Pyroprobe 5000 Manual

Page 1.
1
100818
P0 BOX 277 465 Limestone Road, Oxford, PA 19363

Phone 610-932-3636 Fax 610-932-4158
TABLE OF CONTENTS
SECTION 1. Contents
Informational symbols 1.3
SECTION 2. Specifications and warranty

Pyroprobe 5000 specifications 2.3
Warranty 2.6
Consumables and part numbers 2.8
CE Declaration 2.9
SECTION 3. Product description and probe calibration

Pyroprobe 5000 description 3.1
Front panel 3.2
Start-up and calibration 3.5
Sample capacities 3.6
Care of filaments 3.7
Failure Codes 3.9
Microswitches 3.11
Flow diagrams 3.12
5150 3.12
5200 3.14
Page 1.2
SECTION 4. Pyroprobe 5000 programming
Base screen 4.1
File menu 4.2
Edit menu 4.3
Tools Menu 4.4
Configuration menu 4.5
Communications menu 4.7
Initial set-up 4.7
Filament programming 4.8
Accessory (interface) programming 4.9
Programmable interface 4.10
5200 Collection Trap 4.11
Cryogenic focuser 4.12
Sequence 4.13
Isothermal zones 4.14
Method editor 4.15
SECTION 5. Operation
Single step pyrolysis 5.2
Removing volatiles 5.3
Desorption 5.4
Trapping mode - 5200 5.5
Multi-step analysis 5.6
Changing to Direct GC Pyrolysis - 5200 5.7
Sample placement 5.8
Filament replacement 5.9
Thermal desorption with 1/4” tube 5.10
Initial start-up of the 5000 series 5.11
Failure Codes 5.12
Test tube desorber 5.18
VOST tube desorber 5.20
SECTION 6. Pyroprobe Installation and GC Interfacing

Model 1500 (isothermal) 6.1
Installation of 1500 6.3
Adapting the septum retainer 6.9
Operation of the 1500 6.10
Page 1.3
Diverter valve installation 6.11
Inserts 6.12
Transfer line - 5150, 5200 6.13
Module assembly - 5150, 5200 6.17
GC Installation - 5150, 5200 6.19
Electrical connections 6.20
Main fuse 6.21
Cryogenic trap 6.30
SECTION 7. Alternative Probes

Direct Insertion Probes for Mass Spectrometers 7.1
Probe connections for DIP 7.2
Connections for FT-IR probes 7.3
Thermocouple probes 7.4
Changing the ballast resistor 7.5
Quartz lined (protected coil) probe 7.7
1/2” Coil Probe 7.9
SECTION 8. Pyroprobe FT-IR Interfacing

Brill Cell Description 8.1
Installation, general 8.2
FT-IR cover 8.3
Pneumatics module 8.3
Pyrolysis using the Brill Cell 8.3
Use with 5150 or 5200 8.4
Brill Cell diagram 8.5
Universal mounting 8.8
Elevated pressure option 8.9
SECTION 9. Sample Handling Kit

Contents of kit 9.1
SECTION 10. Pyroprobe 5250 Autosampler 10.1

Principle of operation 10.1
Sensors 10.4
Operation 10.7
Sample Loading 10.10
Page 1.4
Sequencing GC 10.12
Installation 10.13
Maintenance 10.18
Valve rotor replacement 10.20
Valve break-in mode 10.22
O-rings 10.22
Changing from front to rear tube discharge 10.23
5250T - Trapping autosampler 10.25
Installation 10.26
Operation 10.28
Trap functions 10.31
Cryogenic trapping 10.32
Valve diagram 10.33
SECTION 11. Specialized Systems
Pyrobot
Description 11.1
Installation 11.5
Operation 11.5
High Pressure 5200

Description 11.7
Setting pressure and flow 11.11
Sample loading 11.12
Reactant Gas Option 11.13
Pneumatic connections 11.15
Catalytic Reactor 11.16
SECTION 12. INDEX 12.1

