Copy to titrator User methods Resources Memory copies Esc DATA TRANSFER
OK
User methods: Use <F5> to show the mask of the method ID. If you do not know the identification, press <F4>: The list of user methods appears from which you can select the one you wish to copy. If a method with the same ID is stored in the user data memory, an appropriate message appears. If the sample data list contains data, you can not copy the method until you have deleted these data (see Section 4). Resources: Use <F5> to show the list of resources from which you can select those you wish to copy. Titrants stored in the titrator are overwritten if their names and concentrations are the same as the titrants being copied. All other titrants remain stored. Sensors and solvents stored in the titrator are overwritten if their names are the same as those being copied. All other resources are overwritten (temperature sensors, auxiliary values, titration stands, peripherals).
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Data Transfer
From card
Memory copies: With <F5> the following appears (example): Load memory copy 10-Oct-1996 11-Nov-1996 12-Dec-1996 Esc Load 16:45 10:12 14:34 Start DATA TRANSFER DATA TRANSFER
Notice: All data of the user data memory will be overwritten! Esc Start
Start: All data of the user data memory are overwritten by those of the memory copy of Oct. 10, 1996. If the sample data list contains data, you can not load the copy until you have deleted these data (see Section 4). Format card To delete all data on the card in one operation, you can reformat the card (see start of this section).
6.8.2
Computer
You can transfer user methods and/or defined resources from the titrator to a computer. A requirement for this is that you have defined the computer in the Setup menu and attached it loaded the DLWin or the LabX titration software or an appropriate program. Switch on the computer and start required program. Confirm "Computer" with OK: Computer DATA TRANSFER
Transfer from titrator to computer
Esc
OK
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Data Transfer
From titrator...
Transfer to computer User methods Resources Memory copy Esc
DATA TRANSFER
OK
User methods: Use <F5> to show the mask with the method ID. If you do not know the identification, press <F4>: the list of user methods appears from which you can select the one you wish to transfer. Resources: Use <F5> to show the list of resources from which you can select those you wish to transfer. Memory copy: With <F5> the following appears: Transfer DATA TRANSFER
All data of the user data memory will be transferred to the computer Esc Start
Start: All data except those in the sample data memory are transferred. During the operation, the message "Data are transferred" appears. Note: You can also transfer data stored in the computer back to the titrator. You will find further information in the Operating Instructions of the computer interface or in the Operating Instructions of the DLWin or the LabX titration software.
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Data Transfer
6.8.3
Remote control
You determine whether the titrator is controlled exclusively by a computer. The requirement for this is that you have loaded the DLWin or the LabX titration software or an appropriate program. Remote control DATA TRANSFER Status Off
Esc Status
Modify
OK
Press <F4> to select "On": The titrator can be controlled only by the computer, i.e. you can neither enter data on the titrator, nor start an analysis nor execute an auxiliary function. When you have confirmed "On", all that appears is: Data transfer Remote control Bar-code string Esc OK DATA TRANSFER
If the sample data list contains data or an auxiliary function is running, an appropriate error message appears beforehand.
To follow the entries and commands of the computer in the display of the titrator, you can use the following keys: Arrow keys Scroll parameters of a mask Run key Display of the active function of an ongoing method Sample key Sample data list Data transfer key Switch off remote control Enter a bar-code string (see next section). You will find further information on remote control in the Operating Instructions of the computer interface or in the Operating Instructions of the DLWin or the LabX titration software.
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Data Transfer
6.8.4
Bar-code string
This parameter is intended for automatic systems. The string which is read in by a defined and attached bar-code reader is immediately transferred to the computer (see Section 2.7.3). If you do not have a bar-code reader, you can enter the string here with the titrator keyboard. Enter bar-code string > DATA TRANSFER
Esc
OK
When you confirm the entry with OK, the string is transferred to the computer.
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DL58
DL58
Contents
Page 7. 7.1 7.1.1 7.1.1.1 7.1.1.2 7.1.2 7.1.2.1 7.1.2.2 7.1.2.3 7.2 7.2.1 7.3 7.3.1 7.3.2 7.3.3 7.3.4 7.3.4.1 7.3.4.2 7.3.4.3 7.3.4.4 7.3.5 7.3.6 7.3.7 The DL58 .................................................................................................... Additional resources ................................................................................ Control inputs (only with TTLIO) .............................................................. Modify ....................................................................................................... Add ........................................................................................................... Control outputs (only with TTLIO) ............................................................ Delete ....................................................................................................... Modify ....................................................................................................... Add ........................................................................................................... Special methods ........................................................................................ Additional commands ............................................................................... Additional functions ................................................................................. Temperature ............................................................................................. Instruction ................................................................................................. Pump ........................................................................................................ Two-phase titration ................................................................................... Titrant/Sensor ........................................................................................... Predispensing .......................................................................................... Titrant addition.......................................................................................... Measure mode ......................................................................................... Control input ............................................................................................. Control output ........................................................................................... Sync ......................................................................................................... 7-3 7-4 7-4 7-4 7-5 7-5 7-6 7-6 7-6 7-7 7-7 7-10 7-10 7-11 7-11 7-12 7-12 7-13 7-14 7-14 7-15 7-16 7-18
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7-1
DL58
DL58
7.
The DL58
This section explains the resources, commands and functions for the development of methods which the other three titrators do not possess. With the preloaded METTLER and standard methods, you can change only the parameters of the functions. The DL58 memory holds additional, Special methods which allow the insertion of identical or new functions or the deletion of existing functions thus enabling you to develop completely new methods.
Setup menu
Method menu Special methods Commands Add Delete Functions Temperature Instruction Pump Two-phase titration Control input Control output Sync
Resources Control inputs Control outputs
Note: You can also run the special methods with the DL53 and DL55 if you purchase a dongle and the special methods available on memory cards (see Section 11.2).
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Control inputs
DL58
7.1
Additional resources
"Control inputs" and "Control outputs" are available in the Setup menu as additional resources which you must define.
7.1.1
Control inputs (only with TTLIO)
You can use the parameters of this resource only if you have installed an RS option in the third slot. The two inputs In 3.1 and In 3.2 of the TTLIO socket are used for the attachment of devices whose signal should be scanned (see Sections 6.7.5 and 10.7). If you select this menu and press <F4>, the following appears: Control inputs (only with TTLIO) Fill level sensor SETUP
Esc Notes
Add
Modify
OK
1. When the titrator is delivered, the English name for the fill level sensor is defined. Should you wish to store the Spanish name, use the Modify command (see Section 7.1.1.1). 2. If you have added device names to the list, the Delete command appears (<F2>).
7.1.1.1
Modify
Press <F4>, "Modify", to show the parameters of the control input whose name and input you can change. Control input parameters Name Input Esc Name Fill level sensor In 3.1 Modify OK SETUP
You can change the name by pressing <F4> and selecting a new name from the list of input names which appears. Select with <F4>: "In 3.1" or "In 3.2".
Input
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DL58
Control outputs
Storage procedure The definition of the control input is stored when you confirm both the parameter mask and the list of names of the control inputs with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of Section 2.1.2).
7.1.1.2
Add
With this command you can add a new device to the list of the defined devices. The following mask always appears: Control input parameters Name Input Esc _ _ _ _ _ _ _ _ _ _ _ _ _ _ In 3.1 Modify OK SETUP
You can modify the parameters by the procedure described in Section 7.1.1.1. If you define, e.g. several devices with the same name, you must provide these with an additional identification so that the titrator can distinguish them, e.g. Fill level sensor/2. If you do not, a message appears (see Section 2.1.3).
7.1.2
Control outputs (only with TTLIO)
You can use the parameters of this resource only if you have installed an RS option in the third slot. The four outputs Out 3.1...Out 3.4 of the TTLIO socket are used for the attachment of, e.g. dosing equipment (see Sections 6.7.6 and 10.7). If you select this menu and press <F4>, the following appears: Control outputs (only with TTLIO) Pump Dispenser Valve Esc Delete SETUP
Add
Modify
OK
Note: When the titrator is delivered, the English name for the stored devices is defined. Should you wish to store the Spanish name, use the Modify command (see Section 7.1.2.1).
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Control outputs
DL58
7.1.2.1
Delete
If you press <F2>, "Delete", the device for the defined output will be deleted from the list.
7.1.2.2
Modify
Press <F4>, "Modify", to show the parameters of the control output whose name and output you can change. Control output parameters Name Output Esc Name Output Pump Out 3.1 Modify OK SETUP
You can change the name by pressing <F4> and selecting a new name from the list of output names which appears. Select with <F4>: "Out 3.1", "Out 3.2", "Out 3.3" or Out "3.4".
Storage procedure The definition of the control output is stored when you confirm both the parameter mask and the list of names with OK. The modification of a parameter is always stored when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of Section 2.1.2).
7.1.2.3
Add
With this command you can add a new device to the list of defined devices. The following mask always appears: Control output parameters Name Output Esc _ _ _ _ _ _ _ _ _ _ _ _ _ _ Out 3.1 Modify OK SETUP
You can change the parameters by the procedure described in Section 7.1.2.2. If you define, e.g. several devices with the same name, you must provide these with an additional identification so that titrator can distinguish them, e.g. Pump/2. If you do not, a message appears.
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DL58
Special methods
7.2
Special methods
If you press the Method key and scroll the menu downward (Shift and -key), the following appears:
Print Special methods 91001 91002 Esc Surfactant determination Vitamin C determination Delete Print Modify
OK METHOD
You can change these two special methods to meet your requirements and store them under a different method ID. Each new method is stored in the "Special methods" group.
7.2.1
Additional commands
You can modify the special method by changing or deleting its functions or by adding new functions. Virtually all functions can occur more than once in a method.
Special method
delete Functions add
Parameters
modify
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7-7
Methods METTLER methods Special methods
METHOD
Special methods
DL58
Press <F4> when the surfactant determination is selected: The list of functions appears. Method: 91001 Title Sample Stir Esc METHOD
Add
Modify
OK METHOD
Method: 91001 Title Sample Stir Two-phase titration Esc Add Method: 91001 Sample Stir Two-phase titration Calculation Esc Delete Add Add
Modify
OK METHOD
Modify
OK
You can insert a new function after every selected function (see following page). If you select a wrong order when inserting functions (e.g. you can not place the EQP titration function before the Sample function), an error message appears, but not until the method is stored. You can not delete the Title function as it is used to identify the method and must always be placed at the head of the functions. You can not delete the Sample function as it provides the titrator with information regarding the titration stand at which titration is performed.
Delete
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DL58
Special methods
If, e.g. Stir is selected and you press <F3>, the list of functions you can add appears: Stir Measure Temperature Instruction Dispense Pump EQP titration EP titration Learn titration EQP titration (Ipol/Upol) EP titration (Ipol/Upol) Two-phase titration pH/mV-stat Control input Control output Calculation Auxiliary value Titer Calibration Report Sync .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. .............................. (6) (10) (10) (10) (6) (6) (*) (*) (*) (*) (*) (*) (2) (6) (6) (12) (20) (1) (1) (8) (20) see Section 3.3.3 see Section 3.3.4 see Section 7.3.1 see Section 7.3.2 see Section 3.3.5 see Section 7.3.3 see Section 3.3.6 see Section 3.3.7 see Section 3.3.8 see Section 3.3.9 see Section 3.3.10 see Section 7.3.4 see Section 3.3.11 see Section 7.3.5 see Section 7.3.6 see Section 3.3.12 see Section 3.3.15 see Section 3.3.14 see Section 3.3.13 see Section 3.3.16 see Section 7.3.7
Select the function you wish to add and press <F5>. It will be inserted under the Stir function. Note: The number in brackets is the maximum possible number of this function a special method can contain. (*): A special method can contain maximum 6 titration functions.
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Temperature
DL58
7.3
7.3.1
Additional functions
Temperature
You can use this function to measure the temperature of a solution under defined conditions. The titrator acquires the measured value as raw result T (see Note a. in Section 3.3.4). Sensor Unit of meas. T [C, F, K] t [s] t(min) mode t(max) [s] Sensor Temp A C 0.02 2.0 Fix 30.0
Press <F4> to select the temperature sensor: TEMP A, TEMP B, TEMP C or TEMP D. Press <F4> to select the unit: C, F or K. The temperature drift must be less than T/t (0.01 C/s) during the period t (2 s) if the temperature is to be acquired as a measured value. This occurs within a defined time interval t(min) and t(max). t(min) is earliest time for the acquisition of the measured value. Select t(min) from the selection menu: t(min) mode Fix T > set value T < set value Esc METHOD
Unit of meas. T t t(min) mode
Modify
Fix: With <F4> the mask appears in which you can change t(min). T greater than set value: Instead of a fixed time you can select a condition: The measured value must be greater or T less than set value: less than a specified set value: <F4> is used to show the mask in which you can enter the set value [C, F, K]. t(max) is the latest time for the acquisition of the measured value. If you have selected one of the conditions for t(min), the titrator starts the next function when the measured temperature T is greater than (less than) the set value and the drift condition is met, but at the latest after t(max).
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DL58 7.3.2 Instruction
Instruction/Pump
This function allows you to intervene manually in the sequence of the titration method, in other words the method is interrupted. The entered text appears at the desired position during the current method in the display. The method does not continue until you confirm the instruction with Run. Instruction Text Text Text Esc Text METHOD
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
OK
Enter the desired instruction.
7.3.3
Pump
With the aid of this function you can add solvent with a pump attached to the sample changer. Pump Solvent Volume [mL] Stir Esc Solvent H2O 10 No Modify OK METHOD
With <F4> select the solvent from the list which contains those you have defined in the Setup menu (see Section 2.8). Enter the volume that should be added. You have defined the pump rate of the device in the Setup menu. Select whether (Yes) or not (No) stirring should be effected during the dosing operation.
Volume
Stir
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Two-phase titration
DL58
7.3.4
Two-phase titration
This section explains the first 4 parameter groups of this titration function. The explanations for those of the group Recognition, Termination and Evaluation can be found in Sections 3.3.6.5 through 3.3.6.7. Titrant/Sensor Predispensing Titrant addition Measure mode Recognition Termination Evaluation The titrator records several measured values and volumes as raw results (see Section 8.1).
7.3.4.1
Titrant/Sensor
To modify the titrant or sensor, press <F4>: Titrant Concentration [mol/L] Sensor Unit of meas. Titrant Concentration Sensor Unit of measurement Hyamine 0.004 DP550 mV
Press <F4> to open the list containing the titrants you have defined in the Setup menu (see Section 2.1). Confirm the one you want with OK. The defined concentration of the titrant is entered automatically. Press <F4> to open the list containing the sensors you have defined in the Setup menu (see Section 2.2.). Confirm the one you want with OK. The defined measurement unit is entered automatically. If you select the unit from the selection menu, you should select mV or the unit defined in the Setup menu, otherwise you will receive an error message when the method is started.
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DL58 7.3.4.2 Predispensing
Two-phase titration
Predispensing shortens the titration time. You can select one of two predispensing modes when you press <F4>. Predispensing to volume to (factor x sample size) No Esc Volume METHOD
Modify
You dispense a specified volume [mL] which you can enter when you press <F4>. Instead of a number, you can enter a formula. You can also enter a wait time: After the predispensing, the titrator waits for this time to elapse before it adds the titrant in a controlled manner. Notice: The wait time includes the time of the dosing operation! You dispense to a specified volume that is calculated from the product of the sample weight or volume and a factor; you can enter this factor when you press <F4>. You can also enter a wait time (see "Volume"). You do not wish to predispense.
No
The titrator adds the volume in one step. It adopts the potential values ET1 and ET2.
ET1: Potential at the start of predispensing or the titration ET2: Potential after predispensing
E [mV]
ET2 ET1
V [mL]
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Two-phase titration
DL58
7.3.4.3
Titrant addition
For the two-phase titration, only the incremental addition mode is available. Titrant addition V [mL] 0.05 METHOD
Esc V
OK
The volume increment that the titrator adds is constant (see Section 3.3.6.3: Incremental titrant addition).
7.3.4.4
Measure mode
You define the duration of the mixing and separation time as well as the stirrer speed during the separation time. Measure mode Mixing time [s] 15.0 Separation time [s] 50.0 Stirrer speed (sepn time) [%] 10 Esc Mixing time METHOD
OK
After the addition of every increment, the two phases are stirred for this time at the speed selected in the Stirrer function. During this time, the two phases should separate so that a stable measured value of the corresponding phase can then be acquired. You can set your "own" speed for the separation time or set it to 0. Note: If you use the auxiliary function Stirrer to change the speed during the mixing time, this applies only to the mixing time during the two-phase titration and for any functions after the two-phase titration. change the speed during the separation time, this applies only to the separation time during the two-phase titration.
Separation time Stirrer speed
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DL58 7.3.5 Control input
Control input
With this function you can influence the progress of a method externally via the inputs of the TTLIO socket. This is possible only with an RS option installed in the third slot (see Section 10.7). The titrator waits for the defined signal to be detected or the maximum time to elapse before it processes the next function. Control input Name Input signal Max. time [s] Esc Name _ _ _ _ _ _ _ _ _ _ Rising 10.0 Modify METHOD
OK
With <F4> open the list containing the names of the inputs you have defined in the Setup menu (see Section 7.1.1). Confirm the one you wish to use with OK. With Rising or Falling you specify the direction of change of the input signal when the signal you have defined is detected. This time defines the wait time for detection of the signal. On elapse of this time, processing of the method continues even if no signal has been detected.
Input signal
Max. time
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Control output
DL58
7.3.6
Control output
With this function you can generate TTL signals. This is possible only with an RS option installed in the third slot (see Section 10.7). The nature of the signal depends on the control mode you have selected. The standard status of the control outputs is "high". Control output Name Control mode Instruction Esc Name _ _ _ _ _ _ _ _ _ _ Fixed time Modify OK METHOD
With <F4> open the list containing the names of the outputs you have defined in the Setup menu (see Section 7.1.2). Confirm the one you wish to use with OK. The mode determines the number and nature of the generated TTL signals. The following modes are possible (press <F4> ): "Fixed time", "On/Off", "Input controlled" or "Sequential". Fixed time Select this mode when you wish to operate a device that is attached to the control output over a fixed time period. Enter the time during which the control output should be switched on. On/Off With this mode you can, e.g. switch on a device attached to the control output at the start of the method and switch it off at the end of the method. Select whether the control output should be switched on or off. The status of the control output will be automatically set to off on completion of the method. Input controlled This mode allows a device attached to the control output to be switched on or off by a device attached to the control input (e.g. pushbutton). The function is ended when the signal at the defined control input changes or after elapse of a maximum time.
Control mode
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DL58 Control mode
Control output
Input controlled Name Output signal Max. time [s] Esc _ _ _ _ _ _ _ _ _ _ Normal 10.0 Modify
METHOD
OK
Name: With <F4> open the list containing the names of the inputs you have defined in the Setup menu (see Section 7.1.1). Use OK to confirm the one which should control the control output function. Output signal "Normal": The signal is routed directly from the control input to the control output. Output signal "Inverted": The signal of the control input is first inverted and then routed to the control output. Max. time: The maximum time defines the wait time for the signal change. On elapse of this time, the method is processed further even if no signal has been sent. Sequential Use this mode to select devices which you can use to either trigger various actions through different sequences or repeat particular actions through single pulses of the sequence (see Section 6.7.6). Sequential Number of pulses Pulse duration [s] Interval [s] Esc 10 1.0 1.0 OK METHOD
Number of pulses: Enter the number of pulses of the desired sequence. Pulse duration: Enter the time during which a pulse should be switched on. Interval: Enter the wait time between the pulses. Instruction You can enter a text which is shown while the function is active.
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Sync
DL58 Sync
7.3.7
Under this function you specify the parameters for the synchronization of the titrator with an external control unit. The synchronization takes place via the system interface (RS option in the slot 3!). Sync Sync mode Code Comment Esc Sync mode Send 1 Modify OK METHOD
Press <F4> to select: "Send" or "Send/Wait". Send: The titrator transmits the numeric code you have defined to the external control unit and then begins to process the next method function immediately. Send/Wait: The titrator transmits the numeric code you have defined to the external control unit and then waits until this sends back the same code. Only then does the titrator start to process the next method function. Enter a number between 1 and 32, which is sent to the external control unit. Enter a comment, which appears on the display when the function is executed.
Code
Comment
Notes 1. You will find additional information regarding the communication between the titrator and the external control unit in the Operating Instructions "DL50/DL53/DL55/DL58: RS232C Interface Description". 2. Two titrators can also be synchronized by means of the system interface using the Sync function. You must then connect the two titrators using a null modem.
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Symbols and explanations
Contents
Page 8. 8.1 8.1.1 8.2 8.2.1 8.3 8.3.1 8.3.2 8.3.3 8.3.4 8.4 8.4.1 8.4.2 8.4.3 8.5 8.5.1 8.5.2 8.5.3 8.5.4 8.5.5 8.5.6 Symbols and explanations ........................................................................ List of symbols ........................................................................................... Compilation of the raw results ...................................................................... 8-3 8-3 8-8
Use of indices ............................................................................................. 8-9 Compilation of the symbols by indexing forms ............................................. 8-12 Evaluation procedures .............................................................................. Standard ....................................................................................................... Minimum/maximum ...................................................................................... Segmented ................................................................................................... Asymmetric .................................................................................................. Examples of formulas ................................................................................ Results ......................................................................................................... Constants ..................................................................................................... Formulas for restriction of the equivalence point ......................................... 8-14 8-14 8-14 8-15 8-16 8-17 8-17 8-18 8-19
Restrictions in the analysis ....................................................................... 8-20 Maximum number of samples ........................................................................8-20 Maximum number of sample series in the sample data memory ................. 8-20 Maximum number of equivalence points per sample determination ............ 8-20 Maximum number of measured values per Titration function ...................... 8-20 Maximum number of results per sample series ........................................... 8-20 How long does the titrator store data? ......................................................... 8-20
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8-1
8-2
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List of symbols
8.
Symbols and explanations
In this section you will find additional information which supplements Sections 3 to 7.
8.1
List of symbols
This list shows you the abbreviations of all symbols of the parameters and the raw results determined by the titrator together with their definition. If you enter the symbols using an external keyboard, you must comply with the uppercase or lowercase notation. Function/Resource Titrant Symbol c t N Definition Nominal concentration of the titrant in mol/L Titer of the titrant c * t: actual equivalent concentration of the titrant in mol/L (ACTUAL value); it is calculated automatically by the titrator. Zero point of the pH electrode Slope of the pH electrode Auxiliary value : H1 to H20 Sample size of the weight in g or volume in mL (for Calculation function) Molar mass in g/mol Equivalent number: Number of reaction entities compared to the titrant Note: For technical reasons, the notation z* of DIN standard 32 625 has not been used for the titrator. Correction factor Time of a sample determination in seconds
Sensor
ZERO SLOPE
Auxiliary value Sample (Sample data)
H m M z
f Current sample TIME
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List of symbols
Function EQP titration Learn titration EP titration(Ipol/Upol) EQP titration (Ipol/Upol) Two-phase titration*
Symbol ET1
Definition Initial potential of the measured solution before the first addition of titrant in the defined unit of the sensor used Potential after predispensing in the defined unit of the sensor used Titrant consumption in mL up to the equivalence point or end point; the equivalence points are numbered consecutively Titrant consumption in mmol up to the equivalence point or end point; the equivalence points are numbered consecutively. Q = VEQ * c * t Calculated excess of titrant in mL Calculated excess of titrant in mmol Total titrant consumption in mL (VEQ + VEX) Total titrant consumption in mmol (Q + QEX) Calculated equivalence point potential of the equivalence or end point VEQ in the defined unit of the sensor used Calculated half neutralization value (potential at VEQ/2) referred to the equivalence point VEQ in the defined unit of the sensor used Number of equivalence points found (applies to one Titration function) Potential 1 in the defined unit of the sensor used (evaluation parameter) Potential 2 in the defined unit of the sensor used (evaluation parameter) Titrant consumption in mL up to potential P1 or potential P2 Titrant consumption in mmol up to potential P1 or potential P2
ET2 VEQ
VEX QEX VEND QEND EPOT
EQP titration EQP titration (Ipol/Upol) Two-phase titration*
EHNV
neq P1 P2 VP1 VP2 QP1 QP2 * Two-phase titration: Special methods
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List of symbols
Predispensing to a: Volume or (factor x sample size) b: Potential c: Slope
E [mV] neq = 3 EPOT3 EHNV3 3
Example of an EQP titration with 3 equivalence points
EPOT2 EHNV2 EPOT1 EHNV1 VEQ1 Q1 VEQ2 Q2 VEND QEND 1
VEQ3 Q3
VEX QEX
V [mL]
E [mV]
+200 P1 +100
Example of an EQP titration with evaluation of the defined potential values
-100 P2 -200 VP1/QP1 V [mL] VP2/QP2
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List of symbols
Function pH/mV-stat
Symbol VTOT QTOT VT1 VT2 VT QT1 QT2 QT CSTAT VSTAT QSTAT
Definition Total titrant consumption in mL Total titrant consumption in mmol Titrant consumption in mL up to time limit t1 or time limit t2 Titrant consumption in mL up to a different time limit Titrant consumption in mmol up to time limit t1 or time limit t2 Titrant consumption in mmol up to a different time limit Correlation coefficient of the regression lines between t1 and t2 of the V t curve Mean titrant consumption in mL/min within the time limits t1 and t2 Mean titrant consumption in mmol/min within the time limits t1 and t2
V [mL]
V/ tt[mL/s] V/ [mL/s]
VTOT QTOT VT2 QT2 VT1 QT1
VSTAT QSTAT
t [s] t1 t2 t1 t2
t [s]
Note: VSTAT/QSTAT is determined by means of linear regression of the measured values between t1 and t2. CSTAT is the correlation coefficient of this linear regression. For a correct result, CSTAT should be greater than 0.95.
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List of symbols
Function Measure
Symbol E
Definition Measured value in mV or in the defined unit of the sensor used (does not apply to polarized sensors) Total dispensed volume in mL Total dispensed amount of substance in mmol Calculated result Calculation constant Calculation constant (applies only to the auxiliary function "Perform calculations") Mean value of the statistics evaluation (calculated only when the Statistics parameter is defined) Standard deviation Relative standard deviation in % Measured temperature in C, F or K of the Pt sensor used
Dispense
VDISP QDISP
Calculation
R C Cx
x s srel Temperature* T
* Temperature: Special methods
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List of symbols
8.1.1
Compilation of the raw results Raw results Printed out when "Raw results" is selected in the report function no yes yes no yes yes no yes no no yes yes yes yes no no no yes no yes
Analysis/Function
Current sample Measure Dispense EQP/EP titration Learn titration EQP/EP titration (Ipol/Upol) Two-phase titration*
TIME E VDISP, QDISP ET1, ET2 VEQ, Q VEX, QEX VEND, QEND EPOT EHNV neq P1, P2 VP1, QP1 VP2, QP2 VTOT, QTOT VT1, QT1 VT2, QT2 VT, QT VSTAT, QSTAT CSTAT T
EQP titration EQP titration (Ipol/Upol) Two-phase titration*
pH/mV-stat
Temperature* Notes:
1. * Two-phase titration, Temperature: Special methods 2. To obtain the raw results which are not printed out as standard, assign these to the result R, e.g. R = QP1, R = VT1.
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Use of indices
8.2
Use of indices
As some functions can occur a number of times within a method and parameters can also appear a number of times within a function, indices are needed in addition to the parameter symbol (see Section 8.2.1: Compilation of the symbols by indexing forms). The titrator recognizes 4 different indexing forms: 1. Parameters without index These parameters include, e.g. c, t, M, ZERO, SLOPE, TIME. The parameters always refer to the current titrant, the current sensor or the current sample determination. The parameters of the functions which occur only once within the standard methods also do not need an index, e.g. E of the Measure function or VSTAT of the pH/mV-stat function. 2. Parameters of the form Xi Parameters which use an index without brackets are all those whose link with the method function is meaningless. This indexing form includes R, C and H. Example: R3: third result (see fourth indexing form) Note: R = R1 holds, in other words if the index = 1 it may be omitted. This also applies to the indexing forms under points 3 and 4. 3. Parameters of the form X [j] Index j is the function counter. This indexing form includes, e.g. VDISP, QEX and x. Example: QDISP[2]: Measured value of the second Dispense function (extract from standard method "2 Step titration (EQP)") After confirmation of the "Current sample", the titrator dispenses and determines the raw result QDISP of the first Dispense function. The titrator executes the Stir function, then
Dispense
Stir
EQP titration
the EQP titration followed by the
Calculation
first calculation function. To obtain the measured value QDISP as a result, set R1 = QDISP[1]. The titrator executes the second calculation function, then
Calculation
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Use of indices
Report
the Report function before it dispenses again and determines the raw result QDISP of the second Dispense function. The titrator runs the second Stir function, then the second EQP titration, followed by the third Calculation function. To obtain the measured value QDISP as a result, set R3 = QDISP[2].
Dispense
Stir
EQP titration
Calculation
4. Parameters of the form Xi [j] Index i is the number of times a parameter should be run within a function. Index j is the counter for the number of functions within a method. This indexing form includes Q, VEQ, EHNV and EPOT. Example: Q2[2]: mmol consumption up to the second equivalence point of the second EQP titration function. Extract from the standard method "2 Step titration (EQP)", which has been adapted for the determination of HCl, CH3COOH and NH4Cl with NaOH. (The 2 titration functions were selected as other values have been defined for the equilibrium controlled measured value acquisition in the determination of CH3COOH and NH4Cl.)
EQP titration
E [mV]
The titrator executes the first EQP titration function and titrates until the equivalence point of HCl. It determines, among other things, the mmol consumption Q1[1] and the mmol excess QEX[1].
EQP1
Q1[1] Q QEX[1] QEX.

