Professional Documents
Culture Documents
Maintenance Manual
Spectro-FTIR Oil Analyzer
160 Ayer Road Littleton, MA 01460 U.S.A. • Tel. 978.486.0123 • Fax 978.486.0030
email: service@spectroinc.com • web page: www.spectroinc.com
Table Of Contents
1.0 INSTALLATION............................................................................................................. 1
1.1 SITE REQUIREMENTS................................................................................................. 1
1.2 SPECTRO-FTIR HARDWARE DESCRIPTION........................................................... 2
1.2.2 Internal Components of the Spectro-FTIR ...................................................................... 6
1.3 SPECTRO-FTIR HARDWARE INSTALLATION.......................................................... 7
1.3.1 Installing the Spectro-FTIR and the Base Cabinet............................................................ 7
1.3.2 Connecting the Spectro-FTIR to a Computer................................................................... 9
1.3.2.1 Stand-alone Configuration................................................................................................ 9
1.3.2.2 Spectro-FTIR and PC on a Network............................................................................... 10
1.3.2.3 Spectro-FTIR on a Network Computer.......................................................................... 10
1.4 SPECTRO-FTIR PLUMBING INSTALLATION......................................................... 11
1.4.1 Flow-Through Cell Plumbing......................................................................................... 12
1.4.2 Wedge Cell Plumbing..................................................................................................... 13
1.4.3 Manual Operation.......................................................................................................... 14
1.4.4 Automatic Operation...................................................................................................... 15
WARNING!!!
High Voltages are Present During the Operation of the
Spectro-FTIR !
Definitions
WARNING!!!
An operating procedure or practice that may cause injury if not carefully observed or
followed.
CAUTION!!!
An operating procedure or practice that may cause damage to the Spectro-FTIR if not
carefully observed or followed
NOTE!!!
An operating procedure or practice that is essential to emphasize
Revision History
to the arrival of the Spectro-FTIR, or it can be Disk, (2) RJ-45 Ethernet ports. With an
performed at the same time. English operating system of either; Windows
XP or Windows 2000.
The Spectro-FTIR is a bench-top instrument and • Recommended Solvent: Pentane, see Section
can be placed on a laboratory counter or a sepa- 3.10.
rate table. The comfort of the operator must also • Waste Container (for oil & solvent): The
be considered if samples are to be analyzed for waste container must be corrosive resistant,
long periods of time. The physical requirements non-pressurized and located below the FTIR.
for the laboratory are as follows: • Purged Gas Option (available for humid
environments): Dried compressed air or
• Location: The Spectro-FTIR must be placed nitrogen regulated at 6-9 Psi.
on a level surface.
• It is always good practice to place instruments Important Consideration:
away from windows or doors where direct To provide for good data quality and a long spec-
sunlight or drafts could cause temperature trometer service life, ensure that the following site
fluctuations. requirements are met:
• General Space Requirements: Dimensions
are: 66.5 x 43.4 x 28.1 cm (26 x 17 x 11 • Do not install the spectrometer near sources
inches at a weight of 37kg (82 lbs.). of potential inductive electrical interference
• Operating Temperature: Minimum to (e.g. pumps, switching motors, microwave
maximum 18-35˚C (64-95˚F). Temperature ovens etc.), sources of high energy pulses, and
fluctuations of more than 1 ˚C shift during a sources that might cause magnetic or radio
sample measurement and 2˚C shift between frequency interference.
background measurements are not recom- • Do not place devices such as large electric
mended for optimum accuracy and repeat- motors, heaters, welding equipment, radio
ability. transmitting equipment, units emitting
• Humidity: For optimum performance life the pulsed NMRs, or high powered lasers in close
operational relative (non-condensing) humid- vicinity to the spectrometer. These devices
ity should be ≤ 80%. An optional purge kit can interfere with the spectrometer and cause
is available for high humidity environments. spectrometer malfunction. Ensure that these
types of devices are not connected to the
IMPORTANT NOTE: The Spectro-FTIR must same electrical circuit as the spectrometer.
be placed as far away as possible from any sources • If there are any problems concerning main
of vibration within the confines of the laboratory. power supply (e.g. brownouts, power surges,
Due to the sensitive nature of the instrument, the frequent thunderstorms), take precautions to
unit should isolated from any source of vibration ensure an uninterruptible power supply.
during analysis (Spectroil M, ventilation hoods,
motors elevators, air conditioners, etc. 1.2 SPECTRO-FTIR HARDWARE
DESCRIPTION
The resources and facilities external to the Spec-
tro-FTIR that are required for operation are: This chapter identifies the main components of
Minimal Electrical Requirements: 100-240 VAC the Spectro-FTIR. The user should become fa-
±10%, 50-60 Hz. miliar with the terminology in order to make it
easier to understand the operational and mainte-
• Computer (when not supplied by Spectro nance functions of the instrument as described in
Inc): Minimum requirements are Pentium this manual.
2 @800 MHz, 128MB RAM, 10GB Hard
Source/Laser
Compartment
Electronic Interferometer
Compartment Compartment
Detector AutoSampler
Compartment
Sample
Compartment
Figure 1.2-2, Sample Compartment Doors Figure 1.2-3, Status Indicator Display
MPE 1 PORT
CAN BUS
CONNECTOR
SR LED W
and
MAIN POWER
SG LED
SWITCH
RES BUTTON
FUSE BLOCK
TX LED
and
RX LED
PRIMARY POWER
ETEHRNET PORT
RECEPTACLE
Figure 1.2-4, Spectro-FTIR REar View
IR Source
Detector
Beam
Splitter
Desiccant Desiccant
Cartridge Cartridge
Figure 1.2-, Internal Components of the Spectro-FTIR
1 1 1 1
2 2 2 2
3 3 3 3
4 4 4 4
5 5 5 5
6 6 6 6
peristaltic pump by moving its handle from the 1.4.2 Wedge Cell Plumbing
left side to the right hand side when you are Locate the parts listed below to assemble and in-
ready to analyze samples. stall the wedge cell sample introduction system.