Page 1.5
INFORMATIONAL SYMBOLS
Warning
The WARNING symbol indicates that failure to observe the proper procedures described in
this manual could result in injury to the operator.
Caution
CAUTION is used to indicate that failure to observe the proper procedures in this manual
could result in damage to the Pyroprobe instrument.
Note
The NOTE symbol is used to call attention to particularly important sections of information
within the text of this manual.
!
The Exclamation Point symbol is used on the Pyroprobe instrument to indicate that the
adjacent parts should not be touched before becoming completely familiar with the informa-
tion about those parts in this manual.
Page 1.6
The Shock symbol is used on the Pyroprobe to indicate the potential for an electrical shock
to the user, and that the Pyroprobe must be turned off and unplugged before accessing
these parts.
The Hot Surface Warning symbol is used to indicate the potential that the indicated surface
may be hot and should not be handled until the unit has been turned off and the part has
cooled.
Page 2.1
SECTION 2. SPECIFICATIONS AND WARRANTY
GENERAL
Dimensions
280 mm (11”) W x 381 mm (15”) H x 432 mm (17”) D
Weight 11.8 kg (26 lb)
Electrical Requirements
The CDS Model 5000 Series Pyroprobes operate on 100 - 240 VAC 50/60 Hz 15 amp
grounded power service.
Pneumatic Requirements
The 5000 requires 80 psig maximum of helium or nitrogen (at least 99.999% purity) for purge
operations.
Equipment Rating (Pollution Degree) 2
Installation Overvoltage Category II
The equipment does not contain batteries.
The equipment does not employ laser sources
The equipment does not contain flammable liquids.
The CDS Model 8000 is manufactured in only one location, 465 Limestone Road, Oxford, PA
USA.
Transfer line
Stainless steel clad fused silica
1.2 m standard
0.6, 0.9, and 1.5 m available
Temperatures °C
Recommended Max. Max. Programmable Failsafe Default
Valve Oven 300 350 375 50

Interface (5150, 5200) 325 350 425 50
Transfer Line 300 350 475 50
Adsorbent Trap 300 400 425 50
Aux 1 300 350 475 50
Spares 5,6 300 450 475 50
Probe 1300 1400 1600
Page 2.2
Cleaning
In the event that the external surfaces of the Model 5000 require cleaning, a mild soap and
water solution and a soft cloth should be used. Take standard safety precautions when using
liquids around electrical equipment.
Fuses
The main power fuses are located in the power entry module, where the power cord connects
to the unit.
Individual zone fuses are located inside the electronics cabinet of the Pyroprobe, arranged as
shown in the diagram below.
Warning
The Pyroprobe must be turned off and unplugged before accessing fuses. Only qualified
persons should access the electronics components of the Pyroprobe
R11 R14 R17 R20 R23 R26
R5 R8
U1 U2 U3 U4 U5 U6
R9 R12 R15 R18 R21 R24
J1
J3
TR3 TR4 TR5 TR6 TR7 TR8
U7 U9
R3 R6
TP1
SEE JUMPERS
E1
TR1 TR2 R10 R13 R16 R19 R22 R25
J2 R1
! F1 ! F2 ! F3 ! F4 ! F5 ! F6 ! F7 ! F8
E2
R4 R7 K1
D1
U9
!
C1 E3 REFER TO MANUAL FOR
FUSE VALUES AND TYPES
Q1
J4 R2
L2 L1
WARNING: DANGEROUS VOLTAGES N H
DISCONNECT AC POWER CORD
BEFORE SERVICING
CDS ANALYTICAL,
INC. 6A0053 J5 J6
NOTE: Fuse number and locations depend on specific Pyroprobe model according to the
following chart.
Model F1 F2 F3 F4 F5 F6 F7 F8
220v 115v
5000 2A 4A 2A
5150 2A 4A 2A 2A
5200 2A 4A 2A 2A 0.5A 2A
Page 2.3
SPECIFICATIONS
PYROPROBE 5000
FILAMENT TEMPERATURE Settable in 1°C increments to 1400°C
TIMES Settable in units of 0.01 second to

999.99 sec. or in units of 0.01 minute to 999.99 min.
HEATING RATES Settable in units of 0.01°C/millisecond

from 0.01 to 20.00°C/mS, or
0.01 to 999.99°C/Second, or
0.01 to 999.99°C/Minute
INTERFACE TEMPERATURE Settable in l°C increments to 350°C
TIMES Settable in units of 0.01 minute to

999.99 minutes
HEATING RATES Isothermal Model 1500
DRY MODE User selectable
CLEAN MODE User selectable
SEQUENCE Up to 8 methods, each with GC start

Page 2.4
SPECIFICATIONS
PYROPROBE 5150


0.01 to 999.99°C/Minute

999.99 minutes
HEATING RATES Settable in units of 0.01°C/minute to

60.00 °C/minute.

Page 2.5
SPECIFICATIONS
PYROPROBE 5200


0.01 to 999.99°C/Minute

999.99 minutes
HEATING RATES Settable in units of 0.01°C/minute to

60.00 °C/minute.