V [mL]
Q1[1]
QEX[1]
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Use of indices
Calculation Formula .................................. Constant................................. Decimal places ...................... Result unit .............................. Result name ........................... Statistics.................................
R1 = Q1[1] 4 mmol HCl Yes
In the first Calculation function, you define the mmol consumption for HCl. As you can omit the Index 1, the formula can also be R = Q.
EQP titration
E [mV]
EQP1
The titrator executes the second EQP titration function. It determines, among other things, the mmol consumption Q1[2] up to the first equivalence point (CH3COOH), then the mmol consumption Q2[2] up to the second equivalence point (NH4Cl).
EQP2 V [mV]
Q1[2]
Q2[2]
R2 = Q1[2]+QEX[1] 4 mmol CH3COOH Yes
In the second (third) Calculation function, you define the mmol consumption for acetic acid. Here, you take into account the titrated excess of the first EQP titration function.
R3 = Q2[2] 4 mmol NH4Cl Yes
In the third (fourth) Calculation function you define the mmol consumption for NH4Cl.
Note: The two Dispense functions of the standard method are skipped (0 mL has been defined as volume in the method); the second Calculation function is skipped (no formula has been defined in the method for the result).
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Use of indices
8.2.1
Compilation of the symbols by indexing forms Symbol Unit Index Examples
Analysis/Resource / Function Current sample Titrant
TIME c t
[s] [mol/L]
Sensor
ZERO SLOPE
[mV, pH ...] [mV/ mV, pH ...] [g] or [mL] [g/mol]
Sample
m M z f
Auxiliary value Calculation
H R C E T VDISP QDISP ET1 ET2 VEX QEX VEND QEND [mV, pH ...] [C, F, K] [mL] [mmol] [mV, pH, A...] [mV, pH, A...] [mL] [mmol] [mL] [mmol] Xi
H1H20 R3 C2
Measure** Temperature* Dispense
X[j]
QDISP[2]
EQP/EP titration EQP/EP titration (Ipol/Upol)** Two-phase titration*
QEX[2]
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Use of indices
Function EQP titration EQP titration(Ipol/Upol)** Two-phase titration*
Symbol neq P1 VP1 QP1 P2 VP2 QP2
Unit
Index
Examples neq[3]
[mV, pH, A...] [mL] [mmol] [mV, pH, A...] [mL] [mmol] [mL] [mmol] [mV, pH, A...] [mL] [mmol] [mL] [mmol] [mL] [mmol] [mL/min] [mmol/min] VT1[2] X[j] Q[2]
EP titration EP titration (Ipol/Upol)**
VEQ Q EPOT
pH/mV-stat**
VTOT QTOT VT1 QT1 VT2 QT2 VSTAT QSTAT CSTAT
Calculation (Statistics)
x s srel
x[3]
EQP titration EQP titration(Ipol/Upol)** Two-phase titration*
VEQ Q EPOT EHNV
[mL] [mmol] [mV, pH, A ...] [mV, pH, A ...] Xi[j] Q2[1] EPOT1[2]
Note: The parameters of the functions which occur only once in a method do not need an index in "[ ]". * Temperature, Two-phase titration: Special methods; ** Measure, pH/mV-stat, EQP titration (Ipol/Upol), EP titration (Ipol/Upol): two or more of these functions are possible only with special methods.
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Evaluation procedures
8.3
The titrator has various evaluation procedures for precise determination of the equivalence points of a titration curve: Standard Minimum/maximum Segmented Asymmetric 8.3.1 Standard
You use this procedure for all S-shaped titration curves. The evaluation uses an iterative procedure (nonlinear regression) [1]. The titration of a strong acid with a strong base is used as a mathematical model. With this model, the determined equivalence point always lies in the vicinity of the inflection point.
E
Inflection point
At least five measured points around the the inflection point are used for the evaluation. The slope from measured point to measured point must increase or decrease. If this condition is not met, the iterative procedure can not be employed. In such a case, the inflection point of the titration curve is determined by interpolation. A reference to this effect appears in the report of the "raw results".
V
8.3.2
Minimum/maximum
The result of this evaluation is the calculated minimum (maximum) from the measured points of the titration. The classical example of a titration curve with a minimum is the determination of surfactants with photometric indication. The minimum (maximum) is calculated by a polynomial approximation of the titration curve in the region of the minimum (maximum). The equivalence point is recognized directly using the data of the titration curve.
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8.3.3
Segmented
Different indication methods (e.g. photometry, conductometry and amperometry) generate titration curves with linear or approximately linear segments (segmented curves). The titrator also evaluates these curves. The evaluation procedure used is based on the following consideration:
E Titrierkurve Titration curve
The first derivative of a segmented curve has the typical shape of an Sshaped curve, its inflection point represents a good approximation of the equivalence point.
V E/V
1st derivative 1. Ableitung
Segmented curves are evaluated with the Standard procedure, which uses the calculated data of the first derivative instead of the data points of the titration curve. The equivalence point recognition is thus effected not with the calculated first derivative but with the calculated second derivative. The threshold for the equivalence point recognition also refers to data of the second derivative. The individual segments do not need to be exactly linear. Decisive for an accurate determination of the equivalence point is the presence of a clear kink between the individual segments of the titration curves.
V 2E/V2 2. Ableitung 2nd derivative
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8.3.4
Asymmetric
With pronounced asymmetric curves, the standard procedure can lead to a systematic error. The difference between the true equivalence point and the inflection point can then be greater than the precision normally attained. For these cases, the titrator is equipped with the evaluation based on the Tubbs method [2]. This empirical approximation method is a tried and tested procedure for the evaluation of asymmetric, analog recorded titration curves. It can also be applied to titration curves measured digitally. The result of the Tubbs evaluation provides a better approximation of the true equivalence point than the inflection point. The evaluation procedure is based on the following considerations:
E
M2
Intersection point EQP M1
A circle of curvature with minimum radius can be drawn on both branches of the titration curve. The ratio of the two radii is determined by the asymmetry of the curve. The mean intersection point of the line connecting the centers of the circles M1 and M2 with the titration curve represents the sought-after equivalence point. Theoretical calculations show that the true equivalence point with asymmetric titration curves always lies between the inflection point and that branch of the titration curve which has the greater curvature (the smaller radius of curvature).
In the titrator the calculation is implemented according to Ebel [3]. This involves approximating those parts of the titration curve which lie in the region of the greatest curvature by a hyperbola. The vertex is determined for each approximated hyperbola. This point on the hyperbola lies at the site of greatest curvature. The mid-points of the assigned smallest radii of curvature are the focal points of the two hyperbolae. As in the graphical variant, the intersection point of the line connecting the two focal points with the titration curve results in the required equivalence point. For the evaluation at least six measured points both before and after the inflection point of the titration curve are required in the region of the greatest curvature. If the titration curve has a profile which does not allow calculation of the radii of curvature, the titrator calculates the equivalence point by the standard procedure. This will be indicated in the report of the "raw results".
[1] [2] [3] 8-16
K. Waldmeier and W. Rellstab, Fres.Z.Anal.Chem., 264, 337, (1973) C.F. Tubbs, Anal. Chem., 26, 1670 (1954) S. Ebel, E. Glaser, R. Kantelberg and B. Reyer, Fres. Z. Anal. Chem., 312, 604 (1982)
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Examples of formulas
8.4
8.4.1
Results Content of a sample with weighing % ppm, mg / g, TAN [mg KOH / g], mol / kg, mmol / g Content of a sample solution % (g/mL), g / L, ppm, mg / L, g / 100mL, mol / L, mmol / L
R = Q C / m (standard formula) C = f (M, z, unit)
R = m / (VEQ c C)
Titer determined with primary standard Titer determined with volumetric standard Content per sample mmol consumption as result mL consumption as result mL consumption per unit weight or per unit volume as result Back titration: QDISP: dispensed amount of substance in mmol of the Dispense function Q: mmol consumption up to the equivalence point or end point of an EQP or EP titration function. Solvent blank value included in the calculation (blank value is stored as auxiliary value Hj ) Matrix blank value included in the calculation [mmol / g] (matrix blank value is stored as auxiliary value Hj) Initial potential of the second EQP or EP titration function as result Ion concentration in mmol/L, measured with an ionselective electrode Extinction of a solution, measured as % transmission with a phototrode
R = QC R=Q R = VEQ R = VEQ / m R = (QDISP Q) C / m
R = (Q Hj) C / m R = (Q / m Hj) C
R = ET1 [2] R = pw(E) 1000 R = lg(E)
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8.4.2
Constants Unit mg / g or g/L % % (g/100 mL) ppm (mg/kg) ppm (mg / L) mol / kg (mmol / g) TAN and TBN (mg KOH / g) Titer mmol / L mol / L
Weight or volume of the sample known C = M/z C = M / (10 z) C = M / (z 10 ) ... ( = density of the solution) C = M 1000 / z C = M 1000 / (z )...( = density of the solution) C = 1/z C = 56.1 C = M / (1000 z) C = 1000 C=1 Volume and weight of the sample unknown C = M/z C = 1/z
mg mmol
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8.4.3
Formulas for restriction of the equivalence point
To calculate the titrant consumption in mmol of a particular equivalence point when a titration curve has several equivalence points, you can have Q identified by a condition, e.g. R1 = Q(EPOT > -50) Titrant consumption up to the equivalence point of the 1st EQP titration function whose potential is above -50 mV. Here, the equivalence point which first meets this condition is determined. Equivalence points whose potential lies between, e.g. -51 and -300 mV are not considered. Titrant consumption up to the equivalence point of the 2nd EQP titration function whose potential lies above -50 mV. Titrant consumption up to the equivalence point of the 2nd EQP titration function whose potential is nearest to 100 mV. Titrant consumption up to the equivalence point of the 1st EQP titration whose potential is nearest to potential P1. Titrant consumption up to the equivalence point of the 1st EQP titration function whose value is nearest to the value stored under auxiliary value H11. Titrant consumption up to the equivalence point of the 1st EQP titration lying within the range of potential P1 and 300 mV. The equivalence point which first meets this condition is determined.
R1 = Q(EPOT > -50)[2]
R1 = Q(EPOT ~ 100)[2] R1 = Q(EPOT ~ P1) R1 = Q(EPOT ~ H11)
R1 = Q(P1 < EPOT < 300)
Note: You can also define these conditions with VEQ or EPOT, e.g. R 1= EPOT(VEQ ~ 5).
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Restrictions
8.5
8.5.1
Restrictions in the analysis

Maximum number of samples
The sample data of maximum 60 samples can be entered.
8.5.2
Maximum number of sample series in the sample data memory
DL50/DL53: Maximum 1 sample series can be entered. DL55/DL58: Maximum 3 sample series can be entered.
8.5.3
Maximum number of equivalence points per sample determination
Per sample determination, the titrator can determine maximum 16 equivalence points (EQP titration), divided between one or two EQP titration functions. If there are more than 16 equivalence points, these will not be determined, but the determination will be continued.
8.5.4
Maximum number of measured values per Titration function
The titrator can store 300 measured values per titration function (EQP, EP, Learn, EQP (Ipol/ Upol), Two-phase); it then aborts the function. With the titration functions EP (Ipol/Upol) and pH/mV-stat, the number of measured points will be reduced automatically (see Sections 3.3.10 and 3.3.11).
8.5.5
Maximum number of results per sample series
The titrator can store 180 results per sample series; it then aborts the series. Example: If you titrate 40 samples with a method, the titrator can store 4 results for each individual sample.
8.5.6
How long does the titrator store data?
1. Measured values of the titration functions The titrator stores the measured values up to the next titration function or up to the start of the next sample determination. 2. Raw results The titrator stores all raw results up to the titration of the next sample within a series. 3. Results The titrator stores all results of a sample series up to the start of a new series.
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Error messages and malfunctions
Contents
Page 9. 9.1 9.2 Error messages and malfunctions .......................................................... Error messages from the titrator ............................................................. Other errors and malfunctions ................................................................ 9-3 9-3 9-6
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9-1
9-2
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9.
9.1