NOTE: It is good practice to open the pump to • P/N FT2042 Wedge Cell
take pressure off the tubing when the Spectro-FT- • P/N FT2046 Valve 25 PSI Wedge Cell As-
IR is not in use. This extends the life of the tube sembly (Pressure Relief Valve)
and avoids tube deformation. • P/N FT2032 Input Tubing Assembly
• P/N FT2033 Drain Tubing Assembly
8. Plug the pump power connector into the • P/N ASP118 Carboy Assembly (Waste Con-
appropriate power outlet (110 or 220 VAC). tainer)
9. Connect and RS 232 cable from the RS • For automatic operation, additional tubing
232 Input connector on the back of the sample and a second peristaltic pump are supplied.
introduction pump, Figure 1.4-7, to the
COM 1 port on the PC. A completed sample introduction system for the
flow-through cell is shown in Figure 1.4-1b. Fol-
For manual operation and sample analysis, pro- low the steps below to assemble the sample this
ceed with Section 1.4.3 introduction system.
For automatic operation with an AutoSampler 1. Locate the Wedge Cell, P/N FT2042 and
proceed with Section 1.4.4. install it by sliding it into the right hand side
of standard 2x3 inch cell holder. The cell
should easily slide in from the top.
Wedge Cell
FT2042
NOTE: It may be easier to install the tubing 232 Input connector on the back of the sample
with the cell holder removed. To remove the cell introduction pump, Figure 1.4-7, to the
holder, push the lever on the floor of the compart- COM 1 port on the PC.
ment away from you and lift out the holder.
For manual operation and sample analysis, pro-
2. Locate and unpack the Wedge Cell As- ceed with Section 1.4.3
sembly (Pressure Relief Valve) Assembly P/N
FT2046. Install it by pressing it into the clip For automatic operation with an AutoSampler
on the floor of the sampling compartment. proceed with Section 1.4.4.
3. Connect the Drain Tubing Assembly P/N
FT2033 to the output connection of the Valve 1.4.3 Manual Operation
Assembly using the ½ turn Leuer-Lock con- 1. Connect the free end of the Input Tubing
nector. Assembly to the Sipper Tube Assembly, Figure
1.4-2.
WARNING: Avoid over torquing the fittings to 2. Connect the free end of the Drain Tubing
avoid strpping them. Assembly to the Waste Container ASP118.
Additional tubing may be required depending
4. Connect the Input Tubing Assembly P/N on the proximity of the Waste Container to the
FT2032 to the input connection of the Valve Spectro-FTIR.
Assembly using the ½ turn Leuer-Lock con-
nector. NOTE: The ideal location for the waste con-
5. Connect the wedge cell input tubing to the tainer is on the floor below the Spectro-FTIR. In
first stage of the Valve Assembly P/N FT2046 all instances, it must be located lower than the
input using the ½ turn Leuer-Lock connector.
6. Connect the wedge cell output tubing to
the second stage of the Valve Assembly P/N
FT2046 input using the ½ turn Leuer-Lock
connector.
7. Place the peristaltic pump on the top right
front right corner of the Spectro-FTIR. In-
stall the pump head with the two provided
screws. Open the peristaltic pump by moving
its handle from the left side to the right hand
side. Place the peristaltic pump tubing (black
section) into the peristaltic pump. Close the
peristaltic pump by moving its handle from the
left side to the right hand side when you are
ready to analyze samples.
Spectro-FTIR so that waste oil sample and sol- Tubing will have to be cut to length depending
vent flow to the Waste Container due to gravity. on the location of the components. Additional
pieces of tubing will be required to connect to
3. This completes the manual sample plumb- the Waste Container, one-way valve and to the
ing setup of the Spectro-FTIR. solvent reservoir on the AutoSampler.
3. Connect a piece of tubing between the “T”
1.4.4 Automatic Operation connector and the waste container.
1. A filter is installed between the sample 4. Cut tubing to size and install the one-way
introduction peristaltic pump and the AutoS- valve into the tubing going to the AutoSampler
ampler sipper tube, Figure 1.4-3. Connect a solvent reservoir. Note that the fluid flow is in
short piece of tubing to the input side of the the direction as shown on Figure 1.4-4. This
filter and a longer piece between the output keeps the oil sample from flowing into the
of the filter and the AutoSampler sipper tube. solvent reservoir on the AutoSampler.
2. Connect the free end of the Drain Tubing 5. Connect the other end of the tubing from
Assembly to the ‘T” connector, Figure 1.4-4. the one-way valve to the top connection on the
solvent reservoir, Figure 1.4-5.
6. Place the second peristaltic pump used for
pumping solvent to the AutoSampler beneath
the first pump as shown in Figure 1.4-6.
7. Open the solvent peristaltic pump by mov-
ing its handle from the left side to the right
hand side. Place the peristaltic pump tub-
ing (black section) into the peristaltic pump.
Close the peristaltic pump by moving its
Solvent Reservoir Waste Output Connection
To Solvent Reservoir
on AutoSampler
Solvent Flow
One-Way Valve
Drain Tubing
from Sample
‘T” Connector
Compartment
Figure 1.4-4, ‘T” Connection and One-Way Figure 1.4-5, Waste Tubing Connection to the
Valve Solvent Reservoir
Initial Software and the computer. The software and settings will
be pre-installed at Spectro Inc. when the comput-
er is supplied along with the Spectro-FTIR. The
2.2 DISABLE VIRUS AND FIREWALL Use the following procedure for configuring Sy-
SOFTWARE mantec Norton AntiVirus Corporate Edition on
a workstation to exclude the WIBUKEY, WIBU-
There have been reports of virus checking software SYSTEMS, and OPUS program directories from
adversely affecting performance and sometimes continuous virus scanning:
even causing errors in the Spectro-FTIR software.
It has been established that virus checking soft- 1. Select Start | Programs | Symantec Client
ware can slow down performance in certain situ- Security | Symantec AntiVirus Client.
ations. We recommend that virus checking soft- 2. Select Configure | File System Realtime
ware be configured in such a way as to minimize Protection.
the effects of virus scanner interference. 3. In the Options section, select the Exclude
selected files and folders check box.