Page 2.6
WARRANTY
1. Term of Warranty: Covered Events. Products manufactured by CDS are warranted

for one (1) year parts and labor from the date of shipment against defects in materials
or workmanship.
2. Handling of Warranty Claims: CDS will repair or replace the defective product with
out charge within the warranty period, provided the defective item is shipped to CDS
Analytical, Inc., 465 Limestone Road, Oxford, Pennsylvania 19363. All items re
turned for warranty work must be assigned a Service Return Number (SR #) by the
CDS Service Department before the equipment is returned to the factory. Equip
ment returned to the factory without this number will not be received. Cost of ship
ment to the factory must be paid by the Buyer; cost of return shipment to the Buyer
will be prepaid by CDS. Repair or replacement of a defective item shall not extend
the initial warranty term.
3. Exclusions: This warranty does not cover the following items and events.
a. Failure of mechanical parts due to normal wear and tear.

b. Electrical components that deteriorate due to age, such as tubes, lamps and
the like.
c. Any defect caused by misuse, negligence, accident, or improper installation,
except the installation in accordance with written directions supplied by CDS
shall not be considered improper.
d. Certain parts such as septa, quartz tubes, platinum filaments, etc., are ex
pendable in normal use and their service life is unpredictable. These items
are not covered by this warranty.
e. Buyer-induced contamination or leaks.
4. Limitation of Damages: CDS SHALL NOT BE LIABLE FOR CONSEQUENTIAL

DAMAGES OF ANY KIND ARISING OUT OF THE PURCHASE, INSTALLATION,
USE OR MISUSE OF THE PRODUCTS. CDS’S LIABILITY FOR INCIDENTAL
DAMAGES SHALL BE LIMITED TO THE PAYMENT FOR THE RETURN FREIGHT
(AS SPECIFIED ABOVE) ON DEFECTIVE PRODUCTS SHIPPED TO CDS FOR
REPAIR OR REPLACEMENT.
5. Sole Warranty: This warranty is given in lieu of all other warranties, express or
implied. THERE ARE NO WARRANTIES WHICH EXTEND BEYOND THE DE
SCRIPTION ON THE FACE HEREOF. The Buyer having furnished or agreed to the
specifications of the products sold, NO WARRANTY IS MADE AS TO THE FIT
NESS OF THE PRODUCT FOR ITS INTENDED PURPOSE. Except as specifically
set forth herein, NO WARRANTY IS MADE AS TO THE MERCHANTABILITY OF
THE PRODUCT.
Page 2.7
6. “Warranty Registration Card”: The Warranty Registration Card included with this
package must be returned to register the product.
7. Modification in Design or Discontinuance of Products: CDS reserves the right to

discontinue manufacture of products without notice, and to make modifications in
design at anytime without incurring obligation to make such modifications to prod-
ucts previously sold.
Page 2.8
ORDER NUMBERS FOR CONSUMABLES
The following is a list of parts and accessories which are the most likely to be reordered and
replaced, along with the corresponding part numbers. These items may be obtained directly
from CDS Analytical, Inc. by calling 610-932-3636 and requesting the sales department, or by
contacting your local international distributor. Contact information for international distributors
may be found at www.cdsanalytical.com by selecting “Sales Distribution”, then International.
Item Part Number
1/4" Coil filament rod 10P25003
1/4" Ribbon filament rod 10P25002
Probe seals (25) 1002-0333
Graphite ferrules (10) 1006-0345
Economy quartz tubes (100) 10A1 3008
Fire-Polished quartz tubes (20) 10A1 3007
Quartz wool 1001-0345
Septum retainer for interface 1001-0162
Sample handling kit 0100-9014
Collar for 1/4" probe 2002-0642
6 mm Vespel ferrules PL50 4912
Probe Rod Repairs - Each size and style of probe has a different part number. These numbers
can be obtained by calling CDS Analytical.
Page 2.9
Declaration of Conformity
Application of Council Directives:
EMC 98/33/EEC as amended by 92/31/EEC and 93/68/EEC

LVD/ 73/23/EEC as amended by 93/68/EEC and IVD 98/79/EEC
Standards to which Conformity is Declared:
EN 61326: with A1 1998 and A2 2001 and EN 55011: 1998 Class A/B
EN 61010-1:2001
Declarer’s Name: CDS Analytical, Inc.
Declarer’s Address: 465 Limestone Road, Oxford, PA 19363-0277 USA
Type of Equipment: Laboratory Analytical Device

Model Number: Pyroprobe 5000 Series, Models 5000, 5150, 5200 and 5250
MET Report: 16874 July, 2005
I, the undersigned, hereby declare under my sole responsibility that the equipment specified above
conforms to the above Directives and Standards
July 13, 2005