Error messages from the titrator
You yourself can rectify all errors which the titrator displays as messages. Some of these messages refer to this section (errors 1...6). However, if the EPROM or RAM test following startup of the titrator failed ("test failed"), the only measure available is: "Press any key to continue". The program memory or the program data memory is faulty. After any key has been pressed, the titrator attempts to continue the startup process: This may be successful, but does not necessarily guarantee 100% perfect operation. Measure: Please contact METTLER TOLEDO service! 1. Internal ERROR: ... (error which should be noted down, e.g. PB, M1) Parts of the hardware may be faulty. Measure: Before you contact METTLER TOLEDO service, note the fault and the operation which initiated it, note the instrument number of the titrator (rear panel) print out the system information, which provides details of the titrator equipment: Press the shift and <F4> keys to print out the information. Finally, inform the service of these points and the attached peripherals with the defined configuration. 2. Memory faulty Parts of the user data memory are faulty. Measure: Call METTLER TOLEDO service to have the memory changed. Meanwhile, you can still continue working with the titrator. 3. Faulty data deleted a. The titrator has stored only parts of a method, e.g. as the power failed during storage of this method. It deletes the entire method (it is also possible that it has deleted several methods). As a result, the sample data of this method which are stored in the sample data memory will also be deleted. Measure: Confirm the message. Check which of your methods have been deleted and reenter.
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b. The titrator has stored only parts of parameters of a resource, e.g. as the power failed during storage of these parameters. It deletes the entire list of this resource (e.g. all titrants or all sensors). Measure: Confirm the message. The titrator now loads the default list of the deleted resource, e.g. all titrants stored in the titrator in the factory. Check which list has been changed: If the user data memory has insufficient storage space, only the titrants which can be accommodated in the available space will be stored. If the memory is full, the titrator will not store any titrants. In such a case, you must delete data of other resources or one of your methods to create memory space. Switch the titrator off then on again. Check that all resources are again available. If the error messages appears repeatedly, inform METTLER TOLEDO service!
4. Storage not possible a. The titrator can not assign the titer, the auxiliary value or the calibration data to the corresponding resources as the list is missing (titrant, sensors or auxiliary values). Measure: Confirm the message. Check whether the list of the resource has been deleted. Switch the titrator off then on again: The titrator will then reload the default list of the corresponding resource, e.g. all the titrants which were stored in the titrator in the factory. If the user data memory has insufficient storage space, only the titrants which can fit in the available space will be stored. If the memory is full, the titrator will not store any titrants. In such a case, you must delete other resources or one of your methods to create storage space. Switch the titrator off then on again. Check that all resources are again available. b. The titrator can no longer store, e.g. data as the user data memory is full. This is possible with resources which you wish to add in the Setup menu in the case of a method you generate in the Method menu with sample data you wish to enter in the Sample menu on storage of a changed, active method on storage of the evaluation parameters of the titration functions EQP, EQP (Ipol, Upol) and Two-phase of an active method (parameter: "Stop for reevaluation").
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Measure: Confirm the message. Delete methods or resource data or copy to a memory card. 4 c. The titrator performs a learn titration. If the method for this is stored on the memory card or in the computer, the parameters of the function are not stored. Measure: Confirm the message. Always perform a learn titration with a method stored in the titrator and do not remote-control the titrator! If the error message appears repeatedly, contact METTLER TOLEDO service! 5. Error: Memory card a. An error appears during copying. Measure: Confirm the message. Check that the card is inserted properly and restart the copying process. If the process is aborted again, reformat the memory card and attempt to repeat the copying process (the data on the card will be deleted). If the process is again aborted, use a new memory card. b. An error appears when a memory copy is loaded. Measure: Confirm the message. Check that the card is inserted properly and restart the copying process. If the process is again aborted, switch the titrator off then on again. Use a new memory card. 6. Measuring inputs not adjusted (refers only to a pH option on which the calibration data are not stored, see Section 6.7.2). The calibration data for the characteristic line of the measuring inputs are missing. Measure: Enter the data from the data sheet enclosed with the pH option (see Section 6.7.2). When the measuring inputs are adjusted, this message appears if system data have been deleted in the user data memory. Measure: Switch titrator off then on again: the system data will be reloaded. Reenter zero point and slope for all measuring inputs.
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9-5
9.2
Other errors and malfunctions
The following compilation of errors and malfunctions are not reported by the titrator and may frequently help you rectify the faults yourself without the need to contact METTLER TOLEDO service. If you have to contact the service, please print out the system information to obtain details of the titrator equipment and pass these data on to the service: Press the Shift and <F4> keys to print out the information.
Fault
No display on titrator
Possible cause
Titrator not connected to power supply
Rectification
Connect to power supply, if fault persists contact METTLER TOLEDO Service Contact METTLER TOLEDO Service Contact METTLER TOLEDO Service
Several points of the display missing Display does not match the pressed key Stirrer does not rotate Stirrer not properly assembled or sensors block it at the titration stand Peripheral faulty or switched off Device not switched on Wrong settings Configuration (switch settings) wrong Burette drive faulty
Check stirrer and seating of the sensors
Transfer error to attached peripheral Device (printer, balance, terminal) at Centronics or RS interface do not react
Check attached device is functioning properly Switch on device Settings and configuration must match (see Section 2.7) Contact METTLER TOLEDO service Check electrode (see electrode data sheet) Check defined data Use new electrode Clean burette tip Insert follower cam correctly (see Section 10.2.3)
Burette does not move to zero position when switched on Wrong potential or pH values
Electrode faulty Calibration data wrong
No dispensing, the titrant is discharged from stopcock or piston
Burette tip clogged Follower cam on burette mounted wrongly
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Installation and maintenance
Contents
Page 10. 10.1 10.2 10.2.1 10.2.2 10.2.3 10.2.4 10.2.5 10.3 10.4 10.5 10.5.1 10.6 10.7 10.8 10.8.1 10.9 Installation and maintenance ...................................................................... 10-3 Installing the burette drive .......................................................................... 10-3 Installing and maintaining the interchangeable burette ........................... 10-4 The DV1001, DV1005, DV1010, DV1020 burettes ........................................10-4 Equipping the burette .....................................................................................10-5 Inserting the burette .......................................................................................10-6 Maintaining the burette parts ..........................................................................10-7 General information ........................................................................................10-8 Equipping the titration stand ...................................................................... 10-9 Rear view of the titrator ............................................................................. 10-10 Installing the sensor, Centronics or RS option ....................................... 10-11 Calibration data for the characteristic curve of the measuring inputs ..........10-12 Inserting the memory card ........................................................................ 10-12 Using TTL inputs and outputs .................................................................. 10-13 Attaching a keyboard ................................................................................. 10-15 Attaching a bar-code reader .........................................................................10-16 Configuration of the terminal (DEC VT340) ............................................. 10-16
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10-1
Burette drive
10.

Switch the titrator off and disconnect the power cable before you open the housing! An electric shock could be lethal.
You can clean the housing of the titrator with a cloth moistened with ethanol.
10.1
Installing the burette drive

Screw
Position 2
Unscrew the burette guide at position 2. Pull out the ribbon cable that is located in the titrator below this second opening.
Note Please place the burette drive on the second opening. DL50/DL53 The burette drive is defined as the middle position by the software (drive 2), in other words you can not control a drive installed at position 1. DL55/DL58 For the first titration, which you perform in accordance with the instructions in the Quick Guide, the 2nd burette drive is defined.
Plug the coupling of the ribbon cable in the connector of the burette drive.
Coupling Ribbon cable Connector
Position the burette drive on the second opening of the titrator from the first opening press the ribbon cable downward at an angle (ensure it is not pinched!) and fasten with the screw. Screw the burette guide to the first opening.
Ribbon cable
DL55/DL58 If you wish to use a second burette drive, follow the above procedure: Unscrew the burette guide at position 1 etc.
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10-3
Interchangeable burette
10.2
10.2.1
Installing and maintaining the interchangeable burette

The DV1001, DV1005, DV1010, DV1020 burettes
The 5, 10 and 20 mL burettes differ only in the size of their cylinder, centering ring and piston, whereas the 1 mL burette has a different construction: its piston is longer, piston guide and cylinder holder ''replace'' the centering ring of the other burettes. Instead of the locking screw, its glass cylinder is fastened with an O-ring and a knurled nut.
1 mL burette
5 / 10 / 20 mL burette
Connection tubing
Knurled nut Stopcock O-ring Stopcock Locking screw Cylinder holder Glass cylinder Piston Piston rod Piston guide Protection tube Piston Piston rod Burette housing Centering ring Lip seals
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10.2.2
Equipping the burette
Lay gasket on bottle and screw on burette holder. Insert stopper (or a drying tube with holder). Caution: If you use a stopper as protection for the titrant, always use the stopper with flat side! Otherwise a partial vacuum forms in the bottle (order no. 23646). Push suction tubing into the bottle, slide the red PVC tubing over the fitting as kink protection, and fasten other end to left connection of burette head. Screw dispensing tubing into connection at right and place burette tip in tip holder.
Suction tube Dispensing tube
Tip holder
Burette assembled Stopper Burette holder Gasket
1 L bottle
Fitting
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10-5
10.2.3
Inserting the burette Slide the burette onto burette drive 2 with the stop of arrestment knob (1) located on left side. Check that piston rod (2) is correctly positioned in push rod (3). Fix burette by turning the arrestment knob to the right.
3 1
Note Before sliding the burette onto the titrator, check the exact position of the stopcock and the piston rod. If the piston has been pushed too far into the cylinder, carefully take it out a short way. Then press the burette onto the burette holder thus positioning the piston exactly. Piston must project 7 mm!
Position of the valve
Position of the piston
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10.2.4
Maintaining the burette parts
Depending on the titrant, you should clean the burette cylinder, piston, stopcock and tubing relatively often. Slide the burette off the titrator, invert it so that the stopcock points towards you and carefully take out the piston; this causes the burette contents to flow out through the suction tubing (waste or titrant bottle!). In the same position, turn the stopcock through 90 clockwise and any liquid in the stopcock will flow out through the dispensing tubing (waste bottle!). Unscrew the suction, dispensing and connection tubing. 1 mL burette Unscrew the knurled screw of the burette and remove the O-ring from the glass cylinder using tweezers. Unscrew the holder of the glass cylinder and take out the cylinder. Caution: Do not misplace O-ring! 5, 10, or 20 mL burette Unscrew the locking screw of the burette and take out the glass cylinder. Caution: Do not misplace the centering ring of the burette housing!
Press the cam of the stopcock inward and lift the stopcock up and out.
Cam
Depending on the contamination caused by the titrant, rinse cylinder and tubing with acids or deionized H2O then with ethanol and finally dry the parts with oil-free compressed air or vacuum. Rinse the stopcock with solvents or deionized H2O only! Then dry it with oil-free compressed air. Never place O-rings in organic solvents! Never attempt to remove any crystals in the cylinder by scratching with a hard object! Pipe cleaners or Q tips are more suitable. Never put the parts in a drying oven whose temperature is above 40 C! Replace the piston if it leaks or is badly scored at the edge. Pay special attention to crystal formation between the lip seals of the piston if you work with NaOH/KOH and KF solutions!
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10.2.5
General information
You can remove air bubbles at the piston surface by taking the burette out of the guide and lightly tapping its base. This causes air bubbles to rise to the top. Then rinse the burette. You can remove air bubbles in the tubes by tapping the tubes with your fingers while titrant is being siphoned off or dispensed. If this does not help, undo the suction tube so that titrant flows back into the bottle, screw it on again and rinse the burette (air purging). In obstinate cases undo both tubes, rinse with deionized H2O and ethanol and dry using oil-free compressed air or vacuum. Titrants such as KMnO4 or KOH in MeOH can easily crystallize in the tip of the burette and block it. If you have no immediate use for a titrant, it is best to empty and clean the dispensing tube: Unscrew connection to let the titrant flow out. Check the threaded connection and wipe off any drops. KF titrants are subject to outgassing, above all at elevated room temperatures (SO2), which leads to the formation of air bubbles in the tubes and in the burette (stopcock). You should thus rinse these burettes before titrations!
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Titration stand
10.3
Equipping the titration stand

Screw on titration arm (1) with nurled screw (2). Insert stirring rod (3) and attach propeller stirrer (4) from below to rod. Press spacing ring (5) onto titration head, place clamping ring (6) in threaded ring (7) and screw into place. To install a titration vessel, turn the threaded ring half a turn to the left, attach the vessel and tighten threaded ring. Insert burette tip (8) and electrode (9) diagonally opposed this ensures better control in the titration and close the remaining openings with stoppers (11 & 12). (9a) is the plug-in electrode cable. (10): This opening is intended for the rinsing bottle connection. (13) is the electrode holder.
3 9a
9 13 8 10
12
11
5 6 4 7
Always test the titration vessel for firm seating in the titration head! If it falls off, you could injure yourself if working with toxic titrants and solvents or strong acids or bases.
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10-9
Rear view
10.4
Rear view of the titrator

Slot: No. 1 No. 2 No. 3 No. 4
TTLIO socket TTLIO socket (used by titrator) RS232 interface for sample changer RS232 interface for balance Centronics interface for printer RS232 interface for system
Input: Reference electrode Sensor inputs: Sensor 1 Sensor 2 Temperature sensor input: Temp 1 Stirrer outputs: Stirrer 1 Stirrer 2 Analog outputs
pH
KF
RS
Centronics option
Connector for power cable
On/off switch
The diagram shows a possible occupancy of all slots. The basic version of the titrator has the following installed a pH option at slot No. 1 an Centronics option at slot No. 4. pH and KF options You can install a sensor option in any slot. Each option has a number which is also affixed to the data sheet enclosed with each sensor option (see Section 10.5.1). DL53/55/58: You can use the inputs and outputs of maximum four sensor options, e.g. two pH options at slot No. 1 and 2, two KF options at slot No. 3 and 4. DL50: You can use the inputs and outputs of maximum one sensor option. Centronics option You can use the Centronics option only if it is installed in slot No. 4. The TTL inputs and outputs of the socket can be used only for the commands preallocated by the titration software (see Section 10.7).
10-10
08/2004
Installing options
RS options You can install an RS option either in slot No. 3 or slot No. 4. Although the options are identical, the functions of the connections are not! Slot No. 3: You can freely control the TTL inputs and outputs of the socket. To the upper RS interface you can attach only a sample changer, to the lower only a computer or a terminal. Slot No. 4: You can use the TTL inputs and outputs of the socket only for the commands stipulated by the titration software (see Section 10.7). To the upper RS interface you can attach only a balance, to the lower only a printer.
10.5
Installing the sensor, Centronics or RS option

Switch the titrator off and disconnect the power cable before you unscrew the cover plate of the slot! An electric shock could be fatal.
Unscrew the cover plate of the slot. Insert the option in the two guide rails, push in option and fasten with the two screws. Notes 1. When you have installed a pH option that has not stored the calibration data you should enter the calibration data for the characteristic line of the measuring inputs (see Section 10.5.1). calibrate the electrodes/temperature sensors at the new inputs (see Sections 2.2 and 6.1.3).
Soldering scheme
2. To attach temperature sensors of other companies, you can use a Lemo cable plug (4-pin) and solder on the appropriate cable (see Section 11.2: Accessories).
2 3
1 4
Shield
Pt100/Pt1000 sensor
08/2004
10-11
Memory card
10.5.1
Calibration data for the characteristic curve of the measuring inputs
When the titrator is delivered, the measuring inputs are calibrated for a sensor and temperature sensor (Pt100 and Pt1000) of the pH option. The data sheet filed in Section 14 documents the data for the characteristic line of the measuring inputs of this pH option. If the data are not stored on the actual option, you must reenter them (see Section 6.7.2) if system data are lost (see Section 9.1) if you install this option in a different slot. If you order an additional pH option, you receive a data sheet with the number of the option and the calibration data for its measuring inputs. You must enter these data for correct potential and temperature measurements if they are not stored on the actual option (see Section 6.7.2). The data for the characteristic line of the measuring inputs are always stored on KF options! Note: As the characteristic line of the measuring inputs can exhibit long-term drift, we advise you to have the inputs recalibrated every 2 years by METTLER TOLEDO Service.
10.6
Inserting the memory card
Note: Ensure that you are not electrostatically charged when you perform this operation! We recommend you touch the metallic part of the titrator housing before you insert the memory card to ensure the charge is not transferred to the titrator interior. Swing open the cover (1) of the slot for the memory card. Push in the memory card until knob (2) springs out. To remove the card, press the knob back in.
10-12
08/2004
TTLIO
10.7
Using TTL inputs and outputs
The TTLIO socket of the Centronics option has two inputs and four outputs (In 1/In 2 and Out 1...Out 4). These are assigned by the titrator to commands which are triggered during an analysis. You can wire these inputs and outputs mechanically or electronically to trigger the defined commands by auxiliary units or systems (see following examples). The RS option has the same TTLIO socket as the Centronics option. When it is installed in slot 3, the inputs and outputs are always available and freely configurable (see Sections 6.7.5 and 6.7.6). At slot 4, they are assigned by the titrator to commands which you trigger during an analysis: Socket
1 8 5 7 6 2 3 4
Assignment (see Section 12.10.2: Technical data) GND (Pin 1) ...... In 1 (Pin 2) ........ In 2 (Pin 3) ........ Out 1 (Pin 4) ..... Out 2 (Pin 5) ..... signal ground triggers the start of the analysis or confirms the mask "Current sample" (titration stand 1, 2 or external) triggers the abort of the analysis (Reset) gives a pulse after the sample function the output signal assumes a "low" status during the titration; this does not change until the sample is analyzed (on display of the result list) the output signal assumes a "low" status in the case of an error message; this does not change until the message has been confirmed with OK supply voltage on request for the next sample of a series, this triggers a pulse (only with titration stand 1, 2 or external)
Out 3 (Pin 6) .....
VCC (Pin 7) ...... Out 4 (Pin 8) .....
Wiring mechanically If you wire, e.g. pin 1 (ground) with pin 2 (input 1) by attaching a manual event sensor, you can initiate the start of the analysis with this switch. The mask "Defined are" must be blocked from the analysis sequence for this as it can not be confirmed (see Section 6.7.3).
In Event sensor GND
08/2004
10-13
TTLIO
Wiring electronically Input In 1 or In 2

Titrator external
Output Out 1, Out 2, Out 3 or Out 4

Titrator external
Out
In
GND
GND GND
Output Out 1, Out 2, Out 3 or Out 4 Relay supply internal (relay operate voltage: max. 3.5 V); Icc: max. 60 mA
Titrator external Relay VCC
Relay supply external
Titrator
external Relay
Out
Out
GND
Note: TTL are signals which do not transfer power. To operate, e.g. a pump it is necessary to connect an amplifier in the circuit.
10-14
08/2004
External keyboard
10.8
Attaching a keyboard
A DIN socket is located on the left side of the titrator and can be used for the attachment of an external keyboard for alphanumeric entries. Attach the keyboard using the appropriate DIN cable (see Section 12.10: Technical data). The following table shows the keys and key combinations which correspond to the command, menu, auxiliary function and entry keys of the titrator: Titrator key
F1 F2 F3 F4 F5 Setup Method Sample Run Sensor Stirrer Changer Burette Results Report Misc... Data Transfer Reset Arrow key / Shift + Arrow key / Shift + Shift 1...9, . Del CE (Shift + Del) Break (Pause) / Page up / Page down Shift 1...9, . Del Shift + Del (b)1...9 (a)1...9
External keyboard key