Some virus checking software systems have the 4. Click Exclusions.
ability to virus scan continuously in the back- 5. Select the Check file for exclusion before
ground. This type of configuration can slow scanning check box.
down the performance of software, particularly in 6. Click Files/Folders.
a network environment. 7. Browse to the WIBUKEY software pro-
gram directory (for example, C:\Program Files\
The Spectro-FTIR software is data processing soft- WIBUKEY) and select the corresponding
ware that is very disk I/O intensive. The software check box.
is constantly opening files, writing to them and 8. Browse to the WIBU-SYSTEMS software
closing them. The software also makes frequent program directory (for example, C:\Program
use of temporary files. For these reasons, the po- Files\ WIBU-SYSTEMS) and select the corre-
tential performance decrease caused by continu- sponding check box.
ous virus scanning may be more apparent in our 9. Browse to the OPUS software program
software than in some other types of applications. directory (for example, C:\Program Files\
OPUS) and select the corresponding check
The Spectro-FTIR software uses a network in- box.
terface for communication. This communication 10. Click OK three times to save your changes.
cannot be run through a firewall protection sys- 11. Click Exit to exit Symantec AntiVirus Cor-
tem. The delays caused by the firewall can severe- porate Edition.
ly interrupt the analysis process and cause system
errors. The network adapter that communicates NOTE: Additional instructions regarding how
with the FTIR should be disabled in any firewall to exclude files and directories can be found on
software and in Windows XP Firewall. Symantec’s Knowledge Base on the Internet.
1. Open the On-Access Scan Properties dia- 2.2.2.2 Disable Windows Firewall in Windows
log box, then select one of the following icons XP SP2
in the left-hand pane: A firewall is designed to help protect your com-
• Default Processes puter from attack by malicious users or by mali-
• Low-Risk Processes cious software. Malicious software includes virus-
• High-Risk Processes es that use unsolicited incoming network traffic
2. On the Detection tab, click Exclusions in to attack your computer. Before you disable your
the What Not to Scan area. This will open the firewall, you must disconnect your computer
3. Set Exclusions dialog box. from all networks, including the Internet. To do
The Set Exclusions dialog box lets you add this, follow these steps:
or edit files, folders, or drives. Windows File
Protection is listed by default. 1. Click Start, click Run, type Firewall.cpl,
• To add an item to the list of exclusions, open and then click OK.
the Add Exclusion Items dialog box by click- 2. On the General tab, click Off (not recom-
ing Add. mended), and then click OK.
• To edit an item in the list, you can double-
click it or select it and then click Edit.
Figure 2.3-7, Availabe Features Selection 12. When the installation is complete, the
Screen installation protocol can be printed by select-
selected, click the boxes to select the following ing “Print”, or by selecting “Accept”. A link to
files: the OPUS software will be placed on the PC’s
OPUS desktop
Basic Features
OPUS Lab 2.3.2 Registering OPUS
Standard
Documentation
OnLine Help
Extended Demodata
QUANT
QUANT Tutorial
TENSOR
TENSOR 27
VERTEX
VERTEX 80
Click on the “Next” button when the above
selections have been made.
9. On the next screen, Figure 2.3-8, select
“Tensor 27” from the window and click on Figure 2.3-9, Import from Previous Installation
“Next”. Screen
Figure 2.3-12, OPUS Login Screen Figure 2.3-15, Registration Dialog Screen
Figure 2.3-25, Optic Setup and Service Screen Figure 2.3-26, Select User Settings
Figure 2.3-27, Deselect Work in GLP Mode Figure 2.4-1, Spectro Oil Analysis Install Screen
Figure 2.6-6, LWN Calibration Reference Values Figure 2.6-8, PQ Test Protocol
Test Setup” tab and the OVP Test Setup can take about 5 to 10 minutes to complete.
main screen shown in figure 2.6-7 will appear. When the reference spectra have been gath-
Confirm that the Run PQ and Run OQ check ered, a green “√” mark appears on the Measure
boxes are selected. The PQ test should be Reference Spectra button to signify the process
default to “12” and “Hours” while the OQ test has been completed, Figure 2.6-9. Click on
should default to “12” “Months”. Click on the the “OK” button to proceed.
“Setup” button to the right of the PQ test to
proceed. 11. The OVP Test Setup main screen reappears
with a green “√” mark to the right of the PQ
9. The screen shown in Figure 2.6-8 will test to signify that it has been setup successful-
appear for the PQ Test Protocol. The default ly Figure 2.6-10. The red caution sign on the
configuration will already have all the op- OQ Setup button signifies that this second test
tion boxes selected, if not select them. Click needs to be performed. Click on the “Setup”
on “Measure Reference Spectra” button to button to the right of the OQ test to proceed.
proceed. Note that the Caution symbol on
the button signifies that user intervention is 12. The screen shown in Figure 2.6-11 will
required. appear for the OQ Test Protocol. The default
configuration will already have all the option
10. The Spectro-FTIR is now gathering the boxes selected, if not select them. Click on
reference spectra for the PQ test. This test “OK” button to proceed.
Figure 2.6-7, OVP Test Setup Main Screen Figure 2.6-9, Successful Completion of
reference Spectra Test
Analysis FTIR.
3.1 INTRODUCTION
ment.
3.3 MANUAL SAMPLE MEASUREMENT
Figure 3.1-8, Performing Cell Cleanliness The figure shows the main operator screen con-
Screen
figured for manual operation. The left side of
the screen contains a field that will display the
result of each analysis to the operator. When
the program is opened, the Analytical Results
field will be empty. The results are concatenat-
ed (consecutively linked) unless the “Clear Re-
sults List Before Each Measurement” Option
is selected in the Program Settings, Options 3
Tab, Section 3.7.4.