(Signature) (Date)
Woodford Bowe, Jr. Senior Design Engineer

(Printed name) (Title)
Page 3.1
SECTION 3. PRODUCT DESCRIPTION, PROBE CALLIBRATION
CDS ANALYTICAL, INC. PYROPROBE 5000
DESCRIPTION
The CDS Analytical Pyroprobe 5000 is a multiple step, platinum filament pyrolysis instrument
which prepares samples for analysis by gas chromatography, mass spectrometry or FTIR. The
microprocessor of the Pyroprobe 5000 controls the temperature of the filament by calculating
the resistance of the filament at setpoint temperature and supplying the correct voltage to
achieve that temperature. Filaments are available in a variety of designs and sizes, and the
Pyroprobe 5000 comes supplied with one ribbon probe, for placing samples directly onto the
surface of the filament, and one coil probe, for pyrolysis of samples in a quartz tube. There are
three basic modes of operation: Run, for pyrolysis of the sample in either a single step (like
the Pyroprobe 1000) or in a sequence made of several methods; Dry, for removing solvent
from a sample deposited as a solution onto the ribbon filament; and Clean, for removing
residual material from the filament between runs. In the Pyroprobe 5000, the times and tem-
peratures for the Dry and Clean features are user selectable.
The Pyroprobe 5000 is interfaced to a gas chromatograph by means of a heated chamber

which houses the filament rod during pyrolysis. The temperature of this interface and the
temperature of the pyrolysis filament constitute one method. A sequence of methods may
contain up to eight steps, and each step includes an initial temperature, a heating ramp and a
final temperature for the Pyroprobe filament, plus GC start. For the pyrolysis filament, the
temperatures may go to 1400°C and the rates may range from 0.01°C/ minute to 20,000°C/
second, settable in degrees per minute, second or millisecond. For the interface, tempera-
tures may be set to 350°C.
All programming, temperature selection, calibration and run initiation are performed through
the PC interface of the Pyroprobe 5000. Selecting the Pyroprobe, Accessory or Sequence
icon displays the required fields for those functions. One method includes the Pyroprobe
initial, ramp and final setpoints, and Interface setpoints. Methods are saved, edited and
recalled as with any other Windows based program. During a run, the actual temperatures for
both the probe and interface are displayed on the screen, and setpoints may be examined in
other program methods.
Page 3.2
FRONT PANEL
The front panel of the Model 5000 includes sever LEDs for indicating the running status of the
instrument plus keys which may be used to start and stop a method, run the dry functionand run
the clean function.
At the top of the panel are four status indicators which light Green when the zone is Ready and
Red when it is not. These indicate the ready status of the Probe itself, the GC, the Reactant
Gas option and an external input.
Below the ready status LEDs are running status LEDs which show the state of the 5000 when
it is executing a method. One set of LEDs lights sequentially for the Initial, Ramp and Final
steps of the probe filament, and a second set shows the same for the programmable interface
zone.
Below these are four keys which permit starting the 5000 from the front panel instead of from
the PC. To run, a method must be programmed and downloaded from the PC to the 5000, but
then these keys may be used to execute the Dry and Clean functions, to Start the method and
to stop (Reset) the method.
At the bottom of the front panel are two more LEDs which light to show that the Dry and Clean
functions are in progress.
Page 3.3
PYROPROBE 5150
The Model 5150 adds to the Model 5000 the ability to program a low-mass interface zone.
Instead of using the standard Model 1500 GC interface on the injection port of the GC, the
Model 5150 incorporates the interface zone into the body of the Pyroprobe, and connects to
the GC using a heated transfer line. In addition, the on-line/off-line valve is placed into a sepa-
rate valve oven. This greatly reduces the mass of the interface and permits heating and cool-
ing the interface zone of the Pyroprobe quickly. All of the setpoints and features of the
Pyroprobe filaments themselves are the same for the 5000 and 5150, and both insturmants
may run a sequence of up to eight methods.
In the Pyroprobe control software, under Configuration, then Accessory type, the 1550 must be
selected when using the 5150. In addition to providing rapid heating and cooling of the inter-
face zone, the 5150 automatically places the Pyroprobe on-line and off-line for multiple runs in
a sequence.
Page 3.4
PYROPROBE 5200
The Model 5200 adds to the 5150 a second heated zone connected to the valve oven. This
second zone may be used with a sorbent as a trapping zone, permitting the use of a reactant
gas for pyrolysis. In this mode, air sweeps the Pyroprobe filament during pyrolysis, but the flow
goes to the trap, not to the GC. After collection, the trap zone is placed on-line with the GC
and desorbed to make the injection. A manual valve is located on the front of the pneumatics
which permits easy switching from trapping to direct pyrolysis mode.
Page 3.5
START-UP AND CALIBRATION
To insure probe-to-probe reproducibility of pyrolysis temperature, each probe rod is tested and
calibrated at the factory by CDS Analytical. A calibration number is determined for each rod,
and this number is printed on the shaft of the rod (see diagram below). This number is entered
into the computer under the Configuration menu as shown below. By clicking on Configuration,
then Probe Cal #, a small window is brought up that asks for the numerical value of the figure
on the probe rod band. Simply enter this number and click on OK.
Page 3.6
PYROPROBE SAMPLE CAPACITIES
When introducing a sample to a gas chromatograph by pyrolysis, it is important to consider the