F1 F2 F3 F4 F5 F12 F10 F11 F9 e s c b r p m d
<Alt> + key
<Ctrl>+ key
The characters /, -, +, =, etc., which are written with the Shift key, depend on the assignment of the keyboard. Additional characters not on the titrator keypad are: x <Alt Gr> + x <Alt Gr> + u <Alt Gr> + d
08/2004
10-15
Bar-code reader/terminal
10.8.1
Attaching a bar-code reader
You can attach a bar-code reader to the external keyboard. To ensure this is recognized by the titrator, you must program a "header" and "terminator" with the external keyboard (see Operating Instructions of the keyboard in question). The titrator requires the key sequence "Shift"/"Enter" for both parameters. You can then read in, e.g. the bar code for the sample identification without having to define the bar-code reader in the Setup menu. You must define the bar-code reader if you wish to use it for direct data transfer to a computer (see Section 2.7.3).
10.9
Configuration of the terminal (DEC VT340)
You have attached the terminal to the titrator and defined it (see Section 2.7.3). To configure it, proceed as follows: Switch off the titrator. Switch on the terminal and wait until the message VT340 OK appears. Press the Set-Up key: The SET-UP DIRECTORY appears. a. If you have already configured the terminal for other connections, first select Recall Factory Default Settings to reactivate the default settings. b. If you have not yet used the terminal, you can change some of the default parameters directly. Select General Set-UP and change the following parameters: Terminal mode VT300-8bit Select Display Set-Up and change the following parameters: Scrolling jump Status Display host writable Select Communications Set-Up and change the following parameters: Transmit Speed 9600 * Receive XOFF Point 512 Character Format 8 bits, even parity * * These parameters must match the defined terminal settings! (See Section 2.7.3) Select Keyboard Set-Up and change the following parameters: Keypad mode numeric, so that the numeric keys of the numeric key field (on extreme right of keyboard) are active.
10-16
08/2004
Terminal
Select Save Current Settings to save the modified parameters. Press the Set-Up key to quit the SET-UP DIRECTORY. Switch on the titrator: The terminal screen is now built up by the titrator. If you have switched off both instruments, first switch on the terminal, then the titrator. You can use the keyboard of the terminal to operate the titrator. The keys have the following assignments: Titrator key F1 F2 F3 F4 F5 Setup Method Sample Run Sensor Stirrer Changer Burette Results Report Misc... Data Transfer Reset Arrow key / Shift + Arrow key / Shift + Shift 1...9, . Del Shift + Shift + F20 / Prev. screen / Next screen Shift 1...9, . Remove key F6 F7 F8 F9 F10 F14 F12 F13 F11 8 5 4 7 3 2 1 6 Terminal numeric key field
08/2004
10-17
Accessories
Contents
Page 11. 11.1 Accessories .................................................................................................. 11-3 Standard equipment .................................................................................... 11-4 Small accessories .......................................................................................... 11-6 Optional accessories ................................................................................... 11-7 Burette drive ................................................................................................... 11-7 Interchangeable burettes ............................................................................... 11-7 Additional parts for the burette ....................................................................... 11-9 Titration stands ............................................................................................... 11-9 Additional parts for the titration stand ........................................................... 11-11 Sensors ........................................................................................................ 11-13 Temperature sensors ................................................................................... 11-15 Accessories for Karl-Fischer titrations .......................................................... 11-15 Peripherals ................................................................................................... 11-16 Titration software .......................................................................................... 11-16 Miscellaneous .............................................................................................. 11-17 Options ......................................................................................................... 11-19 Documentation ............................................................................................. 11-19 METTLER TOLEDO literature and application brochures ...................... 11-20
11.2
11.3
08/2004
11-1
Accessories
11.
Accessories
All instrument components of and working aids for the titrator that form part of the standard equipment and the optional accessories are listed below. Each part that is listed with an order number can be ordered from METTLER TOLEDO.
08/2004
11-3
Accessories
11.1
Standard equipment
Interchangeable burette (DL50 Graphix/ DL50 Rondolino only)
Propeller stirrer
Rondolino (DL50 Rondolino only)
11-4
Burette drive
Titration stand (DL50 Graphix only)
Electrode holder (DL53/DL55/DL58 only)
08/2004
Accessories
DL50 Graphix Titration stand Rondolino Electrode holder Burette drive DV90 Interchangeable burette (10 mL) DV1010* Propeller stirrer incl. 2 stirring rods pH option Centronics option RS option Titration Software LabX light Power cable Electrode cable Printer cable RS connection cable Reference Handbook Quick Guide Memo card Application broschure No. 12 Small accessories * see optional accessories x
DL50 Rondolino x
DL53 DL55 DL58
x x* x x x x x x x x x x x x x
x x* x x x x x x x x x x x x x (see next page)
x x
x x x x x x x x x x x x x
08/2004
11-5
Accessories
Small accessories (Order No.) 2 knurled screws (25650) Threaded ring (25652) Clamping ring (25653) Spacing ring (23842) Titration vessel (Set) 2 electrode holder (25654) 3 stoppers ST 14.5 (23451) 2 stoppers ST 7.5 (23452) Stopper holder (25662) Phillips screwdriver No. 2 (73072) Operating Instructions LabX light
DL50 Graphix x x x x x x x x x x x
DL50 Rondolino x
DL53 DL55 DL58 x
x x x x x x x x x x x x x
11-6
08/2004
Accessories
11.2
Optional accessories
The numbers enclosed in parentheses refer to the purchase order, e.g. of an interchangeable burette. In case of additional orders some parts are available only in multipack form or as a minimum quantity. Order No. Burette drive Burette drive DV90
Interchangeable burettes Interchangeable burette, complete 1 mL 5 mL 10 mL 20 mL DV1001 DV1005 DV1010 DV1020
comprising: 1 L brown glass bottle (1)
71296
and Burette holder (1) and Piston (1)
23645
DV1001 DV1005 DV1010 DV1020
51107535 51107115 51107116 51107117
08/2004
11-7
Accessories
Order No. and Stopcock (1) with valve disk1) made of: PTFE (light-gray) (standard equipment of interchangeable burette) ceramic (dark-brown) (optional accessories)
1) Both valve disks are chemically resistant. For 24-hour use with titrants that
51107537 51107525
have a tendency to cristallize out, we recommend the ceramic disk.
and Light protection tube (1) and Dispensing tube (1) with siphon tip
23644
0.70 m
25687
and Suction tube (1)
0.83 m
25688
and Gasket (1) for 1 L brown glass bottle and Tip holder (1) for burette tip and Stopper ST 14.5 (1)
min. order quantity: 5
23981
23960
min. order quantity: 5
23646
and
HCl c= Date: mol/L HCl c= Date: mol/L NaOH c= Date: mol/L NaOH c= Date: mol/L AgNO3 c= Date: mol/L AgNO3 c= Date: mol/L
1/2 H2SO4 c= Date:
mol/L
1/2 H2SO4 c= Date:
mol/L
KF c= mg H2O/mL Date:
KF c= mg H2O/mL Date:
Set of labels (1)
51107506
c= Date:
mol/L
c= Date:
mol/L
c= Date:
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mol/L
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11-8
08/2004
Accessories
Order No. Additional parts for the burette Dispensing tube with siphon tip 1.00 m 25961
Drying tube with cover
23961
Drying tube holder
23915
Molecular sieves 250 g
71478
Siphon tip set
set of 5
23240
Adapter for bottles of:
Merck, DE Fisher, US
23774 23787 51107065
Bottle rack for two 1-liter bottles with burettes
Titration stands Titration stand, complete 51108760
Dual titration stand, complete
DV92
08/2004
11-9
Accessories
Order No. Titration stands comprising: Angle bracket (1) 51108760 DV92
25655
Propeller stirrer incl. 2 stirring rods Titration arm (1) x
51109150
25651
Spacing ring (1)
23842
Clamping ring (1)
25653
Threaded ring (1)
25652
Knurled screw (2)
25650
Electrode holder (2) min. order quantity: 5 Stopper ST 14.5 (3) min. order quantity: 5 Stopper ST 7.5 (2) min. order quantity: 5 Titration vessel 100 mL polypropylene (2) set of 1400 x
25654
23451
23452
101974
11-10
08/2004
Accessories
Order No. Additional parts for the titration stand Titration vessel 100 mL polypropylene, red colored set of 1400 25777
Titration vessel 80 mL, glass
set of 20
101446
Titration vessel 250 mL, glass
set of 10
23515
Titration vessel 5-20 mL, glass
23516
Titration vessel for two-phase titration incl. stop cock, threaded ring and gasket Thermostatable titration vessel 80 mL, glass
51107655
23517
Plastic cover for titration vessels
set of 16
101448
Heat exchanger for thermostating incl. adapter with taper joint Gas inlet
23834
23721
Rinsing unit, complete with titration head insert and stoppers for unused openings in titration head 1 set of stoppers for rinsing unit Electrode holder
23821 101230 51108730
08/2004
11-11
Accessories
Order No. Propeller stirrer incl. 2 stirring rods Propeller stirring rod 51109150
101229
Micropropeller stirring rod (for titration vessel 23516) Adapter cable (mini DIN male / RCA female) Peristaltic pump SP250 with Novoprene tubes, adapters, hose clamps Novoprene tubes (1x 1 m + 10x 120 mm) Fluorosilicone elastomer tubes (5x 120 mm) for SP250 Diaphragm pump incl. suction tube Heating system DH100 110 V 230 V Dispensing unit DU200 EU version US version 0.50 m
655073
51107216
51108016
51190969 51108149 51108012
51108779 51108780 51370200 51370210
11-12
08/2004
Accessories
Order No. Sensors Combined pH electrode for titrations in aqueous solutions DG111-SC
Combined pH electrode for small volumes in small titration vessels in aqueous solutions
DG101-SC
Combined glass electrode with movable sleeve frit for titrations in nonaqueous solutions
DG113-SC
Combined glass electrode with movable sleeve frit for titrations in aqueous solutions
DG114-SC
Combined glass electrode with sleeve frit for titrations in aqueous solutions
DG115-SC
Combined platinum ring electrode for redox titrations
DM140-SC
Combined silver ring electrode for argentometric titrations
DM141-SC
08/2004
11-13
Accessories
Order No. Ion selective measuring electrodes Fluoride ISE Chloride ISE Nitrate ISE Sodium ISE Potassium ISE Lithium ISE Ammonia GSE Ammonium ISE Magnesium ISE Cyanide ISE Sulfide ISE Calcium ISE Bromide ISE Fluoroborate ISE Silver ISE Cadmium ISE Iodide ISE Barium ISE Surfactant sensitive electrode Reference electrode for ion selective electrodes surfactant sensitive electrodes
DX219 DX235 DX262 DX223 DX239 DX207 DX217 DX218 DX224 DX226 DX232 DX240 DX280 DX287 DX308 DX312 DX327 DX337 DS500
51089931 51089933 51089934 51089930 51089932 51107673 51107677 51107679 51107684 51107681 51107675 51107683 51107671 51107676 51107682 51107672 51107680 51107674 51107670
DX200 Inlab 301
51089935 52000128
Triaxial cable (Electrode cable with LEMO connector) Cable SC-LEMO-60 0.60 m Cable SC-LEMO-100 1.00 m Cable SC-LEMO-160 1.60 m Phototrode (incl. power supply unit) for color-indicated titrations Transmission measurement at 555, 660, 520, 620, 590 nm Adapter cable1) (DIN-LEMO) for attachment of electrodes or phototrode with DIN connector to the titrator
89601 89602 51108034 DP5
89600
1) If sensors with DIN connectors are attached via the adapter cable to the titrator,
the advantages offered by the triaxial cable high level of protection against electrostatic interference are in part lost. In the case of sensors with a very high resistance, e.g. DG113 in nonaqueous solutions, we advise against use of the adapter cable.
11-14
08/2004
Accessories
Order No. Temperature sensors Pt1000 sensor DT1000
Lemo cable connector (4 pin) for temperature sensors (non-METTLER)
88321
Accessories for Karl-Fischer titrations KF option 51107269
Double-pin platinum electrode
DM143-SC
Electrode cable (SC/Banana)
1.00 m
51108061
External titration stand
DV705
Thermostatable beaker (for KF titration vessel) Stand rod
51107497
51107495
08/2004
11-15
Accessories
Order No. Peripherals

METTLER TOLEDO balances with data output
AG, AM, PM, AT AX, AB, PB, PR, XP on request
Printer DIN A4 / US Letter
Printer
17.37 19.31 5 g 8.003 9 g 7.773 g 6.554 10.50 g g 8.097 6 g 5.876 g 3.205 g 1.098 g g
RS-P42
METTLER TOLEDO
GA4
2 Prin
ter
TBox (control of external devices via TTLIO)

OUT 1 OUT 2
24 VDC 1.2 A
DR42
OUT 3
100-240 V 50/60 Hz unfused max. 9 A
OUT 4
OU T OU 1 T OU 2 T OU 3 T IN 4 1 IN 2 ON
TBox DR42
Sample changer
Rondolino
Sample changer
Rondo 60
Connection cable for Rondolino or TBox
51107424
Connection cable for Rondo 60
51108304
Titration software - LabX pro titration (for Windows 2000/XP) - Instrument licenses for Titrators
11-16
08/2004
Accessories
Order No. Miscellaneous Keypad cover set of 3 51107667
Adapter cable (banana sockets-DIN connector) Memory card (Flash type, 2 MB)
0.23 m
25914
USER DATA
ME-51107230
Memory Card for DL53 and DL55
51107230
Dongle for software updates, upgrading the titrator and special methods
DL53 DL55 DL53 DL55+ DL53 DL53+ DL55 DL55+ DL53 DL58 DL55 DL58
51107210 51107211 51107212 51107213 51107275 51107276
Connection cable: Centronics option Connection cable for AM, PM, AT balances (D sub 9-pin female, 15-pin male) Connection cable for AX balances 229029
11101051
Connection cable for balances with Option 011 (D sub 9-pin female, 25-pin male) Connection cable for AG, AB, PB, PR balances (LC-RS9 cable) Connection cable for SARTORIUS balances (D sub 9-pin female, 25-pin male)
59759
229065
51190363
08/2004
11-17
Accessories
Order No. Connection cable: RS option Connection cable for AM, PM, AT balances 51107196
Connection cable for balances with Option 03 and 011 (RS8 male, D sub 25-pin male) Connection cable for AG, AB, PB, PR balances (LC-RS8 cable) Connection cable for SARTORIUS balances (RS8 male, D sub 25-pin male) Connection cable (RS232C) for printer (RS8 male, D sub 25-pin female) Connection cable (RS232C) for GA42 printer (DTE, 9-pin female)
51107195
229185 200495
200495
201508
Connection cable (RS232C) for computer (DTE, 9-pin female) Connection cable (RS232C) for computer/terminal (DTE, 25-pin female)
201508
201507
11-18
08/2004
Accessories
Order No. Options RS option: 2 RS232C interfaces (DCE) plus 1 TTLIO socket Centronics option: 1 Centronics and 1 RS232C interface plus 1 TTLIO socket KF option: 2 inputs for polarized electrode, 1 stirrer output and 1 analog output pH option: One input each for reference electrode, sensor, temperature sensor plus stirrer and analog output 51107172
51107289
51107269
51107152
Documentation Reference Handbook German English French German English French Spanish Italian German English French Spanish Italian German English German English 51709613 51709614 51709615 51709616 51709617 51709618 51709619 51709620 51709621 51709622 51709623 51709624 51709625 51724764 51724765 51709495 51709496
Quick Guide
Memo card
Application Brochure (No. 12) Computer Interface Description
08/2004
11-19
Accessories
11.3
METTLER TOLEDO literature and application brochures

51725008 51725007 704153 704152 704154 51300047 51300058 51300075 51300201 51724716 51724715 51724717
Basics of Titration Basiswissen in der Titration Fundamentals of Titration Grundlagen der Titration Bases du Titrage Guide to pH Measurement Anleitung zur pH-Bestimmung Guide to Ion Selective Measurement Anleitung zur ionenselektiven Messung Guide to Conductivity and Dissolved Oxygen Anleitung zur Leitfhigkeits- und Sauerstoffmessung Guide de msure da la conductivit et de l'oxygne dissous
DL5x Application Brochure 12 (30 Selected Applications for DL5x Titrators) DL5x Applikationsbroschre 12 (30 ausgewhlte Applikationen fr DL5x Titratoren) DL5x Application Brochure 22 (Surfactant Titration) DL5x Applikationsbroschre 22 (Titration von Tensiden) DL5x / DL7x Application Brochure 29 (Rondo 60 Sample Changer)
51724765 51724764 51725015 51725014 51710082
Memory Card Application package for METTLER TOLEDO Titrators DL53/DL55/DL58 Memory Card and Application Brochure 18 (51724917): Standardization of Titrants Memory Card Applikationssammlung fr METTLER TOLEDO Titratoren DL53/DL55/DL58: Speicherkarte und Applikationsbroschre 18 (51724916): Titerbestimmungen Memory Card Application package for METTLER TOLEDO Titrators DL53/DL55/DL58 Memory Card and Application Brochure 19 (51725012): Determinations in Beverages Memory Card Applikationssammlung fr METTLER TOLEDO Titratoren DL53/DL55/DL58: Speicherkarte und Applikationsbroschre 19 (51725013): Getrnkebestimmungen Memory Card Application package for METTLER TOLEDO Titrators DL53/DL55/DL58 Memory Card and Application Brochure 17 (51724915): Pulp and Paper Industry Memory Card Application package for METTLER TOLEDO Titrators DL53/DL55/DL58 Memory Card and Application Brochure 20 (51725020): Petroleum Industry
51107233 51107234
51107235 51107236
51107237
51107238
11-20
08/2004
Accessories
We have developed applications for the METTLER TOLEDO DL770, DL67, DL70ES and DL77 Titrators, which have a method concept similar to that of the DL50, DL53, DL55 and DL 58 series. You will find these useful when defining the parameters of your method functions. DL70 Application Brochure 1 (18 Customer Methods) DL70 Applikationsbroschre 1 (18 Kundenapplikationen) DL70 Application Brochure 2 (Various Methods) DL70 Applikationsbroschre 2 (Verschiedene Beispiele) DL70 Application Brochure 3 (TAN and TBN) DL70 Applikationsbroschre 3 (TAN und TBN) DL70 Application Brochure 4 (Electroplating) DL70 Applikationsbroschre 4 (Galvanik) DL7x Application Brochure 5 (Determinations in Water) DL7x Applikationsbroschre 5 (Bestimmungen in Wasser) DL7x Application Brochure 6 (Direct Measurement with Ion Selective Electrodes) DL7x Applikationsbroschre 6 (Direktmessung mit ionenselektiven Elektroden) DL7x Application Brochure 7 (Incremental Techniques with Ion Selective Electrodes) DL7x Applikationsbroschre 7 (Additionsverfahren mit ionenselektiven Elektroden) DL7x Application Brochure 8 (Standardization of Titrants I) DL7x Applikationsbroschre 8 (Titerbestimmungen I) DL7x Application Brochure 9 (Standardization of Titrants II) DL7x Applikationsbroschre 9 (Titerbestimmungen II) DL7x Application Brochure 13 (Nitrogen Determination by Kjeldahl Digestion) DL7x Applikationsbroschre 13 (Stickstoffbestimmung nach Kjeldahl Aufschluss) DL7x Application Brochure 14 (Good Labatory Practice in the Titration Lab) DL7x Applikationsbroschre 14 (Gute Laborpraxis im Titrationslabor) DL7x Application Brochure 15 (Guidelines for Result Check, Method Validation and Instrument Certification) DL7x Applikationsbroschre 15 (Leitfaden zur Resultatkontrolle, Methodenvalidierung und Gertezertifizierung) DL7x Application Brochure 16 (Validation of Titration Methods) DL7x Applikationsbroschre 16 (Validierung von Titrationsmethoden) 724492 724491 724557 724556 724559 724558 724561 724560 51724634 51724633 51724646 51724645 51724648 51724647 51724650 51724649 51724652 51724651 51724769 51724768 51724908 51724907 51724910 51724909
51724912 51724911
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Technical Data
Contents
Page
12. 12.1 12.2 12.3 12.4 12.5 12.6 12.7 12.8 12.9 12.10 12.10.1 12.10.2 12.10.3 12.10.4 12.10.5 12.11
Technical data ........................................................................................... 12-3 Measurement system ................................................................................ 12-3 Outputs ...................................................................................................... 12-4 Burette drive module ................................................................................ 12-5 Interchangeable burettes ......................................................................... 12-5 Propeller stirrer ......................................................................................... 12-5 Display ....................................................................................................... 12-5 Memories ................................................................................................... 12-5 Interface for memory card ........................................................................ 12-6 Attachment possibilities for peripheral units ......................................... 12-6 Sockets and connectors ........................................................................... DIN socket ................................................................................................... TTLIO socket ............................................................................................... RS232C connector (Centronics option) ...................................................... Centronics socket (Centronics option) ........................................................ RS232C socket ........................................................................................... 12-7 12-7 12-7 12-7 12-8 12-9
Additional data .......................................................................................... 12-9
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12-1
Technical Data
12.
12.1
Technical data
Measurement system
End point indication potentiometric photometric change of the refractive index and/or the turbidity voltametric/amperometric conductometric Third-party instrument with analog output Temperature compensation for pH/pM/pX measurement Sensor input: pH option (differential amplifier) Input resistance Offset current Measurement range - pH value - voltage Resolution Maximum permissible error Zero point drift Additional reference input Temperature sensor input Measurement range Resolution Maximum permissible error Measurement principle Zero point drift Temperature input via keypad or automatically with the aid of a temperature sensor
Triaxial socket (LEMO) >1012 (protected up to 1000 V capacitatively) <1 pA (20 C) 27.6 pH 2050.0 mV 0.1 mV, 0.002 pH (pM, pX) 0.1% <30 V/ C Banana socket, diameter: 4 mm 4-pin socket (LEMO) -30 C to 130 C 0.1 C 0.2 C 4-line measurement technique: Pt100 or Pt1000 <0.01 C/ C
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Technical Data
Sensor input: KF option Sensor input Voltage source Range Resolution Measurement range Resolution Maximum permissible error Current source Range Resolution Measurement range Resolution Maximum permissible error
2 Banana sockets, diameter: 4 mm
-1270 to +1270 mV 10 mV in the range -1270 to +1270 mV 1 mV in the range -127 to +127 mV -150 to +150 A 0.01A (16-bit AD converter) 0.1%
-127 to +127 A 1 A in the range -127 to +127 A 0.1 A in the range -12.7 to +12.7 A -1500 to +1500 mV 0.1mV (16-bit AD converter)) 0.1%
12.2
Outputs
5-pin socket (mini DIN) 0 18 V in no-load operation Typically: <5% the output is protected electronically against overload, Imax: 300 mA 2 banana sockets, diameter: 2 mm 1 35 mV 2000 mV 1% 220
Stirrer output Voltage range Speed stabilized
Analog output Gain Offset: max. permissible error Range Range: max. permissible error Output resistance
12-4
08/2004
Technical Data
12.3
Burette drive module
With direct current motor Equipment Resolution Maximum permissible error Filling time Discharge time
DL50/DL53: max. 1, DL55/DL58: max. 2 1/5000 of the burette volume 0.3% relative to the respective burette volume of 5, 10 and 20 mL 20 s Minimum 20 s
12.4
Interchangeable burettes
1, 5, 10 and 20 mL Fluoroplastic, borosilicate glass, ceramics
Volume Materials which come into contact with the titrant
12.5
Propeller stirrer
3800 rpm Pmax.: Ptypical:
Maximum speed Power consumption
6W 1.2 W at 12 V
12.6
Display
6 lines, 39 characters per line 240 x 64 pixels, backlighting through cold cathode fluorescent lamp English, German, French, Spanish and Italian
LCD with graphics capability
Languages
12.7
Memories
METTLER methods, standard methods User methods, resource and sample data, space for approx. 50 standard methods
Database User data memory (EEPROM)
08/2004
12-5
Technical Data
12.8
Interface for memory card
Slot for 68-pin memory card of type 1 Standards supported: PCMCIA, version 2.0 JEIDA, version 4.1 Memory cards which can be used: 1. Flash memory card series 2 Intel with the designation: Mitsubishi with the designation: 2. SRAM Melcard Mitsubishi with the designation:
iMC002FLSA - 20 (2 MB storage capacity) iMC004FLSA - 20 (4 MB storage capacity) MF82M1-G7DAT 01 (2 MB storage capacity) MF84M1-G7DAT 01 (4 MB storage capacity) MF31M1-LCDAT 01 (1 MB storage capacity)
12.9
Balance
Attachment possibilities for peripheral units

Attachment via RS232C interface of the Centronics or an RS option at slot No. 4 for all METTLER TOLEDO and SARTORIUS balances Attachment via Centronics interface of the Centronics option or via RS232C interface of an RS option at slot No. 4 for various commercial graphics printers (on use of the RS option with XON/XOFF protocol) Attachment via RS232C interface of the RS option at slot No. 3 (available as an option) Attachment via RS232C interface of the RS option at slot No. 3 (available as an option)
Printer
Sample Changer
Terminal or computer (LIMS: in-house laboratory information management system) Auxiliary units (third-party units)
Attachment via TTLIO socket of the RS option at slot No. 3 (available as an option) Attachment via the DIN socket, 5-pin
External keyboard (third-party unit, e.g. commercial PC keyboard)
12-6
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Technical Data
12.10
12.10.1
Sockets and connectors

DIN socket
5-pin, DIN 180, following DIN 41524

Pin assignment CLOCK
2 5 3 4 1
1 2
DATA GND
+
4 5
VCC
VCC: 5 V
Titrator
12.10.2
TTLIO socket
8-pin connector, series 712 waterproof (TTL: Transistor-Transistor-Logic) The socket has 2 TTL inputs and 4 TTL outputs.
Pin assignment GND In 1
1 8 5 7 6 2 3 4
1 2 3 4 5
+5 V
VCC: +5 V, max. 60 mA In: TTL; short circuit proof Pulse 150 ms (the input signal must be at least 150 ms for the titrator)
In 2 Out 1 Out 2 Out 3 VCC Out 4
6 7 8
Titrator
Out: Open collector Vce max. = 24 V Ic max. = 20 mA
12.10.3
RS232C connector (Centronics option)
9-pin, D-Sub
Pin assignment BR
5 9 4 8 3 2 1 7 6
Shielding RxD (In) TxD (Out) DSR RSGND

Titrator
1 2 3
Data to titrator Data from titrator Handshake from titrator, fixed to operational readiness Electrically isolated signal ground
+12 V
330
4 5
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12-7
Technical Data
12.10.4
Centronics socket (Centronics option)
19-pin connector, series 723 waterproof

Pin assignment
/STROBE D0 D1 D2 D3 D4
A: Data ready B: C: D: E: F: G: Data
I K L T U M N B C O D S R P E H G F
D5
H:
D6
I:
D7
K: Data adopted
/ACK
L: Printer occupied
BUSY
M: End of paper
PE SLCT /AUTO FDXT /ERROR /INIT /SLCTIN GND GND
Titrator
N: Printer active O: Automatic line feed P: Printer error R: Initializing printer S: Printer selected T: U: Signal ground
12-8
08/2004
Technical Data
12.10.5
RS232C socket
8-pin connector DIN 45326, series 723 waterproof