You are now ready to perform a sample measure- Figure 3.3-1, Main Analysis Screen
Figure 3.3-2, Subtraction Spectra Folder Figure 3.3-4, Please Clean Cell screen
12. If the “Cell Cleanliness Check” option If another analysis is performed at this time, the
has been enabled in Program Options, Op- results are concatenated (consecutively linked)
tions 1 tab, Section 3.7.2., then the wizard will unless the “Clear Results List Before Each Mea-
perform a cleanliness check of the cell, Figure surement” Option is selected in the Program Set-
3.3-5. If the test fails you will be instructed to tings, Option 3 Tab, Section 3.7.
clean the cell again. The test must pass before
a sample measurement can be performed. 16. Select the “Clear Results List” button to
13. The wizard will instruct you to pump oil
into the sample cell, Figure 3.3-6 when the cell
cleanliness test has passed or is skipped because
it is disabled.
14. Pump the oil into the sample cell, and
then press the “Next” button by clicking on it
to continue. The wizard informs you that a
sample measurement is in progress, Figure 3.3-
7.
There are four columns in the assignment grid Each sample measurement consists of the steps
that must be filled in for each sample in the rack. below and summarized in Figure 3.4-4.
• Analyze: Check this field to instruct the • The sample cell is tested for the presence
program to measure the sample at this posi- of oil or solvent. If found, the cell is auto-
tion on the rack. The position number and matically cleaned and dried. (Only tested
sample cell color turn blue. if Cleanliness Check is enabled in Program
• Sample ID: This is a unique sample ID num- Options, Section 3.7.)
ber for the sample located at this position on • The probe is moved to the next enabled
the sample rack. This is a required field. sample position and inserted into the sample
• Analysis Method: Left-click on this field to bottle.
display a drop-down list of analysis methods. • Oil is pumped into the cell for the Pump
Select one of the methods to be applied to Time specified in Program Options, Section
the analysis of the sample located at this rack 3.7.
Analyze Button
Passed
Passed
Sample
Probe is Removed from Sample
Measurement &
Bottle & Allowed to Drip
Analysis
• The sample cell is tested for the presence of and saved in the designated database.
oil. If oil is not detected, the oil is pumped Any warnings or errors are reported in the line
and the cell is tested again. If after a few tries following the procedure that produced the warn-
the cell still does not contain oil the operator ing or error.
is queried to determine if pumping should
continue. The rack graphic displays different colors depend-
• The probe is removed from the sample bottle ing upon the state of a sample position.
and excess oil is allowed to drip.
• The sample measurement and analysis is
A white cell indicates an unused sample
performed.
position on the sample rack.
• The probe is moved to the rinse station of the
AutoSampler and a rinse cycle is performed.
Solvent is pumped through the line and A blue cell indicates a sample position that
sample cell. has been assigned a sample bottle.
• The probe is removed from the rinse solvent
and air is pumped through the sample cell.
• The sample cell is tested for the presence of A yellow cell indicates the currently se-
oil. If oil is detected, additional rinsing is lected sample position.
performed. If solvent is detected, additional
air pumping is performed. At the completion of the cell analysis, if all
procedures in the analysis method were within
As each sample position is measured, the results specifications, the cell position is displayed in
are displayed to the operator in the Analysis Re- green.
sults section, Figure 3.4-5.
When a database is selected in Program Setup, If an error occurred during the analysis,
Option 3 tab, Section 3.7.4, the results are stored the cell position is displayed in red.
(add blue)
Figure 3.5-3, Locate File to Reprocess Figure 3.6-1, Main Drop-down Menu
Figure 3.6-2, Report Seletion Dialog To view the tabs, select “Program Options” from
the “Setup” menu, Figure 3.7-1.
A.
B.
C.
The spectra generated during the cell cleanliness Upon completion of the cell calibration pro-
test can be saved and archived. However, the de- cedure, the program computes the Cell Path
Length, and the option to enable the Cell Fring-
1 May, 2009 / v.1.2
Spectro-FTIR User Operation & Maintenance Manual | 51
A.
B.
This section of the Options 2 tab defines the files shown in the figure.
and folders used by the Spectro Oil Analysis Soft-
ware. Default values are included. 3.7.3 Options Tab 3
The Program Options, Option 3 tab is shown in
Analysis Methods Database File: Figure 3.7-4. The available settings and corre-
This is the file containing the definitions for the sponding fields are explained in this section.
different oil analysis methods. If you move the
file to a different location you should select it us- A. Setup Password
ing the open folder button to the right of the field. Select this button to create/edit/delete a password
to protect the Setup menu options. When a pass-
Experiment Method File: word has been set, the user must enter the correct
This is the parameter file used by the OPUS pro- password before access is granted to any of the
gram to perform the sample and background options on the Setup menu.
measurements. Any experiment method file
(xpm) can be used as long as it is compatible with Click on “Set Password” and a dialog window
the analysis method(s) being used. One file will appears that allows you to edit or delete the pass-
be used for all measurements. word. Press the “Enter” key when changes have
been made.
Sample Spectra Root Path:
This is the root folder where all spectra measured B. Options
by the program will be stored. This section contains general program options
that did not fit into a particular category.
The Store Results in Database is disabled by de-
fault, however, it is good practice to activate it to By default the program is in manual operation
archive analytical results for future reference. It is mode and fuel pumping and cleaning must be
also not possible to review or print reports unless performed manually. Select the Automatic Mea-
the option is enabled. When enabled, all results surement Mode option to enable the use of the
from analyses are stored in a Microsoft Access da- AutoSampler and pump under computer control
tabase. The filename and path can be specified in to measure a rack of samples automatically. Refer
the field below the option. to Automatic Operation, Section 3.4, for more
information.
B. Analysis Results File
When selected, the Store Analysis Results in Enable Perform Hardware Diagnostics option to
CSV file option stores the results of each measure- perform hardware diagnostics on the spectrom-
ment in a comma-delimited text file. The results eter prior to each measurement cycle. The field
can then be imported into a spreadsheet or other to the right of the checkbox contains the URL
program such as the LabTrak Oil Analysis Infor- for the spectrometer. The default URL is entered,
mation Management System. however if you have changed your spectrometer
settings you need to update this field.
The field below the option checkbox specifies the
filename and path of the file. A new background measurement is required each
time the program is started. When selected, the
The remaining checkboxes are used to specify Force New Background option makes it manda-
what information is stored in the file. These are tory to perform a new background measurement
in the order (left to right, top to bottom) that after a specified period of program operation.
they will appear in the file. Typical selections are This is useful if the program is never shutdown
during day-to-day usage. The field to the right
A.
B.
The Clear Results List Before Each Measure- A. Auto Sampler Settings
ment option clears the main screen list of analy-
sis results between each measurement. When AutoSampler Driver:
disabled the results are appended until the user In order to use the AutoSampler option, driver
for the AutoSampler accessory must be selected.
A.
B.
The COM Port is the serial port number that the Probe Depth is the distance the probe tip will de-
cable from the AutoSampler is attached to the scend into the sample bottle to perform a sample
computer. A typical configuration when per- measurement, and to clean the probe tip. A typi-
formed at Spectro Inc. will have the AutoSampler cal setting for the probe depth is 130 to 135 mm.
RINSE: Press this button to initiate a rinse Air Time is the amount of time the pump will
cycle. The probe is returned to the start spend pumping air after rinsing the line with
position and a rinse cycle is initiated. (Note: solvent. If solvent is still detected in the line,
This option does not use the “Use AUX1 for the air time is repeated.
Solvent Pump” option in the Sample Pump
Settings section.) Oil Pump Time is time after oil is detected in
the cell. If no oil is detected after this time pe-
PUMP ON: Pressingthis button engages the riod elapses, the pump will continue to pump
AutoSampler onboard peristaltic pump. oil until the system detects the presence of oil
in the sample cell.
PUMP OFF: Pressing this button disengages the
AutoSampler onboard peristaltic pump. After the sample measurement is complete, the
system will pump air to empty the tubing be-
MOVE: This button moves the probe to the fore solvent is pumped. The Hose Drain Time
X, Y, and Z coordinates given in millimeters field sets the amount of time the air will pump
in the three fields. Type values in the fields before solvent is pumped.
and press the “MOVE” button. If you enter
a value outside of the range of the probe, the The Use AUX1 for Solvent Pump option is
probe will not move. used if you are connecting another MasterFlex
pump (i.e. MasterFlex Model # 77521-40) to
B. Sample Pump Settings the AUX1 connection on the rear of the pump.
In order to use the sample pump with the AutoS- This will be used to power the manual pump as
ampler, the correct Pump Driver must be selected. the solvent pump in lieu of using the onboard
The default driver included with the software is AutoSampler pump.
for the MasterFlex 7550 Computerized Pump.
Select the open folder button to the right of the The remaining controls in this section are used to
Pump Driver field by clicking on it to open a file test the operation of the pump.
dialog. Select the file “Masterflex.dll”. If this is
a legitimate driver the name of the driver will ap- INITIALIZE: Communications with the Mas-
pear in the text field. (i.e. “MasterFlex L/S Pump”) terFlex pump have to be initialized prior to
sending the pump commands. The LED
AutoSampler Parameters: display on the pump will display “P01” when
There are five parameters for the Sample Pump. the pump has been initialized. After selecting
Default values are provided. this button, a dialog will appear informing you
of the status of the pump. passed through the cell using the normal peristal-
tic pump in the manual mode or automatically
PUMP STATUS: Press this button to view a dia- with the auto sampler.
log that shows the current status of the pump.
3.8.2 Basic IR Subtraction Theory
PUMP ON: This button turns on the pump FTIR subtraction enables oil properties to be re-
using the speed value set in the “Pump Speed” ported in quantifiable units such as % concentra-
field. tion, this makes diagnosis easier to understand,
and end-users and customers often like to know
PUMP OFF: This button turns off the pump. results in units they can comprehend. In IR
subtraction, a generic calibration curve for each
CONTROL: These controls toggle the pump property is performed and stored in the oil analy-
between Local (manual) and Remote (com- sis software. It is assumed that the absorbance
puter) control. response for each property will be the same when
present in different oil types. However, different
3.8 ENGINE OIL PROPERTY oil types will often have a different zero baseline
CALIBRATION PROCEDURE response for each individual property. Subtract-
ing the fresh oil from the used oil of the same
3.8.1 Introduction base, can eliminate this zero offset. The resulting
This procedure outlines how to calibrate the Spec- subtracted absorbance is equal to the amount of
tro-FTIR spectrometer using spectral subtraction the property itself and it can then be referenced to
so that Fuel, Glycol, and Water can be reported in just the slope of the calibration curve.
quantifiable units.
Important Fact!
It is assumed that the operator has setup the Spec- IR subtraction is a very useful way to have a quan-
trometer for oil analysis and is familiar with run- titative calibration that can serve a host of differ-
ning samples using the Spectro Oil Analysis soft- ent oil types, but it does have one big disadvan-
ware. The relevant fringing corrections need to tage - you must have the same oil matrix in both
have been applied so clean “fringe free” spectrums the used sample and the subtracted fresh oil. If
can be gathered and that the cell path length has not, you will create an artificial offset based on
been calculated Sections 3.1.2 and 3.7.1. the absorbance response in the blank oil which
will cause gross inaccuracies in the final result.