Pin assignment Shielding BR 1 2 3 6 +12 V
Titrator
1 6 8 7 3 5 4 2
TxD (Out) RxD (In) RSGND DSR 330
Data to titrator Data from titrator Electrically isolated signal ground Handshake from titrator fixed to operational readiness
12.11
Housing
Additional data
Polyester Polypropylene Polyester, splashwater-proof Width: 260 mm, depth: 395 mm, height: 270 mm Approx. 8 kg with one burette drive 100 240 VAC 10% (automatic range adjustment) 2 x T1,6L250V (not exchangeable) 50/60 Hz 400 mA Ambient temperature: +5 C to +40 C Maximum relative atmospheric humidity of 80% for temperatures of up to 31 C, decreasing linearly to 50% relative atmospheric humidity at 40 C. Use indoors Height up to 2000 m Overvoltage category II Pollution degree 2
Titration stand Keypad Dimensions Weight Power supply Fuse Frequency Maximum power consumption Ambient conditions
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12-9
Index
Index
Numbers incorporating dashes refer to sections in the Reference Handbook (example: 3-38), Numbers without dashes refer to the Quick Guide (example: 9).
<F1>...<F5> 9, 10 E EP titration function 3-39 EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 measure function 3-17 E(set) EP titration function 3-39 EQP titration function 3-22 t EP titration function 3-39 EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 measure function 3-17 Accessories optional accessories 11-7 standard equipment 11-4 Activate control input 6-32 control output 6-33 Adjust measuring inputs 6-28 Amperometric indication EP titration function (Ipol/Upol) 3-58 EQP titration function (Ipol/Upol) 3-47 Analysis aborting (Reset) 5-12 fading out 5-11 is interrupted 5-11 menu sequence 5-4 "Run" menu 5-3 start 5-4 Analysis sequences (examples) CaCl2 determination 5-7 calibration of a pH electrode 27 comparison: titration stand 1/ST20A 5-16 determination of the HCl content 12 pH-stating 5-10 titer determination (NaOH) 32 with the sample changer 5-17 Arrow keys 7 Asterisk (*) 3-4, 3-11 Asymmetric (evaluation procedure) equivalence point recognition 3-28, 3-50 evaluation parameter 3-34, 3-53 explanation 8-16 Audio signal 6-28 Auto stand definition 2-17 sample series 5-6, 5-15 Auxiliary functions explanation 9, 6-3 keys 6-3 overview 1-4, 1-5 Auxiliary value(s) entering 2-15 entry through determination 2-15 function 3-73 memories 3-73 resource 2-15 storage procedure 2-16 Balance(s) configuration (METTLER TOLEDO) 2-22 configuration (SARTORIUS) 2-22 connection 10-10 defining 2-21 Bar-code reader connection 10-16 defining 2-24 Bar-code string 6-43 Baud rate balances 2-22 computer 2-23 printer 2-20 terminal 2-25 Bidirectional transmission mode 2-21, 4-12 Buffer solutions DIN/NIST buffer 3-70 MERCK buffer 3-69 METTLER TOLEDO buffer 3-69 Burette air bubbles 10-8 equipping 10-5 filling 13 inserting 10-6 installing 10-4 maintaining 10-4, 10-7 order No. 11-4 rinsing 6-11 rinsing tip 6-12
08/2004
13-1
Index
Burette drive inserting 10-3 selecting 2-5 Burette volume selecting 2-5 smallest increment 3-24 Burette tip 6-12 C (constant) 3-66, 8-7 c ( nominal concentration) 8-3 c * t (actual concentration) 8-3 Calculation(s) formulas 8-17 function 3-66 indices 8-9 performing (auxiliary function) 6-20 Calibration function 3-69 pH electrodes 27 sensors 3-69 temperature sensors 6-6 Calibration data measuring inputs 6-29 sensors 2-9, 2-10, 3-69 temperature sensors 2-12 Centronics interface GA42 printer 2-18 printer configuration 2-19 Centronics option connection possibilities 10-9 installing 10-10 Changer 6-9 Character set (computer) 2-24 Clock (titrator) 6 Code (sync function) 7-18 Combined termination conditions 3-34, 3-53 Command keys 9 Communication protocol (computer) 2-24 Computer bar-code reader 2-24 bar-code string 6-43 configuration 2-23 connection 10-10 data transfer 6-40 remote control 6-42 Concentration (titrant) 2-4, 8-3 Conditioning 3-15 Conductivity measurement 2-8 Conductometer 2-8 Constants calculation function 3-66 calculations (auxiliary function) 6-20 examples 8-18
Continuous (titrant addition) 3-40, 3-60 Control band EP titration function 3-40 EP titration function (Ipol/Upol) 3-60 pH/mV-stat function 3-63 Control input activating (auxiliary function) 6-32 function 7-15 Control inputs defining 7-4 resource 7-4 Control mode (activate control output) input controlled 6-33 on/off 6-33 sequential 6-34 Control mode (control output function) fixed time 7-16 input controlled 7-16 on/off 7-16 sequential 7-17 Control output activating (auxiliary function) 6-33 function 7-16 Control outputs defining 7-5 resource 7-5 Control range EP titration function 3-40 EP titration function (Ipol/Upol) 3-60 pH/mV-stat function 3-63 Correction factor f 4-6, 5-6 Correlation coefficient 3-62, 3-65, 8-6 CSTAT (correlation coefficient) 3-62, 8-6 Current measurement (Ipol/Upol) 6-7 Current sample (mask) notes 5-6 Cursor 10 Cx (calculation constant) 8-7 Database 12-5 Data bits computer 2-24 printer 2-20 terminal 2-25 Data sheet KF option 10-12 pH option 10-12 Data Transfer 6-36
13-2
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Index
Date entering 6-27 selecting format 6-26 Date specification auxiliary values 2-15 methods 3-11 sensors 2-9 temperature sensors 2-11 titrants 2-5 Defined are (mask) exclusion 6-30 meaning 5-5 Delay 3-42, 3-61 Directory (memory card) 6-37 Dispense auxiliary function (burette) 6-12 auxiliary function (ST20A) 6-10 continuously 6-13 continuously (Ipol/Upol) 6-15 function 3-19 DL58 commands 7-3 functions 7-3 resources 7-3 DLWin software 4-13, 6-41 Documentation information 4 Drift (potential measurement) 3-17 Dynamic (titrant addition) EP titration function 3-39 EQP titration function 3-22 E (potential) 3-17, 8-7 EHNV (half neutralization value) 3-20, 8-4 Electrodes (METTLER TOLEDO) 2-7, 2-13 End point EP titration function 3-41 EP titration function (Ipol/Upol) 3-60 pH/mV-stat function 3-63 range 3-40, 3-60 titration 3-37, 3-56 Entry keys 10 EP absolute 3-41 relative 3-41 EP titration (function) 3-37 EP titration (Ipol/Upol) (function) 3-56 EPOT 8-4 EQP titration (function) 3-20 EQP titration (Ipol/Upol) (function) 3-45 Equilibrium controlled measured value acquisition EP titration function 3-39
EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 measure function 3-17 Equivalence point(s) explanation 3-20, 3-45, 8-14 formulas for restriction 8-19 maximum number/sample determination 8-20 range 3-32, 3-51 recognition 3-28, 3-50 Equivalence point titration 3-20, 3-45 Equivalent number calculation function 3-68 entering 3-13 Error messages "EPROM test failed" 9-3 learn titration 5-11 "RAM test failed" 9-3 referring to Section 9.1 9-3 Esc command (<F1>) 9 ET1 3-22, 3-38, 8-4 ET2 3-22, 3-38, 8-4 Evaluation EQP titration function 3-34 EQP titration function (Ipol/Upol) 3-53 pH/mV-stat function 3-65 Evaluation procedure EQP titration function 3-28, 3-34 EQP titration function (Ipol/Upol) 3-50, 3-53 explanation 8-14 Expert (user level) 6-31 Expiry date (titrant) 2-5, 5-4 External keyboard connection 10-15 defining 2-26 key assignment 10-15 External stand 2-17 Extinction 2-8 f (correction factor) 4-6, 8-3 Fixed time (control output function ) 7-16 Fixed volume note 5-5 selecting 3-12 Form feed (printer) 2-19 Formula(s) auxiliary value function 3-73 calculation function 3-66 calculations (auxiliary function) 6-20 constants 8-18 for restriction of the equivalence point 8-19 results 8-17 titer function 3-72 Frame lines (report) 2-19 Function(s)
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13-3
Index
adding 7-8 deleting 7-8 DL58 7-3 explanation 20, 3-3 maximum number 7-9 modifying 3-10 overview 24 selecting 3-7 H (auxiliary value) 2-15, 8-3 Half neutralization value 3-20 In 3.1/3.2 (TTL inputs) 6-32 Incremental (titrant addition) EQP titration function 3-24 EQP (Ipol/Upol) titration function 3-48 two-phase titration function 7-14 Indexing forms compilation 8-12 examples 8-9, 8-10 Indication EP titration function (Ipol/Upol) 3-57 EQP titration function (Ipol/Upol) 3-46 Indices 8-9 Inflection point 8-14 Initial potential ET1 3-22 Input controlled activate control output (auxiliary function) 6-33 control output function 7-16 Input signal (control input function) 7-15 Installation and maintenance 10-3 Instruction control output function 7-17 function 7-11 Interchangeable burette: see burette 10-4 Interpolation (evaluation) 8-14 Interval (conditioning) 3-15 Karl-Fischer titrations accessories 11-15 Keyboard external 2-26 titrator 7 Key combinations 10 KF option inputs and outputs 10-10 installing 10-11 measuring inputs (calibration data) 6-29 polarized sensors 2-13
LabX titration software 4-13, 6-41 Language (changing) 11, 6-27 Learn titration function 3-43 results 5-9 Lift position (sample changer) 6-9 Line feed (printer) 2-19 Lists (explanation) 8 M (molar mass) 3-68, 8-3 m (sample size) 8-3 Maintenance burette 10-7 titrator 10-3 Malfunctions 9-6 Manual temperature entry 3-13 titration 6-14, 6-16 Masks (explanation) 8 Max. time (control input function) 7-15 Maximum (evaluation procedure) equivalence point recognition 3-28, 3-50 evaluation parameter 3-34, 3-53 explanation 8-14 Maximum time (EP titration function (Ipol/Upol)) 3-61 Maximum volume EP titration function 3-42 EP titration function (Ipol/Upol) 3-61 EQP titration function 3-33 EQP titration function (Ipol/Upol) 3-52 pH/mV-stat function 3-64 Mean value x auxiliary value function 3-73 calculation function 3-67 titer function 3-72 Measure (function) 3-17 Measure mode EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 two-phase titration function 7-14 Measured points for equivalence point recog-nition 3-28, 3-44, 3-50 Measured values displaying 5-7, 6-21 maximum number/titration function 8-20 storage specification 3-64, 3-74, 8-20 Measuring inputs adjusting 6-28 calibration data 6-29
13-4
08/2004
Index
Memory card directory 6-37 formatting 6-36, 6-40 inserting 10-11 interface 12-6 types 12-6 use 6-36 Memory copy(ies) copying on memory card 6-39 loading to titrator 6-40 transferring to computer 6-41 Menus explanation 8 keys 8 overview 1-2, 1-3 Method concept 19 deleting 3-5 explanation 3-3 generating 24 modifying 3-7 modifying (current sample series) 5-12 modifying (ongoing method: DL55/DL58) 5-13 on computer 4-5 on memory card 4-5 printing 3-4 storage procedure 3-7 Methods menu 3-3 printing 3-4 selecting 3-4 Method ID defining 3-11 entering 4-4, 5-5 explanation 3-4 METTLER methods 3-6 modifying 3-9 standard methods 3-5 METTLER methods 90001: performance 14 90002: performance 27 explanation 19 modifying 25, 3-6 printing 3-6 Minimum (evaluation procedure) equivalence point recognition 3-28, 3-50 evaluation parameter 3-34, 3-53 explanation 8-14 Misc. ... 6-26 Mixing time (two-phase titration function ) 7-14 Modify: command (<F4>) 10 Molar mass M calculation function 3-68 entering 3-13
neq (number of equivalence points) 8-4 OK command (<F5>) 9 On/Off activate control output (auxiliary function) 6-33 control output function 7-16 Operating concept 7 Options 10-9 Out 3.1...3.4 (TTL outputs) 6-33 Output (reports) 3-74, 6-24 P1/P2 8-6 Paper (printer) fanfold 2-19 format 2-19 single sheet 2-19 Parameters (explanation) 20 Parity balances 2-22 computer 2-23 terminal 2-25 printer 2-20 t Peripherals (setup menu) 2-18 pH electrode calibrating 26 slope 26 zero point 26 pH measurement 35 pH option inputs and outputs 10-10 installing 10-11 measuring inputs (calibration data) 6-29 sensors 2-7 pH/mV-stat (function) 3-62 pH-stating (example) 3-65 Piston assembling 10-4 inserting 10-4 Polarized sensors adding 2-14 KF option 2-13 modifying 2-13 resource 2-13 storage procedure 2-13 Potential 1/2 (evaluation parameters) 3-35, 3-54 Potential measurement 6-4, 6-7 Predispensing EP titration function 3-38 EP titration function (Ipol/Upol) 3-59 EQP titration function 3-21 EQP titration function (Ipol/Upol) 3-48 two-phase titration function 7-13
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13-5
Index
Pretitration (pH/mV-stat function) 3-63 Primary standard 30, 31 Printer ASCII 2-18 configuration 2-19, 2-20 connection 10-10 defining 2-18 Pt100/Pt1000 sensor 2-11 Pump function 7-11 titration stand parameters 3-13 rate (solvents) 2-27 Q 8-4 QDISP 3-19, 8-7 QEND 8-4 QEX 8-4 QP1/QP2 8-4 QSTAT 8-6 QT1/QT2 8-6 QTOT 8-6 R (result) 3-66, 8-7 Range (equivalence point) 3-32, 3-51 Raw results compilation 8-8 explanation 3-18 recording 3-75, 6-24 storage specification 8-20 Rear view of titrator 10-10 Recalculations 6-20 Recognition (equivalence point) 3-28, 3-50 Reevaluation condition met 5-11 defining condition 3-35, 3-36, 3-55 performing 6-18 Reference electrode 2-7 Relative standard deviation srel 3-67 Remote control 6-42 Report auxiliary function 6-24 function 3-74 header 6-27 Reset key 7, 5-12
Resources changing 5-8 copying on memory card 6-39 copying to titrator 6-39 deleting 2-3 DL58 7-3 explanation 2-3 list 2-3 modifying 2-3 printing 2-3 transferring to computer 6-41 Result(s) auxiliary function 6-18 deleting 6-22 examples 3-67, 8-17 learn titration 5-9 maximum number/sample series 8-20 R 3-66, 3-71 recording 3-75, 6-24 Rx 6-20 storage specification 8-20 units 3-67, 8-17 Result list displaying 6-18 exclusion 6-30 notes 5-9 Rinse auxiliary function (ST20A) 6-10 tip (burette) 6-12 titration stand parameters 3-14 Routine (user level) 6-31 RS option connection possibilities 10-11 installing 10-11 RS232 interface GA42 printer 2-20 printer configuration 2-20 Run analysis menu 5-3 key function 5-3 s (standard deviation) 8-7 Safety measures for operational safety 5 for your protection 5, 10-3 Safety notes 1-1 Sample function 3-12 ID (identification) 4-5, 5-6
13-6
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Index
Samples maximum number 8-20 status 4-7 Sample changer auxiliary function 6-9 connection 10-10 defining 2-25 sample series 5-6, 5-15 titration stand 2-17 titration stand parameters 3-13 Sample data adding 4-8 deleting 4-6 entering 4-4, 5-5, 5-10 list 4-4, 4-6 memory (sample menu) 4-3 modifying 4-7 on computer 4-13 printing 4-7 recording 3-75, 6-24 storage specification 36, 4-3 Sample data mask analysys menu 5-5 sample menu 4-5 Sample series deleting 4-6 entering 4-4 with auto stand 5-6, 5-15 with ST20A 5-6, 5-15 Sample series (DL55/DL58) entering 4-9 executing 5-15 Sample size 3-21, 3-38, 3-48, 3-59, 8-3 Save (storage procedure) auxiliary values 2-16 devices for control intput 7-5 devices for control output 7-6 methods 3-7 polarized sensors 2-13 sensors 2-10 solvents 2-28 temperature sensors 2-12 titrants 2-6 Segmented (evaluation procedure) equivalence point recognition 3-28, 3-50 evaluation parameter 3-34, 3-53 explanation 8-15 Send mode (computer) 2-24
Sensor(s) adding 2-10 auxiliary function 6-4 deleting 2-7 modifying 2-7 order No. 11-10 pH option 2-7 resource 2-7 storage procedure 2-10 Sensor inputs polarized sensors 2-13 sensors 2-8 temperature sensors 2-11 Separation time (two-phase titration function) 7-14 Sequential activating control output (auxiliary function) 6-34 control output function 7-17 Setup (menu) 2-3 Shorten analysis sequence 6-30 SLOPE 8-3 Slope calculation 3-69 entry through determination 2-9 explanation 2-9 minimum/maximum value 3-71 pH electrode 26 theoretical value 2-9 Slots 10-10 Software LabX 4-13, 6-41 Software version 1-1 Solvents adding 2-28 deleting 2-27 modifying 2-27 storage procedure 2-28 Special methods DL58 7-7 explanation 7-3 Speed defining 3-16 modifying 5-8, 6-8 srel (relative standard deviation) 8-7 ST20A connection 10-10 outputs 2-28 Stand 1/2 (titration stands) 2-17 Standard (evaluation procedure) equivalence point recognition 3-28, 3-50 evaluation parameter 3-34, 3-53 explanation 8-14 Standard deviation s 3-67
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Index
Standard method(s) application examples 22 explanation 19, 3-5 functions 20 modifying 25, 30 number 20 printing 3-5 Start/end character (computer) 2-24 Statistics modifying 6-22 selecting for calculations 3-67 Status remote control 6-42 peripherals 2-18 samples 4-7 Steepest jump only 3-31 Stir (function) 3-16 Stirrer auxiliary function (stirrer) 6-8 output 2-17 speed 5-8, 6-8 Stirring time 3-16 Stop bits computer 2-24 printer 2-20 terminal 2-25 Stop for reevaluation 3-35, 3-55, 5-11 Storage interval (pH/mV-stat function) 3-64 Storage procedure measured values 3-64, 3-74, 8-20 raw results 8-20 results 8-20 sample data 4-3 Symbols explanation 8-3 list 8-3 Sync (function) 7-18 Synchronization mode (Sync function) 7-18 System computer/terminal 2-23 titrator (information) 9-3, 9-6
T (temperature) 7-10 t (titer) 3-72, 8-3 t(max) EP titration function 3-39 EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 measure function 3-18 temperature function 7-10 t(min) EP titration function 3-39 EQP titration function 3-25 EQP titration function (Ipol/Upol) 3-49 measure function 3-17 temperature function 7-10 Table of measured values displaying 5-7, 6-21 recording 3-75, 6-24 Technical data burette 12-5 burette drive 12-5 Centronics socket 12-8 DIN socket 12-7 display 12-5 measurement system 12-3 memories 12-5 outputs 12-4 peripherals 12-6 RS232C connector (Centronics option) 12-7 RS232C socket (RS option) 12-9 stirrer 12-5 TTLIO sockets 12-7 Temperature correction 3-13, 3-69 entering 2-9, 4-6, 5-6 function 7-10 measurement 2-9, 3-13, 3-18, 3-20, 3-37, 3-62, 3-69, 7-10 measuring (auxiliary function) 6-5 Temperature sensor(s) calibrating 6-6 Lemo cable plug 10-10 Pt100/Pt1000 2-11 resource 2-11 selecting 3-13 storage procedure 2-12 Tendency EP titration function 3-42 EP titration function (Ipol/Upol) 3-61 EQP titration function 3-32 EQP titration function (Ipol/Upol) 3-51 pH/mV-stat function 3-64
13-8
08/2004
Index
Terminal configuration (keyboard) 10-16 configuration (titrator) 2-25 connection 10-11 key assignment 10-17 Termination (parameters) EP titration function 3-42 EP titration function (Ipol/Upol) 3-61 EQP titration function 3-33 EQP titration function (Ipol/Upol) 3-52 pH/mV-stat function 3-64 Threshold 3-29, 3-51 Threshold value evaluation procedure "Asymmetric" 3-30 evaluation procedure "Minimum/Maximum" 3-30 evaluation procedure "Segmented" 3-31 evaluation procedure "Standard" 3-30 TIME 5-4, 8-3 Time entering 6-27 sample function (conditioning) 3-15 selecting format 6-26 stir function 3-16, 5-7 Time specification auxiliary values 2-15 methods 3-11 sensors 2-9 temperature sensors 2-11 titrants 2-5 Timed increment measured value acquisition EP titration function 3-41 EP titration function (Ipol/Upol) 3-60 EQP titration function 3-27 EQP titration function (Ipol/Upol) 3-49 Titer checking 2-5 determination (NaOH solution) 32 entering 2-4 entry through determination 2-4 explanation 30 function 3-72 Title function 3-11 METTLER methods 19 standard methods 19 Titrant adding 2-6 concentration 2-4, 8-3 deleting 2-4 modifying 2-4 storage procedure 2-6
Titrant addition EP titration function 3-39 EP titration function (Ipol/Upol) 3-60 EQP titration function 3-22 EQP titration function (Ipol/Upol) 3-48 pH/mV-stat function 3-63 two-phase titration function 7-14 Titrate manually 6-14 manually (Ipol/Upol) 6-16 Titration curves 1st derivative 3-30, 3-31, 3-54, 8-15 2nd derivative 3-31, 3-54, 8-15 displaying 5-8, 5-8, 6-21 recording 3-75, 6-24 Titration stand equipping 10-9 meaning 7-8 order No. 11-7 resource 2-17 selecting 3-13 Titrator battery 6 cleaning housing 10-3 connections 6, 10-10 documentation 4 front view 6 ID (identification) 6-27 internal clock 6 keypad 7 opening housing 10-3 rear view 6, 10-10 remote control 6-42 self test 7 settings 6-26 Transmission mode (balance) bidirectional 2-21 unidirectional 2-21 TTL inputs activating 6-32 wiring electronically 10-14 wiring mechanically 10-13 TTL outputs activating 6-33 wiring electronically 10-14 TTLIO socket(s) inputs and outputs 10-13 technical data 12-7 used by titrator 10-13 Turntable (sample changer) 6-10 Two-phase titration function 7-12 special method 7-12
08/2004
13-9
Index
Unidirectional transmission mode 2-21 Units 3-67, 8-17, 8-18 Units of measurement (sensors) 2-8 Urgent sample (DL55/DL58) 4-10 User data memory 12-5 User level 6-31 User method(s) copying on memory card 6-38 copying to titrator 6-39 deleting 3-6 explanation 19, 3-6 printing 3-6 "titer by EQP titration" 34 transferring to computer 6-41 VDISP 3-19, 8-7 VEND 8-4 VEQ 8-4 VEX 8-4 Voltage measurement (Ipol/Upol) 6-7 Voltametric indication EP titration function (Ipol/Upol) 3-57 EQP titration function (Ipol/Upol) 3-46 Volume entering 4-5, 5-6 selecting 3-12 Volume limits at volume entry 4-5, 5-6 entering 3-12 VP1/VP2 8-4 VSTAT 8-6 VT 3-65, 8-6 VT1/VT2 8-6 VTOT 8-6
Wait time predispensing 3-21, 3-38, 3-48, 3-59, 7-13 stir function 3-16, 5-7 Weight entering 4-5, 5-6 selecting 3-12 transferred by balance 4-12 Weight limits at weight entry 4-5, 5-6 entering 3-12 x (mean value) 8-7 z (equivalent number) 3-13, 3-68, 8-3 ZERO 8-3 Zero point (sensor) calculation 3-69 entry through determination 2-9 explanation 2-9 pH electrode 26 theoretical value 2-9 Zero point (temperature sensor) entry through determination 2-12 explanation 2-11 theoretical value 2-12
13-10
08/2004
Indice
Indice
Los nmeros separados por un guin (ejemplo 3-38) se refieren al captulo correspondiente en el Manual de Instrucciones, las cifras aisladas a la Gua de Manejo (ejemplo 9).