NOTE: More accurate limits of detection can When an oil sample is received for analysis with
be achieved if an optional wedged cell is used to an FTIR spectrometer and the results are required
perform these calibrations. The wedged cell will in % concentration, it’s imperative that the user
eliminate much of the noise at zero levels caused know exactly what the matrix of the fresh oil sam-
by fringing. ple is, and also that a replicated scan of the base
oil is stored on your FTIR. Unfortunately, over
The calibrations for water and glycol contamina- time, used oil in an engine is frequently topped
tion must be undertaken immediately after the off by a mechanic with a multitude of different
standards are shaken so that the water remains in a brands, or even worse, a new and different brand
homogenized state. It is therefore recommended was used without the knowledge of the laboratory
that all oil property calibrations be done manually and the FTIR operator. This will result in many
using lure lock syringes. The oil can be flushed false positives, or even worse a false negative. The
from the cell using a pump on the exit port and response for fuel and glycol is very susceptible to
pentane solvent on the input side. If lure lock sy- these kinds of problems because the response of
ringes are not available, then the standards can be the property is so small in relation to the peak
already present in the fresh oil itself. the sample and add the contaminant until
the weight gathered from the spreadsheet is
3.8.3 Step-by-Step Calibration Procedure reached to within 0.01 grams.
In order to create IR subtraction calibrations, a. Fuel – 0, 2, 5, 8, 10 %
fresh oil types that you plan to analyze will be b. Water – 0, 0.1 , 0.25 , 0.5, 0.75%
required along with quantities of fuel, water and c. Glycol - 0, 0.1 , 0.2 , 0.3 , 0.5 %
glycol which will be mixed in exact amounts with
the fresh oils. The procedure also requires the use Note: It is very important that the diesel fuel be
of a spreadsheet called “ftir_subtraction_tools.xls” weathered to simulate the fuel contaminate in a
and a copy of Microsoft Excel. The “ftir_subtrac- crankcase. Heat the fuel to 107 degrees C then
tion_tools.xls” spreadsheet can be downloaded hold it at this temperature for 30 minutes. This
from the Spectro Inc. web site by using the part- represents a loss of around 5% by weight.
ner Login feature and selecting “Documented
Procedures” after logging in. Note: Glycol standards should be made using
a 50:50 mixture of glycol based antifreeze and
NOTE: This procedure assumes that the user has water.
operating experience with the Spectro-FTIR and
a detailed knowledge of the Spectro-FTIR Oil 6. Make sure to thoroughly shake each of the
Analysis Software. Experience in mixing fluids samples to ensure that the contaminant prop-
to create standards by weight is also essential. If erty gets into complete suspension in the fluid.
you are unsure about any of this, contact some- Extra care needs to be taken with the water and
one in your organization who has knowledge in glycol standards because these properties are
this area or contact your local representative for difficult to homogenize. Placing these samples
assistance. in an ultrasonic bath will help homogenize the
water and the glycol.
Follow the step-by-step procedure below to create 7. Ensure that the cell is clean and collect a
the required calibration curves. fresh background.
8. Do the following calibrations in this order:
1. Gather all the fresh oil types from engine Water, Fuel, Glycol – start with zero and work
oils that you plan to run on the FTIR. up to the highest concentration. Ensure to
2. Store a scan of each fresh oil type on the shake the water and Glycol standards thor-
FTIR using the standard Direct Trending oughly before injecting.
Method. 9. Use the corresponding individual prop-
3. Rename the spectral files with the oil type erty methods (e.g. Spectral subtraction diesel
and put them in the computer’s subtraction_ calibration) on the Main Oil Analysis screen
spectra folder in the spectro oil analysis folder. to analyze each calibration set. Enter at least 4
ml of oil into the top of the cell using lurelock
CAUTION: Ensure that the .0001 extension is syringes if possible. Reconnect the hose and
not removed, (example: citgo_10w40.001). flush the cell and check for cleanliness before
entering the next sample. Make note of the re-
4. Open the ftir_subtraction.xls tools work sulting absorbance value in the Analytical Re-
sheet. sults screen and enter it in the corresponding
5. Create the following five standards by % box on the worksheet. As you enter more
weight for each property making sure to tare values a linear calibration curve will begin to
the scale with the empty bottle for each cali- form in the graph box.
bration standard. After adding the oil, and 10. After each property calibration set is com-
recording the weight on the spreadsheet, tare plete, flush out the oil thoroughly with pen-
(Original Equipment Manufacturers) may vary oil lowers overall viscosity, but continuous water
somewhat from these values. Also, the ever- contamination eventually causes oxidation and
changing formulation of high performance addi- viscosity increase.
tive packages in the highly competitive lubricant
market may also have some effect on the values 3.9.2.1 Water in Extreme Pressure (EP)
stated in this guide. Guidelines are provided for: Additive Fluids
These limits apply to mineral / synthetic gear lu-
• Water Contamination, Section 3.9.2 bricants and hydraulics with EP additive pack-
• Soot Contamination, Section 3.9.3 ages.
• Glycol (antifreeze) Contamination, Section
3.9.4 Normal and Abnormal Limits
• Fuel Contamination, Section 3.9.5 • Synthetic Hydraulic Ground Equipment:
• Degradation based on Nitration, Section Normal <200 ppm, Alert at 1000ppm
3.9.6 • Synthetic Hydraulic Air Equipment: Normal
• Degradation based on Oxidation, Section <20ppm, Alert at 350ppm
3.9.7
• Degradation based on Sulfation, Section NOTE: This is only used for EP additive fluids,
3.9.8 it is not to be used for synthetic turbine oils or
• Lubricant Breakdown, Section 3.9.9 petroleum crankcase oils
• Antiwear Reading (ZDDP) Additive, Section
3.9.10 3.9.2.2 Water in Synthetic Turbine Lubricants
These limits apply to water measurement in Syn-
Reference ASTM E 2412 & JOAP thetic (polyol ester) lubricants used in high per-
formance jet engines. Common lubricants in this
3.9.2 Water Contamination class are Mil-PRF-7808 and Mil-PRF-23699.
The presence of water needs to be monitored be-
cause it can cause costly breakdowns due to inter- Normal and Abnormal Limits
nal corrosion and lubricant degradation. Through • Synthetic Turbine Lubes: Normal 0-30 abs
periodic oil analysis with instruments such as the units, Alert at 45 units (approx 1000ppm)
Spectro-FTIR, water can be detected giving the
user the opportunity to react accordingly and 3.9.3 Soot Contamination
make adjustments to rectify the problem before it Soot in used oil is an indication of the amount
gets out of hand. of insoluble carbon suspended in the lubricant.