<F1>...<F5> 9, 10 E func. medir 3-17 func. valoracin EP 3-39 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 E (nom.) func. valoracin EP 3-39 func. valoracin EQP 3-22 t func. medir 3-17 func. valoracin EP 3-39 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 Accesorios accesorios facultativos 11-7 equipo bsico 11-4 Acondicionamiento (ST20A) 3-15 Activar entrada mando a distancia 6-32 salida mando a distancia 6-33 Acumulador 6 Adicin de reactivo func. pH/mV-Stato 3-63 func. valoracin EP 3-39 func. valoracin EP (Ipol/Upol) 3-60 func. valoracin EQP 3-22 func. valoracin EQP (Ipol/Upol) 3-48 func. valoracin en dos fases 7-14 Adquisicin datos medidos: incremental tiempo func. valoracin EP 3-41 func. valoracin EP (Ipol/Upol) 3-60 func. valoracin EQP 3-27 func. valoracin EQP (Ipol/Upol) 3-49 Agitador funcin auxiliar (Stirrer) 6-8 seleccionar salida 2-17 Agitar (funcin) 3-16 Ajustar entradas de medida 6-28 Anlisis empezar 5-4 men "Run" 5-3 se interrumpe 5-11 secuencia men 5-4 terminar (Reset) 5-12 visualizar 5-11 Asimtrica (procedimiento de evaluacin) explicacin 8-16 parmetro de evaluacin, 3-34, 3-53 reconocimiento punto de equivalencia 3-28, 3-50 Asterisco (*) 3-4, 3-11 Avance de lnea (impresora) 2-19 de pgina (impresora) 2-19 Aviso de errores con indicaciones en cp. 9.1 9-3 "EPROM test failed" 9-3 "RAM test failed" 9-3 valoracin de aprendizaje 5-1 Avisos de seguridad 1-1 Balanza (s) conectar 10-10 configuracin (METTLER TOLEDO) 2-22 configuracin (SARTORIUS) 2-22 definir 2-21 Banda de control func. pH/mV-Stato 3-63 func. valoracin EP 3-40 func. valoracin EP (Ipol/Upol) 3-60 Base de datos 12-5 Baudios balanza 2-22 impresora 2-20 ordenador 2-23 terminal 2-25 Bits de datos impresora 2-20 ordenador 2-24 terminal 2-25 Bits de parada impresora 2-20 ordenador 2-24 terminal 2-25 Bomba funcin 7-11 parmetros cabeza de valoracin 3-13
08/2004
13-11
Indice
Bureta burbujas de aire 10-8 funcin auxiliar 6-11 insertar 10-6 instalar 10-4 llenar 13 llenar (lavar) 6-11 mantenimiento 10-4, 10-7 montaje 10-5 C (constante) 3-66, 8-7 c (concentracin nominal) 8-3 c * t (concentracin real) 8-3 Cabeza de val. auto definicin 2-17 serie(s) de muestras 5-6, 5-15 Cabeza de val. externa 2-17 Cabeza de valoracin medios auxiliares 2-17 montaje 10-8 nmero de pedido 11-7 seleccionar 3-13 significado 7-8 Clculo posterior 6-20 Clculo(s) frmulas 8-17 funcin 3-66 indicativos 8-9 realizacin (funcin auxiliar) 6-20 Calibracin electrodo de pH 27 funcin 3-69 sensores 3-69 sondas de temperatura 6-6 Cambiador de muestras cabeza de valoracin 2-17 conectar 10-10 definir 2-25 funcin auxiliar (Changer) 6-9 parmetros cabeza de valoracin 3-14 serie de muestras(s) 5-6, 5-15 Cambiar: mando (<F4>) 10 Cambio de buretas: ver buretas Cambio de lengua 11, 6-27 Centronics: ver interface/tarjeta Cdigo (func. sincronizacin) 7-18 Cdigo de barras 6-43 Coeficiente de correlacin 3-62, 3-65, 8-6 Combinacin de teclas 10 Concentracin (reactivo) 2-4, 8-3 Concepto de manejo 7 de mtodos 19 Conductmetro 2-8
Constantes ejemplo 8-18 funcin auxiliar clculo 6-20 funcin clculo 3-66 Continua (adicin de reactivo) 3-40, 3-60 Control de entrada activar salida mando a distancia (funcin auxiliar) 6-33 func. salida mando a distancia 7-16 Control de equilibrio (adquisicin de los valores medidos) func. medir 3-17 func. valoracin EP 3-39 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 Copia de la memoria carga al titulador 6-39 copia a la tarjeta memoria 6-39 transferir al ordenador 6-41 Criterios de terminacin combinados 3-34, 3-53 CSTAT (coeficiente de correlacin) 3-62, 8-6 Curso del anlisis (ejemplo ) calibracin electrodos de pH 27 comparacin: Cabeza de valoracin 1/ST20A 5-16 con cambiador de muestras 5-17 determinacin CaCl2 5-7 determinacin del contenido HCl 12 determinacin del ttulo (NaOH) 32 regulacin del pH 5-10 Cursor 10 Curvas de valoracin 1 derivada 3-30, 3-31, 3-54, 8-15 2 derivada 3-31, 3-54, 8-15 impresin 3-75, 6-24 visualizacin 5-7, 5-8, 6-21 Cx (constantes de clculo) 8-7 Data Transfer (transmisin de datos) 6-36 Datos de calibracin entradas de medida 6-29 sensores 2-9, 2-10, 3-69 sondas de temperatura 2-12 Datos de muestra aadir 4-8 borrar 4-6 cambiar 4-7 condiciones de memorizacin 36, 4-3 desde ordenador 4-13 entrar 4-4, 5-5, 5-10 imprimir 4-7 informe 3-75, 6-24 lista 4-4, 4-6 memoria (men Sample) 4-4, 5-5, 5-10
13-12
08/2004
Indice
Datos tcnicos agitador 12-5 buretas 12-5 conector Centronics 12-8 conector DIN 12-7 conector RS232C (tarjeta RS) 12-9 conector TTLIO 12-7 enchufe RS232C (tarjeta Centronics) 12-7 memorias 12-5 motor de bureta 12-5 pantalla 12-5 perifricos 12-6 salidas 12-4 sistema de medida 12-3 Deriva (medida del potencial) 3-17 Desviacin estndar relativa (srel) 3-67 Desviacin estndar (s) 3-67 Dinmica (adicin de reactivo) func. valoracin EP 3-39 func. valoracin EQP 3-22 Directorio (tarjeta memoria) 6-37 Diversos (Misc. ...) 6-26 DLWin Software 4-13, 6-41 DL58 funciones 7-3 mandos 7-3 medios auxiliares 7-3 Documentacin informacin 4 Dosificacin continua 6-13 continua (Ipol/Upol) 6-15 Dosificacin previa func. valoracin en dos fases 7-13 func. valoracin EP 3-38 func. valoracin EP (Ipol/Upol) 3-59 func. valoracin EQP 3-21 func. valoracin EQP (Ipol/Upol) 3-48 Dosificar funcin 3-19 funcin auxiliar (buretas) 6-12 funcin auxiliar (ST20A) 6-10 E (potencial) 3-17, 8-7 EHNV (valor de semineutralizacin) 3-20, 8-4 Electrodo de referencia 2-7 Electrodos (METTLER TOLEDO) 2-7, 2-13 Electrodos de pH calibrar 26 pendiente 26 punto cero 26
Electrodos polarizados almacenar 2-13 aadir 2-14 cambiar 2-13 tarjeta KF 2-13 medios auxiliares 2-13 Embolo colocacin 10-4 montaje 10-4 Encabezamiento de informe 6-27 Entrada mando a distancia activar (funcin auxiliar) 6-32 funcin 7-15 Entradas de sensores func. salida mando a distancia 7-17 sensores 2-8 sensores polarizados 2-13 Entradas mando a distancia definir 7-4 medios auxiliares 7-4 Entrar tiempo mtodos 3-11 reactivo 2-5 sensor de temperatura 2-11 sensores 2-9 valores auxiliares 2-15 EP absoluto 3-41 relativo 3-41 EPOT 8-4 Esc (salir) mando (<F1>) 9 Estadsticas cambiar 6-22 incluir en el clculo 3-67 Estado mando a distancia 6-42 muestras 4-7 perifricos 2-18 Estn definidos (mscara) bloquear 6-30 significado 5-5 Estndar (procedimiento de evaluacin) explicacin 8-14 parmetro de evaluacin 3-34, 3-53 reconocimiento punto de equivalencia 3-28, 3-50 ET1 3-22, 3-38, 8-4 ET2 3-22, 3-38, 8-4 Evaluacin func. pH/mV-Stato 3-65 func. valoracin EQP 3-34 func. valoracin EQP (Ipol/Upol) 3-53
08/2004
13-13
Indice
Evaluacin posterior condicin satisfecha 5-11 definir una condicin 3-35, 3-36, 3-55 ejecucin 6-18 Experto (nivel de usuario) 6-31 Extincin 2-8 f (factor de correccin) 4-6, 5-6, 8-3 Fallos 9-6 Fecha entrar 6-27 seleccionar formato 6-26 Fecha caducidad (reactivo) 5-4 Forma de control (activar salida mando a distancia) control por entrada 6-33 marcha/parada 6-33 secuencial 6-34 Forma de control (func. salida mando a distancia) control por entrada 7-16 marcha/parada 7-16 secuencial 7-17 tiempo fijo 7-16 Frmula(s) constantes 8-18 funcin auxiliar clculos 6-20 funcin clculo 3-66 funcin ttulo 3-72 funcin valores auxiliares 3-73 para limitar los puntos de equivalencia 8-19 resultados 8-17 Funcin(es) aadir 7-8 borrar 7-8 cambiar 3-10 DL58 7-3 explicacin 20, 3-3 nmero mximo 7-9 seleccionar 3-7 visin de conjunto 24 Funciones auxiliares explicacin 9, 6-3 teclas 6-3 visin de conjunto 1-4, 1-5 Funciones de clculo 3-66 H (valor auxiliar) 2-15, 8-3 Hoja de datos tarjeta KF 10-12 tarjeta pH 10-12
ID mtodos cambiar 3-9 definir 3-11 entrar 4-4, 5-5 explicacin 3-4 mtodos estndar 3-5 mtodos METTLER 3-6 ID muestras 4-5, 5-6 Impresora ASCII 2-18 conectar 10-10 configuracin 2-19, 2-20 definir 2-18 In 3.1/3.2 (entradas TTL) 6-32 Incremental (adicin de reactivo) 3-24, 3-48, 7-14 Indicacin func. valoracin EP (Ipol/Upol) 3-57 func. valoracin EQP (Ipol/Upol) 3-46 Indicacin amperomtrica func. valoracin EP (Ipol/Upol) 3-58 func. valoracin EQP (Ipol/Upol) 3-47 Indicacin de fecha mtodos 3-11 reactivo 2-5 sensores 2-9 sondas de temperatura 2-11 valores auxiliares 2-15 Indicacin voltamtrica func. valoracin EP (Ipol/Upol) 3-57 func. valoracin EQP (Ipol/Upol) 3-46 Indicativos (forma) ejemplos 8-9, 8-10 resumen 8-12 Informe funcin 3-74 funcin auxiliar (Report) 6-24 Informe de comunicacin (ordenador) 2-24 Instalacin (men Setup) 2-3 Instalacin y mantenimiento 10-3 Instruccin funcin 7-11 funcin salida mando a distancia 7-17 Interface Centronics configuracin impresora 2-19 impresora GA42 2-18 Interface RS232 configuracin impresora 2-20 impresora GA42 2-20 Interpolacin (evaluacin) 8-14 Intervalo (acondicionamiento) 3-15 Intervalo de memorizacin (func. pH/mV-Stato) 3-64
13-14
08/2004
Indice
Juego de caracteres (ordenador) 2-24 LabX Software 4-13, 6-41 Lector de cdigo de barras conectar 10-16 definir 2-24 Lengua (cambiar) 11, 6-27 Lmites de peso entrar 3-12 en entrada de muestra 4-5, 5-6 Lmites volumen en entrada de muestras 4-5, 5-6 entrar 3-12 Lista (aclaracin) 8 Lista datos de muestras 4-4, 4-6 Lista de resultado avisos 5-9 bloquear 6-30 visualizar 6-18 Llenar (lavar) funcin auxiliar (ST20A) 6-10 parmetros cabeza de valoracin 3-14 Llenar punta (bureta) 6-12 M (masa molar) 3-68, 8-3 m (tamao muestra) 8-3 Mando a distancia 6-42 Mantenimiento bureta 10-7 titulador 10-3 Manual (entrada de temperatura) 3-13 Marcha/Parada activar salida mando a distancia (funcin auxiliar) 6-33 func. salida mando a distancia 7-16 Mrgenes (informe) 2-19 Masa molar M entrar 3-13 func. clculo 3-68 Mscara (aclaracin) 8 Mscara datos de muestras men anlisis 5-5 men muestras 4-5 Mximo (procedimiento de evaluacin) explicacin 8-14 parmetro evaluacin 3-34, 3-53 reconocimiento punto de equivalencia 3-28, 3-50
Medicin del voltaje (Ipol/Upol) 6-7 Medida de la conductividad 2-8 de la corriente (Ipol/Upol) 6-7 del pH 35 del potencial 6-4, 6-7 Medidas de seguridad en el puesto de trabajo 5 para su proteccin 5, 10-3 Medios auxiliares borrar 2-3 cambiar 2-3, 5-8 copiar en titulador 6-39 DL58 7-3 explicacin 2-3 imprimir 2-3 lista 2-3 transferir a ordenador 6-41 Medir (funcin) 3-17 Memoria de datos de muestras (men Sample) 4-3 de usuario 12-5 Memorizacin datos de muestras 4-3 electrodos polarizados 2-13 instrumento para entrada mando a distancia 7-5 instrumento para salida mando a distancia 7-6 mtodos 3-7 reactivos 2-6 resultados 8-20 resultados sin elaborar 8-20 sensores 2-10 solventes 2-28 sondas de temperatura 2-12 valores auxiliares 2-16 valores medidos 3-64, 3-74, 8-20 Memorizar valor auxiliar 3-73 Mens explicacin 8 teclas 8 visin de conjunto 1-2, 1-3
08/2004
13-15
Indice
Mtodo almacenar 3-7 borrar 3-5 cambiar 3-7 cambiar ( mtodo en curso: DL55/DL58) 5-13 cambiar (actual serie de muestras) 5-12 desde ordenador 4-5 desde tarjeta memoria 4-5 elaboracin 24 explicacin 3-3 imprimir 3-4 Mtodos imprimir lista 3-4 men 3-3 seleccionar 3-4 Mtodo(s) del usuario borrar 3-6 copiar en la tarjeta memoria 6-38 copiar en titulador 6-39 explicacin 19, 3-6 imprimir 3-6 ttulo con valoracin EQP 34 transferir a ordenador 6-41 Mtodo(s) estndar cambiar 25, 30 ejemplo de uso 22 explicacin 19, 3-5 funciones 20 imprimir 3-5 nmero 20 Mtodos especiales DL58 7-7 explicacin 7-3 Mtodos METTLER 90001: Ejecucin 14 90002: Ejecucin 27 cambiar 25, 3-6 explicacin 19 imprimir 3-6 Mnimo (procedimiento de evaluacin) explicacin 8-14 parmetro de evaluacin 3-34, 3-53 reconocimiento punto de equivalencia 3-28, 3-50 Misc. ... (Diversos) 6-26 Motor de bureta instalar 10-3 seleccionar 2-5
Muestra funcin 3-12 men memoria de datos de muestras 4-3 en curso (mscara): aviso 5-6 urgente (DL55) 4-10 Muestras estado 4-7 nmero mximo 8-20 neq (nmero punto(s) de equivalencia) 8-4 Nivel de usuario 6-31 Nombre funcin 3-11 mtodos estndar 19 mtodos METTLER- 19 Nmero de equivalencia entrada 3-13 func. clculo 3-68 OK mando (<F5>) 9 Ordenador cdigo de barras (string) 6-43 conectar 10-10 configuracin 2-23 lector de cdigo de barras 2-24 mando a distancia 6-42 transmisin de datos 6-40 Out 3.1...3.4 (salidas TTL) 6-33 P1/P2 8-6 Papel (impresora) formato 2-19 hojas nicas 2-19 papel sin fin 2-19 Parada para evaluacin posterior 3-35, 3-55, 5-11 Parada pospuesta 3-42, 3-61 Parmetros (aclaracin) 20 Paridad balanza 2-22 impresora 2-20 ordenador 2-23 terminal 2-25 Parte trasera del titulador 10-9 Pendiente clculo 3-69 electrodo de pH 26 explicacin 2-9 registrar 2-9 valor mximo/mnimo 3-71 valor terico 2-9
13-16
08/2004
Indice
Perifricos (men Setup) 2-18 Peso entrar 4-5, 5-6 seleccionar 3-12 transmisin desde balanza 4-12 pH-stato (ejemplo) 3-65 pH/mV-Stato (funcin) 3-62 Plato giratorio (cambiador de muestras) 6-10 Posicin elevador (cambiador de muestras) 6-9 Potencial 1/2 (parmetros de evaluacin) 3-35, 3-54 inicial ET1 3-22 Proceso de evaluacin explicacin 8-14 func. valoracin EQP 3-28, 3-34 func. valoracin EQP (Ipol/Upol) 3-50, 3-53 Punto cero (sensor) clculo 3-69 electrodo de pH 26 explicacin 2-9 registrar 2-9 valor terico 2-9 Punto cero (sensor de temperatura) explicacin 2-11 registrar 2-12 valor terico 2-12 Punto de equivalencia explicacin 3-20, 3-45, 8-14 frmulas para restriccin 8-19 nmero mx./determinacin muestras 8-20 rango 3-32, 3-51 reconocimiento 3-28, 3-50 Punto de inflexin 8-14 Punto final func. pH/mV-Stato 3-63 func. valoracin EP 3-41 func. valoracin EP (Ipol/Upol) 3-60 Puntos de medida para reconocimiento del punto de equivalencia 3-28, 3-44, 3-50 Q 8-4 QDISP 3-19, 8-7 QEND 8-4 QEX 8-4 QP1/QP2 8-4 QSTAT 8-6 QT1/QT2 8-6 QTOT 8-6
R (Resultado) 3-66, 8-7 Rango punto de equivalencia 3-32, 3-51 punto final 3-40, 3-60 Rango de regulacin func. pH/mV-Stato 3-63 func. valoracin EP 3-40 func. valoracin EP (Ipol/Upol) 3-60 Ranuras 10-9 Reactivo almacenar 2-6 aadir 2-6 borrar 2-4 cambiar 2-4 concentracin 2-4, 8-3 Reconocimiento (punto de equivalencia) 3-28, 3-50 Reduccin curso del anlisis 6-30 Registro (tarjeta memoria) 6-37 Reloj (titulador) 6 Report (informe) 6-24 Reset (tecla) 7, 5-12 Resultado(s) borrar 6-22 condiciones de memorizacin 8-20 ejemplos 3-67, 8-17 funcin auxiliar (Results) 6-18 hacer un informe 3-75, 6-24 nmero mximol/serie de muestras 8-20 R 3-66, 3-71 Rx 6-20 unidades 3-67, 8-17 valoracin de aprendizaje 5-9 Resultados sin elaborar condiciones de memorizacin 8-20 explicacin 3-18 hacer un informe 3-75, 6-24 resumen 8-8 Results (Resultados) 6-18 Run men anlisis 5-3 teclas funcin 5-3 Rutina (nivel de usuario) 6-31
08/2004
13-17
Indice
s (desviacin estndar) 8-7 Salida mando a distancia activar (funcin auxiliar) 6-33 funcin 7-16 Salidas mando a distancia definir 7-5 medios auxiliares 7-5 Secuencial activar salida mando a distancia (funcin auxiliar) 6-34 funcin salida mando a distancia 7-16 Segmentada (procedimiento de evaluacin) explicacin 8-15 parmetro de evaluacin 3-34, 3-53 reconocimiento punto de equivalencia 3-28, 3-50 Seal acstica 6-28 de entrada (func. entrada mando a distancia) 7-15 Sensor(es) almacenar 2-10 aadir 2-10 borrar 2-7 cambiar 2-7 funcin auxiliar 6-4 medios auxiliares 2-7 pH tarjeta 2-7 Serie de muestras borrar 4-6 con cabeza val. auto 5-6, 5-15 con ST20A 5-6, 5-15 entrar 4-4 Serie de muestras (DL55/DL58) ejecucin 5-15 entrar 4-9 Setup (men instalacin) 2-3 Smbolo inicial/final (ordenador) 2-24 Smbolos explicacin 8-3 lista 8-3 Sincronizacin (funcin) 7-18 Sistema informacin 9-3, 9-6 ordenador/terminal 2-23 SLOPE (pendiente de electrodos) 8-3 Software LabX 4-13, 6-41 Slo salto ms abrupto 3-31
Soluciones tampn tampones DIN/NIST 3-70 tampones MERCK 3-69 tampones METTLER TOLEDO 3-69 Solventes almacenar 2-28 aadir 2-28 borrar 2-27 cambiar 2-27 Sonda de temperatura almacenar 2-12 calibrar 6-6 enchufe Lemo 10-10 medios auxiliares 2-11 Pt100/Pt1000 2-11 seleccionar 3-13 srel (desviacin estndar relativa) 8-7 ST20A conectar 10-10 salidas 2-28 Stand 1/2 (cabezas de valoracin) 2-17 Stirrer (agitador) 6-8 Sustancia patrn 30, 31 T (temperatura) 7-10 t (ttulo) 3-72, 8-3 t(mx) func. medir 3-18 func. temperatura 7-10 func. valoracin EP 3-39 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 t(mn) func. medir 3-17 func. temperatura 7-10 func. valoracin EP 3-39 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 Tabla de valores medidos hacer un informe 3-75, 6-24 visualizar 5-7, 6-21 Tamao de muestras 3-21, 3-38, 3-48, 3-59, 8-3 Tarjeta Centronics installacin 10-10 posibilidades de conexin 10-9
13-18
08/2004
Indice
Tarjeta KF electrodos polarizados 2-13 entradas de medida: datos de calibracin 6-29 entradas y salidas 10-10 instalar 10-11 Tarjeta memoria directorio 6-37 formatizacin 6-36, 6-40 insercin 10-11 interface 12-6 tipos 12-6 uso 6-36 Tarjeta pH entradas de medida: datos de calibracin 6-29 entradas y salidas 10-10 instalar 10-11 sensores 2-7 Tarjeta RS instalacin 10-11 posibilidades de conexin 10-11 Tecla(s) de entrada 10 flecha 7 Reset 7, 5-12 de mandos 9 Teclado (titulador) 7 Teclado externo asignacin de las teclas 10-15 conectar 10-15 definir 2-26 Temperatura correccin 3-13, 3-69 entrar 2-9, 4-6, 5-6 funcin 7-10 medir 2-9, 3-13, 3-18, 3-20, 3-37, 3-62, 3-69, 7-10 medir (funcin auxiliar) 6-5 Tendencia func. pH/mV-Stato 3-64 func. valoracin EP 3-42 func. valoracin EP (Ipol/Upol) 3-61 func. valoracin EQP 3-32 func. valoracin EQP (Ipol/Upol) 3-51 Terminacin (parmetros) func. pH/mV-Stato 3-64 func. valoracin EP 3-42 func. valoracin EP (Ipol/Upol) 3-61 func. valoracin EQP 3-33 func. valoracin EQP (Ipol/Upol) 3-52
Terminal asignacin de teclas 10-17 conectar 10-11 configuracin 10-16 sincronizacin 2-25 Tiempo entrar 6-27 func. agitar 3-16, 5-7 func. muestra (acondicionar) 3-15 seleccionar formato 6-26 Tiempo de agitacin 3-16 de espera 3-16 de mezcla (func. valoracin en dos fases) 7-14 de separacin (func. valoracin en dos fases) 7-14 fijo (func. salida mando a distancia) 7-16 mx. (func. entrada mando a distancia) 7-15 mximo (func. valoracin EP (Ipol/Upol)) 3-61 TIME 5-4, 8-3 Tipo de medicin func. valoracin en dos fases 7-14 func. valoracin EQP 3-25 func. valoracin EQP (Ipol/Upol) 3-49 Tipo de sincronizacin (func. sincronizacin) 7-18 Tipo de transmisin (balanza) bidireccional 2-21 unidireccional 2-21 Tipo de transmisin (ordenador) 2-24 Titulador acumulador 6 apertura de la carcasa 10-3 autotest 7 conexiones 6, 10-10 configuracin 6-26 documentacin 4 ID (identificacin ) 6-27 limpieza de la carcasa 10-3 mando a distancia 6-42 reloj interno 6 teclado 7 vista frontal 6 vista trasera 6, 10-10 Ttulo controlar 2-5 determinacin (disolucin NaOH) 32 entrar 2-4 explicacin 30 funcin 3-72 registrar 2-4 Transmisin de datos (Data Transfer) 6-36
08/2004
13-19
Indice
TTL (entradas) activar 6-32 cableado electrnico 10-14 cableado mecnico 10-13 TTL (salidas) activar 6-33 cableado electrnico 10-14 TTLIO (conectores) datos tcnicos 12-7 entradas y salidas 10-13 usado con titulador 10-13 Umbral 3-29, 3-51 Unidad de medida (sensores) 2-8 Unidades 3-67, 8-17, 8-18 Valoracin a punto de equivalencia 3-20, 3-45 a punto final 3-37, 3-56 de aprendizaje funcin 3-43 en dos fases funcin 7-12 EP (funcin) 3-37 EP (Ipol/Upol) (funcin) 3-56 EQP (funcin) 3-20 EQP (Ipol/Upol) (funcin) 3-45 manual 6-14 manual (Ipol/Upol) 6-16 mtodo especial 7-12 previa (func. pH/mV-Stato) 3-63 resultados 5-9 Valoraciones Karl-Fischer accesorios 11-12 Valor del umbral procedimiento de evaluacin estndar 3-30 procedimiento de evaluacin: asimtrica 3-30 procedimiento de evaluacin: mnimo/mximo 3-30 procedimiento de evaluacin: segmentada 3-31 Valor de semineutralizacin 3-20 Valor medio x func. clculo 3-67 func. ttulo 3-72 func. valor auxiliar 3-73 Valor(es) auxiliar(es) almacenar 2-16 entrar 2-15 funcin 3-73 medios auxiliares 2-15 registrar 2-15 Valores medidos instrucciones para memorizacin 3-64, 3-74, 8-20 nmero mximo/func. valoracin 8-20 visualizar 5-7, 6-21 13-20
VDISP 3-19, 8-7 Velocidad bombeo (solventes) 2-27 Velocidad de agitacin cambiar 5-8, 6-8 definir 3-16 VEND 8-4 VEQ 8-4 Version software 1-1 VEX 8-4 Volumen entrar 4-5, 5-6 seleccionar 3-12 Volumen bureta incremento mnimo 3-24 seleccionar 2-5 Volumen fijo aviso 5-5 seleccionar 3-12 Volumen mximo func. pH/mV-Stato 3-64 func. valoracin EP 3-42 func. valoracin EP (Ipol/Upol) 3-61 func. valoracin EQP 3-33 func. valoracin EQP (Ipol/Upol) 3-52 VP1/VP2 8-4 VSTAT 8-6 VT 3-65, 8-6 VT1/VT2 8-6 VTOT 8-6 x (valor medio) 8-7 z (valencia, n de equivalencia) 3-13, 3-68, 8-3 ZERO (punto cero, electrodo) 8-3
08/2004
Indice analitico
Indice analitico
I numeri separati da un trattino (esempio: 3-38) si riferiscono alle sezioni e pagine del manuale d'uso, mentre i numeri senza trattino si riferiscono alle istruzioni di base (esempio: 9).
<F1>...<F5> 9, 10 E funzione Misurare 3-17 funzione Titolazione EP 3-39 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 E(nom.) funzione Titolazione EP 3-39 funzione Titolazione EQP 3-22 t funzione Misurare 3-17 funzione Titolazione EP 3-39 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 Abbreviare lanalisi 6-30 Accessori accessori facoltativi 11-7 equipaggiamento di base 11-4 Accumulatore 6 Aggiunta di titolante funzione pH/mV-Stat 3-63 funzione Titolazione a due fasi 7-14 funzione Titolazione EP 3-39 funzione Titolazione EP (Ipol/Upol) 3-60 funzione Titolazione EQP 3-22 funzione Titolazione EQP (Ipol/Upol) 3-48 Agitare (funzione) 3-16 Agitatore funzione ausiliaria (Stirrer) 6-8 selezionare luscita 2-17 Allineamento degli ingressi di misura 6-28 Analisi arresto 5-11 eclissare 5-11 inizio 5-4 interrompere (Reset) 5-12 menu Run 5-3 svolgimento del menu 5-4 Arresto (parametri di) funzione pH/mV-Stat 3-64 funzione Titolazione EP 3-42 funzione Titolazione EP (Ipol/Upol) 3-61 funzione Titolazione EQP 3-33 funzione Titolazione EQP (Ipol/Upol) 3-52 Arresto per rivalutazione 3-35, 3-55, 5-11 Asimmetrico (procedura di valutazione) parametro di valutazione 3-34, 3-53 riconoscimento del punto dequivalenza 3-28, 3-50 spiegazione 8-16 Asterisco (*) 3-4, 3-11 Attivare entrata comando a distanza 6-32 uscita comando a distanza 6-32 Autocampionatore collegare 10-10 definire 2-25 funzione ausiliaria (Changer) 6-9 parametri dello stativo di titolazione 3-13 serie di campioni 5-6, 5-15 stativo di titolazione 2-17 Avanzamento della pagina (stampante) 2-19 delle linee (stampante) 2-19 Banca dati 12-5 Banda di controllo funzione pH/mV-Stat 3-63 funzione Titolazione EP 3-40 funzione Titolazione EP (Ipol/Upol) 3-60 Bidirezionale (modo di trasmissione) 2-21, 4-12 Bilancia(e) collegare 10-10 configurazioni (METTLER TOLEDO) 2-22 configurazioni (SARTORIUS) 2-22 definire 2-21 Buretta bolle daria 10-8 inserire 10-6 installare 10-4 lavare 6-11 manutenzione 10-4, 10-7 montare 10-5 riempire 13 Burette (buretta, funz. ausil.) 6-11
08/2004
13-21
Indice analitico