Soot particles are extremely small, on the order of
Water contamination in lubricating oils or hy- 0.01 µm. They are carbon left over from incom-
draulic fluids comes from two primary sources, plete combustion of the hydrocarbon molecules
leaks in the system or condensation of moisture in diesel fuel. Dispersant additives are present in
in the air space. Large amounts of free water will diesel engine lubricants to prevent soot particles
separate and settle to the base of the lubricating from agglomerating and plugging oil filters that
system reservoir. Most lubricants and hydraulic are meant to capture hard, abrasive particles. Soot
fluids will dissolve small amounts of water, how- by itself is not harmful to diesel engine operation,
ever, the presence of water over approximately 1% but excessive levels of fuel soot in an oil sample are
is detrimental to the formation of an oil film and typically due to an incorrect air/fuel ration due to
thus promotes metal-to-metal contact of rotat- restricted airflow in a filter that results in an in-
ing equipment resulting in abnormal wear. The sufficient air supply to the combustion chamber.
presence of water accelerates oil oxidation and High levels of fuel soot when not corrected will
subsequent oil thickening. At first, water in the lead to oil thickening, the formation of deposits,
An analysis for water by itself may not be reliable Normal and Abnormal Limits
enough since engine temperatures will vaporize • Diesel Engines: Normal 220-230 abs units
low levels of water. Infrared spectroscopy with (E2412 method using multiplier), Alert at
the Spectro-FTIR can also be applied to detect >255 abs units.
antifreeze contamination.
3.9.5.2 Gasoline Fuel Contamination
These limits apply to monitoring the presence of Limit guidelines for gasoline contamination are
Ethylene Glycol (Antifreeze) in crankcase lubri- not available due to the very small number of gas-
cants. oline engines enrolled in condition monitoring
programs, therefore, abnormal and normal values
Normal and Abnormal Limits have not been set. In most cases, using subtrac-
• Diesel Engines: Normal 0-1 abs units , Alert tion will produce a value of close to zero.
at >3 abs units
3.9.6 Degradation based on Nitration
NOTE: As ethylene glycol is approximately a Nitration is similar to oxidation. Nitration results
50:50 dilution with water, a valid glycol alarm from the reaction of oil components with nitro-
should also produce a high water reading for the gen oxides that are produced from the oxidation
mineral water band. A strong glycol reading with of atmospheric nitrogen during the combustion
a low water reading may indicate contamination process. In addition to causing oil thickening, ni-
of a water free silicone fluid. This reading is not tration products are the major cause of the build-
up of varnish or lacquer on engine parts.
NOTE: Sulfation measurement not applicable in 3.9.10 Antiwear Reading (ZDDP) Additives
synthetic based lubes. The most common additive in many different
classes of lubricants, from engine oils to antiwear
3.9.9 Lubricant Breakdown hydraulic fluids is ZDDP. The initial concentra-
Lubricant antioxidants are additives that enhance tion of ZDDP in any oil can be determined by
a lubricant’s thermal stability, improve perfor- measuring zinc and phosphorus levels using and
mance and reduce sludge formation, thus extend- elemental analysis technique such as atomic emis-
ing the useful life of lubricants in virtually any sion spectroscopy. However, emission spectros-
application. They reduce thickening and inhibit copy cannot not be used to monitor in-service
acid formation in a variety of applications, in- ZDDP additive depletion. In-service ZDDP
cluding engine oils, automatic transmission flu- depletion is best measured by molecular spectros-
ids, industrial oils, as well as compressor oil and copy such as FTIR.
gear and hydraulic oils. ASTM E 2412 refers to
two types of lubricant breakdown, Breakdown I These limits apply to monitoring Phosphate an-
and Breakdown II. tiwear compound levels in mineral and synthetic
lubricants.
3.9.9.1 Breakdown I Synthetic Lubricants
These limits apply monitoring the breakdown of Normal and Abnormal Limits
Synthetic (Polyol Ester) Jet Engine Turbine Lu- • Diesel Engines: Normal 8-12 abs units, Alert
bricants. at <5 abs units
• Synthetic Turbines: Normal 95-110 abs
Normal and Abnormal Limits units, Alert at <80 abs units
• Normal <30 for Synthetic turbine lubri-
cants, Alert at 45 Units (approx TAN 1.0 3.10 SOLVENT REQUIREMENTS FOR
mgKOH/g) THE SPECTRO-FTIR
NOTE: The limits and methods do not apply to There are several criteria for choosing a rinse sol-
mineral based oils, result may increase due to vent for the Spectro FT-IR Oil Analyzer. Among
increase in water levels. these are:
- The solvent must be a good oil solvent to dis-
3.9.9.2 Breakdown II Synthetic and Water in solve whatever oil is left in the cell and tubing
Petroleum Lubricants of the flow path.
These limits apply to additional monitoring of - The solvent needs to evaporate quickly so
degradation of polyol ester synthetic turbine oils that no solvent remains in the cell and tub-
and are used as the primary monitoring method ing. This is important both for collecting a
for water in high detergent/ dispersant mineral good clean cell background as described in
based lubricants, typically crankcase oils. It can Section 2.1 and for preventing samples from
also be used as secondary monitoring of water in becoming contaminated with rinse solvent
EP additive lubes. when they are pumped into the cell for analy-
sis.
Normal and Abnormal Limits - The solvent need not be very expensive.
• Mineral Crankcase Oils: Normal <30 abs Reagent grade (high purity) solvent is not
units, Alert at 45 abs units necessary.
• Synthetic polyol –Ester Turbine Oils: Normal - The solvent should conform to local regula-
< 20 abs units, Alert at 24 abs units tions regarding hazardous and toxic sub-
50 units = ~ 1000ppm stances.
The solvent needs to evaporate out of the cell and will not evaporate as quickly and it will take more
the tubing leading to the cell so that the FT-IR time to dry the cell for background collection and
can obtain a hydrocarbon free background dur- the chance of contaminating the oil sample with
ing background collection and when running solvent will be greater.
used oil samples. Also, during routine analysis,
hydrocarbons remaining from the solvent may
interfere with the spectra collected from the oil
sample. The fuel measurement is especially sensi-
tive to any solvent remaining in the cell or tubing
because the spectral signature of the solvent may
be similar to that of the fuel.