C (costante) 3-66, 8-7 c (conc. nominale) 8-3 c * t (conc. reale) 8-3 Calcoli supplementari 6-20 Calcolo(i) eseguire (funzione ausiliaria) 6-20 formule 8-17 funzione 3-66 indici 8-9 Calibrare elettrodo pH 27 funzione 3-69 sonde 3-69 sonde della temperatura 6-6 Cambiare la lingua 11, 6-27 Campione (funzione) 3-12 Campione attuale (maschera) indicazioni 5-6 Campione urgente (DL55/DL58) 4-10 Campioni numero massimo 8-20 stato 4-7 Campo (punto di equivalenza) 3-32, 3-51 Campo di regolazione funzione pH/mV-Stat 3-63 funzione Titolazione EP 3-40 funzione Titolazione EP (Ipol/Upol) 3-60 Carattere iniziale/finale (computer) 2-24 Carta (stampante) formato 2-19 infinito 2-19 pagina singola 2-19 Changer (autocampionatore, funz. ausil.) 6-9 Code (funzione Sync) 7-18 Codice a barre 6-43 Coefficiente di correlazione 3-62, 3-65, 8-6 Comando a distanza 6-42 Combinazioni di tasti 10 Computer codice a barre 6-43 collegare 10-10 comando a distanza 6-42 configurazione (titolatore) 2-23 lettore di codici a barre 2-24 trasmissione dei dati 6-40 Concentrazione (titolante) 2-4, 8-3 Concetto dimpiego 7 di metodo 19 Condizionare (ST20A) 3-15 Condizioni di arresto combinate 3-34, 3-53 Conduttimetro 2-8
Connettore(i) TTLIO dati tecnici 12-7 ingressi ed uscite 10-13 utilizzati dal titolatore 10-13 Continua (aggiunta di titolante) 3-40, 3-60 Controllo dallingresso attivare luscita comando a distanza (funzione ausiliaria) 6-33 funzione Uscita comando a distanza 7-16 Copia(e) della memoria caricare sul titolatore 6-39 copiare su scheda di memoria 6-39 trasferire al computer 6-41 Costanti esempi 8-18 funzione ausiliaria Calcoli 6-20 funzione Calcolo 3-66 CSTAT (coefficiente di correlazione, pH-Stat) 3-62, 8-6 Cursore 10 Curve di titolazione 1a derivata 3-30, 3-31, 3-54, 8-15 2a derivata 3-31, 3-54, 8-15 documentare 3-75, 6-24 visualizzare 5-7, 5-8, 6-21 Cx (costante di calcolo) 8-7 Data introdurre 6-27 selezionare il formato 6-26 Data (indicazione) metodi 3-11 sonde 2-9 sonde della temperatura 2-11 titolanti 2-5 valori ausiliari 2-15 Data di scadenza (titolante) 5-4 Data Transfer (trasferimento dei dati, funz. ausil.) 6-36 Dati di calibrazione ingressi di misura 6-29 sonde 2-9, 2-10, 3-69 sonde della temperatura 2-12 Dati dei campioni aggiungere 4-8 cancellare 4-6 condizioni di memorizzazione 36, 4-3 definire dal computer 4-13 documentare 3-75, 6-24 introdurre 4-4, 5-5, 5-10 modificare 4-7 stampare 4-7
13-22
08/2004
Indice analitico
Dati tecnici agitatore 12-5 buretta 12-5 connettore Centronics 12-8 connettore RS232C (Opzione RS) 12-9 connettori TTLIO 12-7 display 12-5 connettore DIN 12-7 memoria 12-5 motore della buretta 12-5 periferiche 12-6 sistema di misura 12-3 spina RS232C (Opzione Centronics) 12-7 uscite 12-4 Deriva (misura del potenziale) 3-17 Deviazione standard relativa srel 3-67 Deviazione standard s 3-67 Dinamica (aggiunta di titolante) funzione Titolazione EP 3-39 funzione Titolazione EQP 3-22 Disturbi 9-6 DL58 comandi 7-3 funzioni 7-3 mezzi ausiliari 7-3 DLWin Software 4-13, 6-41 Documentazione informazioni 4 Dosaggio continuo 6-13 continuo (Ipol/Upol) 6-15 Dosare funzione 3-19 funzione ausiliaria (buretta) 6-12 funzione ausiliaria (ST20A) 6-10 E (potenziale) 3-17, 8-7 ESC (<F1>) 9 EHNV (valore di semineutralizzazione) 3-20, 8-4 Elettrodi (METTLER TOLEDO) 2-7, 2-13 Elettrodo di riferimento 2-7 Elettrodo per pH calibrare 26 pendenza 26 punto zero 26 Emissione (protocolli) 3-74, 6-24 EP assoluto 3-41 relativo 3-41 EPOT 8-4 Esperto (livello utente) 6-31 Estinzione 2-8 ET1 3-22, 3-38, 8-4 ET2 3-22, 3-38, 8-4
f (fattore di correzione) 4-6, 5-6, 8-3 Formula(e) costanti 8-18 funzione ausiliaria Calcoli 6-20 funzione Calcolo 3-66 funzione Titolo 3-72 funzione Valore ausiliario 3-73 per circoscrivere il punto di equivalenza 8-19 risultati 8-17 Funzione(i) aggiungere 7-8 cancellare 7-8 DL58 7-3 modificare 3-10 numero massimo 7-9 riassunto 24 selezionare 3-7 spiegazione 20, 3-3 Funzioni ausiliarie riassunto 1-4, 1-5 spiegazione 9, 6-3 tasti 6-3 Funzioni di calcolo 3-66 H (valore ausiliario) 2-15, 8-3 ID (identificazione) dei metodi definire 3-11 introdurre 4-4, 5-5 metodi METTLER 3-6 metodi standard 3-5 modificare 3-9 spiegazione 3-4 ID del campione 4-5, 5-6 In 3.1/3.2 (ingressi TTL) 6-32 In funzione/stop (modo di controllo) attivare uscita comando a distanza (funzione ausiliaria) 6-33 funzione Uscita comando a distanza 7-16 Incrementale (aggiunta di titolante) 3-24, 3-48, 7-14 Indicazione funzione Titolazione EP (Ipol/Upol) 3-57 funzione Titolazione EQP (Ipol/Upol) 3-46 Indicazione amperometrica funzione Titolazione EP (Ipol/Upol) 3-58 funzione Titolazione EQP (Ipol/Upol) 3-47 Indicazione del tempo metodi 3-11 sonde 2-9 sonde della temperatura 2-11 titolanti 2-5 valori ausiliari 2-15
08/2004
13-23
Indice analitico
Indicazione voltametrica funzione Titolazione EP (Ipol/Upol) 3-57 funzione Titolazione EQP (Ipol/Upol) 3-46 Indicazioni di sicurezza 1-1 Indice (scheda di memoria) 6-37 Indici esempi 8-9, 8-10 riassunto 8-12 Ingressi del comando a distanza definire 7-4 mezzi ausiliari 7-4 Ingressi TTL attivare 6-32 avvolg. elettronico (wiring) 10-14 avvolg. meccanico 10-13 Ingresso del comando a distanza attivare (funzione ausiliaria) 6-32 funzione 7-15 Ingresso delle sonde sonde 2-8 sonde della temperatura 2-11 sonde polarizzate 2-13 Installazione (menu "Setup") 2-3 Installazione e manutenzione 10-3 Interfaccia Centronics configurazioni delle stampanti 2-19 stampante GA42 2-18 Interfaccia RS232 configurazioni delle stampanti 2-20 stampante GA42 2-20 Interpolazione (valutazione) 8-14 Intervallo (condizionare) 3-15 Intervallo di memorizzazione (funz. pH/mV-Stat) 3-64 Istruzione ESC (<F1>) 9 funz. Uscita comando a distanza 7-17 funzione 7-11 OK (<F5>) 9 modificare (<F4>) 10 LabX Software 4-13, 6-41 Lavare funzione ausiliaria (ST20A) 6-10 parametri dello stativo di titolazione 3-14 la punta 6-12 Lettore di codici a barre collegare 10-16 definire 2-24 Limiti di peso introdurre 3-12 introduzione dei dati dei campioni 4-5, 5-6
Limiti di volume introdurre 3-12 introduzione dei dati dei campioni 4-5, 5-6 Linee di cornice (protocollo) 2-19 Lingua (cambiare) 11, 6-27 Lista dei dati dei campioni 4-4, 4-6 Lista dei risultati bloccare 6-30 indicazioni 5-9 visualizzare 6-18 Liste (spiegazione) 8 Livello utente 6-31 M (massa molare) 3-68, 8-3 m (quantit del campione) 8-3 Manuale (introduzione della temperatura) 3-13 Manutenzione buretta 10-7 titolatore 10-3 Maschera dei dati del campione menu Analisi 5-5 menu "Sample" 4-5 Maschere (spiegazione) 8 Massa molare M introdurre 3-13 funzione Calcolo 3-68 Massimo (procedura di valutazione) parametri di valutazione 3-34, 3-53 riconoscimento del punto dequivalenza 3-28, 3-50 spiegazione 8-14 Memoria dei dati dei campioni (menu "Sample") 4-3 Memoria dei dati utente 12-5 Memoria dei valori ausiliari 3-73 Memorizzare dati dei campioni 4-3 metodi 3-7 risultati 8-20 risultati grezzi 8-20 sensori polarizzati 2-13 solventi 2-28 sonde 2-10 sonde della temperatura 2-12 strumenti per ingresso comando a distanza 7-5 strumenti per uscita comando a distanza 7-6 titolanti 2-6 valori ausiliari 2-16 valori misurati 3-64, 3-74, 8-20 Menus riassunto 1-2, 1-3 spiegazione 8 tasti 8
13-24
08/2004
Indice analitico
Messaggi di errore con riferimento al cap. 9.1 9-3 "EPROM test failed" 9-3 "RAM test failed" 9-3 Titolazione in auto-studio 5-11 Metodi menu 3-3 selezionare 3-4 stampare la lista 3-4 Metodi METTLER 90001: Esecuzione 14 90002: Esecuzione 27 modificare 25, 3-6 spiegazione 19 stampare 3-6 Metodi speciali DL58 7-7 spiegazione 7-3 Metodi standard esempi di applicazione 22 funzioni 20 modificare 25, 30 numero 20 spiegazione 19, 3-5 stampare 3-5 Metodi utente cancellare 3-6 copiare su scheda di memoria 6-38 copiare sul titolatore 6-39 spiegazione 19, 3-6 stampare 3-6 titolo con titolazione EQP 34 trasferire al computer 6-41 Metodo a partire dal computer 4-5 cancellare 3-5 memorizzare 3-7 modificare 3-7 modificare (metodo in corso: DL55/DL58) 5-13 modificare (serie di campioni in corso) 5-12 realizzare 24 spiegazione 3-3 stampare 3-4 sulla scheda di memoria 4-5 Mezzi ausiliari cambiare 5-8 cancellare 2-3 copiare su scheda di memoria 6-39 copiare sul titolatore 6-39 DL58 7-3 lista 2-3 modificare 2-3 spiegazione 2-3 stampare 2-3 trasferire al computer 6-41 08/2004
Minimo (procedura di valutazione) parametro di valutazione 3-34, 3-53 riconoscimento del punto di equivalenza 3-28, 3-50 spiegazione 8-14 Misc. ... (Varia) 6-26 Misura controllata allequilibrio funzione Misurare 3-17 funzione Titolazione EP 3-39 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 Misura in modo incrementale (tempo) funzione Titolazione EP 3-41 funzione Titolazione EP (Ipol/Upol) 3-60 funzione Titolazione EQP 3-27 funzione Titolazione EQP (Ipol/Upol) 3-49 Misurare funzione 3-17 il pH 35 il potenziale 6-4, 6-7 la corrente (Ipol/Upol) 6-7 la tensione (Ipol/Upol) 6-7 Misure di conducibilit 2-8 Misure di sicurezza per la sicurezza sul lavoro 5 per la Sua incolumit 5, 10-3 Modificare: istruzione (<F4>) 10 Modo di controllo (attivare uscita TTL) controllato dallentrata 6-33 in funzione/stop 6-33 sequenziale 6-34 Modo di controllo (uscite TTL) controllato dallentrata 7-16 in funzione/stop 7-16 sequenziale 7-17 tempo fisso 7-16 Modo di misura funzione Titolazione a due fasi 7-14 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 Modo di sincronizzazione (funzione Sync) 7-18 Modo di trasmissione (computer) 2-24 Modo di trasmissione (bilancia) bidirezionale 2-21 unidirezionale 2-21 Motore della buretta inserire 10-3 selezionare 2-5
13-25
Indice analitico
neq (numero di punti di equivalenza) 8-4 No. bits dei dati computer 2-24 stampante 2-20 terminale 2-25 No. bits di stop computer 2-24 stampante 2-20 terminale 2-25 Numero di equivalenza funzione Calcolo 3-68 introdurre 3-13 OK (<F5>) 9 Opzione Centronics installare 10-10 possibilit di collegamento 10-9 Opzione KF ingressi di misura: dati di calibrazione 6-29 ingressi ed uscite 10-10 installare 10-11 sonde polarizzate 2-13 Opzione pH ingressi di misura: dati di calibrazione 6-29 ingressi ed uscite 10-10 installare 10-11 sonde 2-7 Opzione RS installare 10-11 possibilit di collegamento 10-11 Orologio (titolatore) 6 Out 3.1...3.4 (uscite TTL) 6-33 P1/P2 8-6 Parametri (spiegazione) 20 Parit bilance 2-22 computer 2-23 stampante 2-20 terminale 2-25 Pendenza calcolo 3-69 elettrodo per pH 26 spiegazione 2-9 trascrizione automatica 2-9 valore minimo/massimo 3-71 valore teorico 2-9 Periferiche (menu "Setup") 2-18 Peso introdurre 4-5, 5-6 selezionare 3-12 trasferire dalla bilancia 4-12
pH-Stat (esempio) 3-65 pH/mV-Stat (funzione) 3-62 Piatto rotante (autocampionatore) 6-10 Pistone inserire nella buretta 10-4 montare 10-4 Pompe funzione 7-11 parametri dello stativo di titolazione 3-13 Posizione del lift (autocampionatore) 6-9 Posizioni delle opzioni 10-9 Potenziale 1/2 (parametri di valutazione) 3-35, 3-54 iniziale ET1 3-22 Predosaggio funzione Titolazione a due fasi 7-13 funzione Titolazione EP 3-38 funzione Titolazione EP (Ipol/Upol) 3-59 funzione Titolazione EQP 3-21 funzione Titolazione EQP (Ipol/Upol) 3-48 Pretitolazione (funzione pH/mV-Stat) 3-63 Procedura di valutazione funzione Titolazione EQP 3-28, 3-34 funzione Titolazione EQP (Ipol/Upol) 3-50, 3-53 spiegazione 8-14 Protocollo funzione 3-74 funzione ausiliaria (Report) 6-24 di comunicazione (computer) 2-24 Punti di misura condizioni di memorizzazione 3-64, 3-74, 8-20 numero massimo/funz. Titolazione 8-20 visualizzare 5-7, 6-21 Punti di misura per il riconoscimento del punto di equivalenza 3-28, 3-44, 3-50 Punto di inflessione 8-14 Punto finale funzione pH/mV-Stat 3-63 funzione Titolazione EP 3-41 funzione Titolazione EP (Ipol/Upol) 3-60 Punto zero (sonda) calcolo 3-69 elettrodo per pH 26 spiegazione 2-9 trascrizione automatica 2-9 valore teorico 2-9 Punto zero (sonda della temperatura) spiegazione 2-11 trascrizione automatica 2-12 valore teorico 2-12
13-26
08/2004
Indice analitico
Punto(i) di equivalenza campo 3-32, 3-51 formule per circoscrivere 8-19 numero massimo/determinazione di campioni 8-20 riconoscimento 3-28, 3-50 spiegazione 3-20, 3-45, 8-14 Q 8-4 QDISP 3-19, 8-7 QEND 8-4 QEX 8-4 QP1/QP2 8-4 QSTAT 8-6 QT1/QT2 8-6 QTOT 8-6 Quantit del campione 3-21, 3-38, 3-48, 3-59, 8-3 R (risultati) 3-66, 8-7 Report (protocollo) 6-24 Reset (tasto) 7, 5-12 Results (risultati) 6-18 Riconoscimento (punto di equivalenza) 3-28, 3-50 Risultati grezzi condizioni di memorizzazione 8-20 documentare 3-75, 6-24 riassunto 8-8 spiegazione 3-18 Risultato(i) cancellare 6-22 condizioni di memorizzazione 8-20 documentare 3-75, 6-24 esempi 3-67, 8-17 funzione ausiliaria (Results) 6-18 numero massimo/serie di campioni 8-20 R 3-66, 3-71 Rx 6-20 titolazione in auto-studio 5-9 unit 3-67, 8-17 Ritardo nellarresto 3-42, 3-61 Rivalutazione condizione soddisfatta 5-11 definire la condizione 3-35, 3-36, 3-55 eseguire 6-18 Routine (livello utente) 6-31 Run funzione dei tasti 5-3 menu Analisi 5-3
s (deviazione standard) 8-7 Sample (menu Memoria dei dati dei campioni) 4-3 Scheda di memoria formattare 6-36, 6-40 indice 6-37 inserire 10-11 interfaccia 12-6 tipi 12-6 uso 6-36 Scheda tecnica opzione KF 10-12 opzione pH 10-12 Segmentato (procedura di valutazione) parametro di valutazione 3-34, 3-53 riconoscimento del punto di equivalenza 3-28, 3-50 spiegazione 8-15 Segnale acustico 6-28 dingresso (funz. ingresso comando a dist.) 7-15 Sequenziale attivare luscita comando a distanza (funzione ausiliaria) 6-34 funzione Uscita comando a distanza 7-17 Serie di campioni cancellare 4-6 con ST20A 5-6, 5-15 con stativo auto 5-6, 5-15 introdurre 4-4 Serie di campioni (DL55/DL58) eseguire 5-15 introdurre 4-9 Setup (menu Installazione) 2-3 simboli lista 8-3 spiegazione 8-3 Sistema computer/terminale 2-23 informazioni 9-3, 9-6 SLOPE (pendenza degli elettrodi) 8-3 Software LabX 4-13, 6-41 Soglia 3-29, 3-51 Solo il salto pi ripido 3-31 Soluzioni tampone tamponi DIN/NIST 3-70 tamponi MERCK 3-69 tamponi METTLER TOLEDO 3-69 Solventi aggiungere 2-28 cancellare 2-27 memorizzare 2-28 modificare 2-27
08/2004
13-27
Indice analitico
Sonda Pt100/Pt1000 2-11 Sonda(e) aggiungere 2-10 cancellare 2-7 funzione ausiliaria 6-4 mezzi ausiliari 2-7 modificare 2-7 opzione pH 2-10 Sonda(e) della temperatura calibrare 6-6 memorizzare 2-12 mezzi ausiliari 2-11 Pt100/Pt1000 2-11 selezionare 3-13 spina per connettore Lemo 10-10 Sonda(e) polarizzate aggiungere 2-14 memorizzare 2-13 mezzi ausiliari 2-13 modificare 2-13 opzione KF 2-13 Sono definiti (maschera) bloccare 6-30 significato 5-5 Sostanza standard primaria 30, 31 srel (deviazione standard relativa) 8-7 ST20A collegare 10-10 uscite 2-28 Stampante ASCII 2-18 collegare 10-10 configurazioni 2-19, 2-20 definire 2-18 Standard (procedura di valutazione) parametro di valutazione 3-34, 3-53 riconoscimento del punto di equivalenza 3-28, 3-50 spiegazione 8-14 Statistica modificare 6-22 includere nel calcolo 3-67 Stativo 1/2 (stativi di titolazione) 2-17 Stativo auto definizione 2-17 serie di campioni 5-6, 5-15 Stativo di titolazione mezzi ausiliari 2-17 montare 10-8 no. di comanda 11-7 selezionare 3-13 significato 7-8
Stativo esterno 2-17 Stato campioni 4-7 comando a distanza 6-42 periferiche 2-18 Stirrer (agitatore) 6-8 Svolgimento dellanalisi (esempi) calibrazione dell'elettrodo per pH 27 con lautocampionatore 5-17 confronto: stativo di titol. 1/ST20A 5-16 determinazione del titolo (NaOH) 32 determinazione di CaCl2 5-7 titolazione pH-Stat 5-10 Sync (funzione) 7-18 T (temperatura) 7-10 t (titolo) 3-72, 8-3 t(max) funzione Misurare 3-18 funzione Temperatura 7-10 funzione Titolazione EP 3-39 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 t(min) funzione Misurare 3-17 funzione Temperatura 7-10 funzione Titolazione EP 3-39 funzione Titolazione EQP 3-25 funzione Titolazione EQP (Ipol/Upol) 3-49 Tabella dei valori misurati documentare 3-75, 6-24 visualizzare 5-7, 6-21 Tasti delle istruzioni 9 di introduzione 10 freccia 7 Reset 7, 5-12 Tastiera esterna 2-26 titolatore 7 Tastiera esterna assegnazione dei tasti 10-15 collegare 10-15 definire 2-26 Temperatura correttura 3-13, 3-69 funzione 7-10 introdurre 2-9, 4-6, 5-6 misurare 2-9, 3-13, 3-18, 3-20, 3-37, 3-62, 3-69, 7-10 misurare (funzione ausiliaria) 6-5
13-28
08/2004
Indice analitico
Tempo di agitazione 3-16 di attesa 3-16 di mescolazione (funz. Titol. a due fasi) 7-14 di separazione (funz. Titol. a due fasi) 7-14 fisso (funz. Uscita comando a dist.) 7-16 funzione Agitare 3-16, 5-7 funzione Campione (condizionare) 3-15 introdurre 6-27 massimo (funz. Ingresso comando a dist.) 7-15 massimo (funzione Titolazione EP (Ipol/Upol)) 3-61 selezionare il formato 6-26 TIME 5-4 Tendenza funzione pH/mV-Stat 3-64 funzione Titolazione EP 3-42 funzione Titolazione EP (Ipol/Upol) 3-61 funzione Titolazione EQP 3-32 funzione Titolazione EQP (Ipol/Upol) 3-51 Terminale assegnazione dei tasti 10-17 collegare 10-11 configurazione 10-16 configurazione (titolatore) 2-25 Testata del protocollo 6-27 TIME 5-4, 8-3 Titolante aggiungere 2-6 cancellare 2-4 concentrazione 2-4, 8-3 memorizzare 2-6 modificare 2-4 Titolatore accumulatore 6 aprire linvolucro 10-3 autodiagnosi 7 collegamenti 6, 10-10 comando a distanza 6-42 configurazione (titolatore) 6-26 documentazione 4 ID (identificazione) 6-27 orologio interno 6 pulire linvolucro 10-3 tastiera 7 vista anteriore 6 vista dorsale 6, 10-10
Titolazione a punto dequivalenza 3-20, 3-45 a punto finale 3-37, 3-56 EP (funzione) 3-37 EP (Ipol/Upol) (funzione) 3-56 EQP (funzione) 3-20 EQP (Ipol/Upol) (funzione) 3-45 manuale 6-14 manuale (Ipol/Upol) 6-16 Titolazione a due fasi funzione 7-12 metodo speciale 7-12 Titolazione in auto-studio funzione 3-43 resultati 5-9 Titolazione Karl Fischer accessori 11-12 Titolo funzione 3-11 metodi METTLER 19 metodi standard 19 Titolo (concentrazione) controllare 2-5 determinazione (sol. di NaOH) 32 funzione 3-72 introdurre 2-4 spiegazione 30 trascrizione automatica 2-4 Trasferimento dei dati (Data Transfer) 6-36 Unidirezionale (modo di trasmissione) 2-21 Unit 3-67, 8-17, 8-18 Unit di misura (sonde) 2-8 Uscita del comando a distanza attivare (funzione ausiliaria) 6-33 funzione 7-16 Uscite del comando a distanza definire 7-5 mezzi ausiliari 7-5 Uscite TTL attivare 6-33 avvolg. elettronico (wiring) 10-14
08/2004
13-29
Indice analitico
Valore(i) ausiliare(i) funzione 3-73 introdurre 2-15 memorizzare 2-16 mezzi ausiliari 2-15 trascrizione automatica 2-15 Valore di semineutralizzazione 3-20 Valore di soglia procedura di valutazione: asimmetrico 3-30 procedura di valutazione: minimo/massimo 3-30 procedura di valutazione: segmentato 3-31 procedura di valutazione: standard 3-30 Valore medio x funzione Calcolo 3-67 funzione Titolo 3-72 funzione Valore ausiliario 3-73 Valutazione funzione pH/mV-Stat 3-65 funzione Titolazione EQP 3-34 funzione Titolazione EQP (Ipol/Upol) 3-53 Varia (Misc. ...) 6-26 VDISP 3-19, 8-7 Velocit (agitatore) definire 3-16 modificare 5-8, 6-8 Velocit della pompa (solventi) 2-27 Velocit di trasmissione bilance 2-22 computer 2-23 stampante 2-20 terminale 2-25 VEND 8-4 VEQ 8-4 Versione del software 1-1 VEX 8-4 Vista dorsale del titolatore 10-9 Volume introdurre 4-5, 5-6 selezionare 3-12 Volume della buretta lincremento pi piccolo 3-24 selezionare 2-5 Volume fisso avviso 5-5 selezionare 3-12 Volume massimo funzione pH/mV-Stat 3-64 funzione Titolazione EP 3-42 funzione Titolazione EP (Ipol/Upol) 3-61 funzione Titolazione EQP 3-33 funzione Titolazione EQP (Ipol/Upol) 3-52
VP1/VP2 8-4 VSTAT 8-6 VT 3-65, 8-6 VT1/VT2 8-6 VTOT 8-6 x (valore medio) 8-7 z (numero di equivalenza) 3-13, 3-68, 8-3 ZERO (punto zero degli elettrodi) 8-3
13-30
08/2004
Contents
Page ISO 9001 certificate for METTLER TOLEDO ...................................................................... Certificado ISO 9001 para METTLER TOLEDO ................................................................. Certificato ISO 9001 per la METTLER TOLEDO ................................................................ Declaration of System Validation ................................................................................ Dclaracin de validacin del sistema ........................................................................ Dichiarazione di validazione del sistema .................................................................... 15-3 15-3 15-3 15-4 15-6 15-8
08/2004
15-1
ISO 9001 certificate for METTLER TOLEDO The Mettler-Toledo GmbH company, Greifensee, was examined and evaluated in 1991 by the Swiss Association for Quality and Management Systems (SQS), and was awarded the ISO 9001 certificate. This certifies that Mettler-Toledo GmbH, Greifensee, has a quality management system that conforms with the international standards of the ISO 9000 series. Repeat audits are carried out by the SQS at intervals to check that the quality management system is operated in the proper manner and is continuously updated in relation to changes brought about. Certificado ISO 9001 para METTLER TOLEDO La firma Mettler-Toledo GmbH, Greifensee, ha sido inspeccionada por la Asociacin Suiza para Sistemas de Calidad y Gestin (SQS), habiendo obtenido el certificado ISO 9001. Esto acredita que Mettler-Toledo GmbH, Greifensee, dispone de un sistema de gestin de calidad que cumple las normas internacionales (ISO serie 9000). Con motivo de las inspecciones de repetibilidad por parte de la SQS, se comprueba peridicamente si el sistema de gestin de calidad se manipula correctamente y se ajusta de modo continuo. Certificato ISO 9001 per la METTLER TOLEDO Il sistema di garanzia della qualit della Societ Mettler-Toledo GmbH, Greifensee, certificato ISO 9001 sin dal 1991 dall'Associazione Svizzera per Sistemi di Qualit e di Gestione (SQS), e cos fornisce la dimostrazione che il suo sistema Garanzia di Qualit soddisfa i massimi requisiti. Il sistema della garanzia della qualit Mettler-Toledo viene verificato periodicamente SQS, dando cos evidenza di un continuo aggiornamento e corretta gestione.
08/2004
15-3
Declaration of System Validation