4.1 TROUBLESHOOTING
+5 Volt
+12 Volt
-12Volt
In this case the troubleshooting procedure depends on the connection topology. The default con-
nection (stand-alone configuration) is established using a cross-over cable between the PC and the
spectrometer, Section 1.3.2. Alternatively, the spectrometer can be connected directly to an Ethernet
network using the Ethernet port. The direction of the data transfer is indicated by the RX and TX
LEDs on the spectrometer’s rear. The TX LED lights when the spectrometer sends data and the RX
LED lights when the spectrometer receives data.
4.2 REPLACING AND REGENERATING latch that is opened with an Allen screw that is
THE DESICCANT IN A located at the left spectrometer side and covered
CARTRIDGE by a black cap.
The desiccant in cartridges must be replaced and 1. Remove this plug and loosen the Allen
regenerated in regular intervals to ensure opti- screw (approximately half a turn)
mum spectrometer performance in case the Spec- using an Allen wrench (6mm), Figure 4.2-2.
tro-FTIR is not purged. 2. Remove the detector compartment lid.
3. Pull the desiccant cartridge out of the
High air humidity level inside the spectrometer holder and inspect the cartrige.
impairs the measurement results. Therefore, a 4 . Insert a new or regenerated desiccant into
desiccant (molecular sieve) is used to reduce the the holder. Ensure that the cartridge top side
air humidity level inside the interferometer and (with the label ’TOP’) is up.
detector compartments. Although these com- 5. Re-install the detector compartment lid by
partments are sealed, the air humidity can reach a performing the above steps (1and 2) in reverse
high level, for example, if the covers are removed order.
because of a component change. The Spectro-
FTIR is equipped with two desiccant cartridges,
one is in the detector compartment and the other
in the interferometer compartment, Figure 4.2-1.
The desiccant cartridges should be regenerated or
replaced approximately every 6 months or at least
when the electronic HUMIDITY indicator (Sec-
tion 1.2.1) on the top of the spectrometer lights
up red.
Detector Interferometer
Desiccant Desiccant
Cartridge Cartridge
4.2.2 Replacing the Interferometer 3. Place the spent molecular sieves in a oven
Compartment Desiccant for at least 24 hours at a temperature of 150
The interferometer compartment lid is secured °C.
with a latch that is opened with an Allen screw 4. Refill the desiccant cartridge with the hot,
that is located inside the source/laser compart- dried sieves and push the black cap on the
ment. white tube.
5. Store the regenerated cartridge in a dry en-
1. Open the source/laser compartment by vironment (e.g. exicator) until a spent cartridge
pressing down near the middle front of the lid needs to be replaced by regenerated one.
and lift it to its full open position.
2. Loosen the Allen screw shown in Figure 4.3 REPLACING THE IR SOURCE
4.2-3 by approximately half a turn using a
6mm Allen wrench to unlatch the interferom- The IR sources are pre-aligned and electrically
eter compartment lid. coded enabling the spectrometer firmware to
3. Take off the interferometer compartment auto-detect the source type. This information is
lid. passed on to the application software, which in
4. Pull the desiccant cartridge out of the turn selects the appropriate parameter set for the
holder and inspect the cartridge. measurement.
5 . Insert a new or regenerated desiccant into
the holder. Ensure that the cartridge top side WARNING: During the spectrometer operation
(with the label ’TOP’) is up. the light source becomes very hot. Avoid any skin
6. Re-install the lids of the interferometer contact. Risk of skin burn! Wait until the light
compartment and the source compartment by source has cooled down sufficiently before you
performing the above steps (1 and 3) in reverse remove it.
order.
To replace the IR source:
4.2.3 Desiccant Cartridge Regeneration 1. Switch OFF the Spectro-FTIR.
Procedure 2. Open the source/laser compartment by
1. Pull off the top black cap (with the label pressing down near the middle front of the lid
’Top’) from the white tube. and lift it to its full open position.
2. Empty the desiccant (molecular sieve) into
a container that can withstand a temperature CAUTION: Wait until the IR source has cooled
of 150 °C. down to room temperature.
Open Compartment with 6mm Allen Wrench
3. Loosen the knurled thumb screw of the IR
source release lever (approximately one turn),
Figure 4.3-1.
4. Press the IR source slightly downwards
while rotating the release lever aside.
5. Take the IR source carefully out of the
holder using the IR source handle.
6. Remove the new IR source from its box
and insert it into the operating position holder.
Ensure that the two pins of the holder engage
in the holes of the IR source.
7. Gently press the IR source downwards and
Figure 4.2-3, Latch for Source/Laser rotate the release lever over the source to secure
Compartment
Manual Configurations
In manual configurations of the Spectro-FTIR,
the filter is on the top of the sipper tube assembly.
To clean or replace the filter disconnect the tubing
at the peristaltic pump to keep it from twisting.
Hold the sipper tube assembly with one hand and
twist the knurled knob on top of the assembly in
a counter clockwise direction, Figure 4.6-1. Re-
move the filter with tweezers or needle nose pli-
ers, Figure 4.6-2. The filter can be cleaned and
Fuse Block
reused unless it is completely clogged with sludge
Figure 4.5-1, Rear View, Locaton of Fuses
and wax, or if there is visual physical damage to
Automatic Configurations
In automatic configurations of the Spectro-FTIR
the filter is in line with the flow cell and the Au-
toSampler sipper tube, Figure 4.. To clean or re-
place the filter, remove the tubing from each end.
Unscrew the two sections of the filter holder. Re-
move the filter with tweezers or needle nose pli-
ers. The filter can be cleaned and reused unless it
is completely clogged with sludge and wax, or if
there is visual physical damage to it. The filter can
be cleaned with kerosene. For stubborn depos-
its on the filter, put the filter in a container with
kerosene. Then put the container in the ultra-
sonic bath for a few minutes, this will probably
break loose any deposits. Install a cleaned or re-
placement filter in reverse order of the procedure
Figure 4.6-1, Gaining Access to the Sipper Tube
described above.
Filter
In-Line Filter