We herewith inform you that the products/systems:
DL50, DL53, DL55, DL58

including software and accessories were developed, tested and successfully validated according to the international ISO9001:1994 based Life cycle rules of Mettler-Toledo GmbH, Analytical. Life cycle checkpoint details were reviewed and approved by the Project Supervisory Group (PSG). The products/systems were tested to meet functional and performance specifications and release criteria at release to shipment. In order to support GLP and validation requirements, we will make the following documents available to an authorized, governmental or regulatory agency for inspection.
Product Guidelines Performance Specifications Documentation Plan Software Specifications Quality Plan Project Management System Test Plan Customer Requirements Review Reports Source Code
Mettler-Toledo GmbH, Analytical will maintain possession of all documents and their reproductions and may require a non-disclosure agreement to be provided by those requiring access to these documents.
Schwerzenbach, January 1999
Dr. Bernhard Grob General Manager Business Unit Analytical
Dr. Urs Spitz Manager Business Area Titration
15-4
08/2004
Product Life Cycle Model Ideas
Project Study
Project Release
Project Start
Phase: Basic Know how
Product Guidelines Performance Specifications Quality Plan Documentation Plan Project Plan Review Report
Phase: Feasibility
Software Specifications Test Plan Review Report
Phase: Confirmation Phase: Readiness
Review Report
Project End
Review Report
Usage
Customer Complaints (CRIS) Customer Requirements
Phase out
08/2004
15-5
Dclaracin de validacin del sistema

Por la presente le informamos que los productos/sistemas
DL50, DL53, DL55, DL58

incluido el software y los accesorios, han sido desarrollados, probados y verificados con xito de acuerdo con las reglas sobre ciclo de vida de producto de Mettler-Toledo GmbH, Analytical. Estas reglas se basan en la norma 9001:1994. Los puntos de control de proyecto han sido comprobados y ratificados por el grupo de Control de Proyecto (Project Supervisory Group o PSG). La comprobacin de los productos/sistemas se ha realizado antes de su entrega. Como apoyo a las exigencias GLP y de validacin, ponemos el siguiente material a disposicin de las personas autorizadas para su examen:
Imagen del producto Especificaciones Documentacin del proyecto Especificaciones del software Plan de calidad Directiva Gestin de Proyecto Plan de ensayos Datos del servicio postventa y de deseos del cliente Protocolos de revisin Cdigo fuente
Mettler-Toledo GmbH, Analytical, conservar la propiedad de todo el material y sus reproducciones y llegar a un acuerdo de confidencialidad con quienes quieran examinar este material.
Schwerzenbach, Enero 1999
Dr. Berbhard Grob General Manager Business Unit Analytical
15-6
08/2004
Modelo del ciclo de vida de un producto Ideas
Estudio del proyecto
Encargo del proyecto
Comienzo del proyecto
Fase: Conocimientos bsicos
Imagen del producto Especificaciones Plan de calidad Documentacin del proyecto Plan del proyecto Protocolo de revisin
Fase: Viabilidad
Especificaciones del software Plan de ensayos Protocolo de revisin
Fase: Verificacin Fase: Preparacin
Protocolo de revisin
Fin del proyecto
Protocolo de revisin
Utilizacin
Servicio tcnico (CRIS) Deseos del cliente
Sustitucin
08/2004
15-7
Dichiarazione di validazione del sistema

Con la presente Vi informiamo che i prodotti/sistemi
DL50, DL53, DL55, DL58

inclusi software e accessori sono stati sviluppati, controllati e validati secondo le regole tecniche relative al ciclo vita dei prodotti della Mettler-Toledo GmbH, Analytical. Queste regole si basano sulle norme ISO 9001:1994. I dettagli di controllo del progetto sono stati verificati ed approvati dall'organo di supervisione del progetto (PSG: Project Supervisory Board). I prodotti/sistemi sono stati controllati e verificati prima della fornitura. Per soddisfare le richieste di validazione e GLP i seguenti documenti sono messi a disposizione per la visione da parte di personale autorizzato:
Specifiche del prodotto Linee direttive Documentazione del progetto Specifiche del software Sistema di qualit Disposizioni per la gestione del progetto Piano dei test Dati del servizio clientela/esigenze dei clienti Rapporti di revisione Codice originale
La Mettler-Toledo GmbH, Analytical, rimarr in possesso di tutti i documenti e di tutte le loro copie e contrarr un accordo di discrezione con coloro che desiderassero visionare tali documenti.
Schwerzenbach, Gennaio 1999
Dr. Bernhard Grob General Manger Business Unit Analytical
15-8
08/2004
Modello di ciclo vita di un prodotto Idee
Studio del progetto
Realizzazione del progetto Fase: Conoscenze di base
Inizio del progetto
Specifiche del prodotto Linee direttive Sistema di qualit Documentazione del progetto Sistema del progetto Rapporto di revisione
Fase: Fattibilit
Specifiche del software Piano dei test Rapporto di revisione
Fase: Conferma Fase: Disponibilit
Rapporto di revisione
Fine del progetto
Rapporto di revisione
Utilizzazione
Servizio clientela (CRIS) Esigenze dei clienti
Sostituzione
08/2004
15-9
To protect your METTLER TOLEDO products future: METTLER TOLEDO Service assures the quality, measuring accuracy and preservation of value of all METTLER TOLEDO products for years to come. Please send for full details about our attractive terms of service. Thank you.
Printed on 100% chlorine-free paper, for the sake of our environment.
*P51709614*
Subject to technical changes and to the availability of the accessories supplied with the instruments. ME-51709614F Printed in Switzerland 0408/2.12
Mettler-Toledo GmbH 1997, 1998, 1999, 2003, 2004
Mettler-Toledo GmbH, Analytical, Sonnenbergstrasse 74, CH-8603 Schwerzenbach, Tel. ++41 1 806 77 11, Fax ++41 1 806 73 50, Internet: http://www.mt.com

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Reference handbook

Methods Method ID Standard methods User methods METTLER methods Print

Modify SETUP Standard methods

METTLER TOLEDO DL50/DL53/DL55/DL58

Samples to be analyzed Number of samples Method ID User Add 1 00001

Add New sample series

Esc Sample entry Number of samples Method ID

Table Result list Method: 00001 Sample 1 R1 = 29.26 %

METTLER TOLEDO DL50/DL53/DL55/DL58

Auxiliary functions: Overview

Sensor Measure potential Measure temperature Calibrate temperature sensors

Sample changer Change lift position Rotate turntable Dispense/rinse

Burette Rinse burette Rinse tip Dispense

Esc Change lift position Lift position

Esc Rinse burette Burette drive

Stop appears only with DL55 and DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

Auxiliary functions: Overview

Results2) Display result list Perform calculations Display measured values

Result list Method: 00001 Sample 1 R1 = 29.26 % Sample 2

Report Output unit writing report

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

Name Sensor type Sensor input

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

Name Stirrer output

METTLER TOLEDO DL50/DL53/DL55/DL58

Centronics interface: Settings for an EPSON printer

METTLER TOLEDO DL50/DL53/DL55/DL58

RS232 interface: Settings for an EPSON printer

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

Instrument type Computer Color terminal Monochrome term. Esc

Baud rate Parity

METTLER TOLEDO DL50/DL53/DL55/DL58

Data bits Stop bits Bar code

Esc Status Press <F4> to select "Defined".

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

Solvents (with sample changer only)

METTLER TOLEDO DL50/DL53/DL55/DL58

Learn titration .............................................................................................. 3-43

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58

METTLER TOLEDO DL50/DL53/DL55/DL58