GC capacity in deciding sample size. Most gas chromatographic analyses use approximately
1 µL sample injections, which translates to about 1 mg of total sample. If a pure organic
material, such as a synthetic polymer, is being pyrolyzed, it will be completely vaporized in
pyrolysis, and transferred to the GC. It is important that the sample is small enough to ensure
complete pyrolysis at the final temperature, and not overload the analytical system. In general,
sample sizes of 10 to 100 µg will pyrolyze readily and not exceed the capacity of the GC
column.
Some analysts pyrolyze samples which are not all organic, or are not completely vaporized,
such as soils, fuel source minerals and composites. Consequently, they must use larger
samples to increase the amount of organic material actually delivered to the GC.
Listed below are the standard quartz tubes and boats available for the coil Pyroprobes, with
approximate maximum sample capacities for each. These assume that the quartz tube is no
more than 1/2 full, and are based on a sample density of 1.0. Dimensions are in overall
Length, Inside Diameter for the tubes, and Depth for the boats.
Probe Size Quartz Tube Dimensions Capacity Boat Dimensions Capacity
1/4" 25 mm L, 1.9 mm I.D. 40 mg 25 mm L, 1.5 mm D 50 mg

PN 10A1-3007 PN 1001-0346
1/2" 25 mm L, 5 mm I.D. 250 mg 20 mm L, 6 mm D 300 mg

PN 1005-0348 PN 10A1-3001
Page 3.7
CARE OF PYROPROBE FILAMENTS
The filament of the Pyroprobe is made of platinum and may be distorted through im-
proper handling. The temperature of the filament is dependent on the resistance of the plati-
num, and will be adversly affected if the filament is bent or damaged. In addition, bending the
coil so that the loops touch each other, or the side of the probe body, will cause the probe to
short circuit, overheating and damaging the filament.
Ribbon filaments expand when heated and may touch the inside of the interface when
fired, causing the filament to short and burn out. To prevent this, observe the flex of the ribbon
while firing it in air, and be sure that it deflects toward the center of the probe rod, instead of
away from the rod.
Always be sure to insert the quartz sample tubes straight into the coil to minimize the
chance of coil damage. Never operate the Pyroprobe if the coil is touching the side of the
probe body or if the coil has been compressed so that the loops are touching.
If the coil has become bent or distorted, it may be straightened using fine point tweezers.
First, insert a quartz tube into the coil to stabilize it. Then using gentle pressure with the twee-
zers, adjust the loops of the coil so that they are not touching each other or the side of the
probe.
Page 3.8
If a coil cannot be straightened satisfactorily, it should be replaced with a new probe
rod. The damaged rod may be sent back to CDS Analytical for repair, which includes replace-
ment of the coil element with a new coil and recalibration of the probe rod.
PYROPROBE RIBBON FILAMENTS
When using a ribbon filament probe rod with a standard Pyroprobe interface, be sure that the
filament flexes away from the interface so that platinum ribbon does not touch the inside the
interface. If the filament contacts the interface during firing, it could become damaged. Test
fire the Pyroprobe in the air to see the direction of flexing as the filament heats. If the ribbon
flexes outward, press it gently (when cold) toward the center of the probe rod, and fire again to
insure that it now flexes inward, away from the interface wall.
When applying a sample to the ribbon, be careful not to puncture or tear the platinum. This will
cause overheating at the damaged spot, and will destroy the filament.
Page 3.9
FAILURE CODES
READY LEDs
Probe (used for Open)
External (used for Shorted)
GC (used for Over Temperature)
Probe LEDs
Initial (used for interface)
Rate (used for transfer line)
Final (used for spare 5)
Accessory LEDs
Initial (used for spare 6)
Rate (used for Aux 1)
Final (Used for trap)
Clean LED
(used for probe)
In addition to displaying the operating step and ready status of the Pyroprobe, the LEDs on the
front panel are used to indicate the location of an electrical failure. Various circuits are moni-
tored, and will be indicated as being OPEN, SHORTED OR OVER TEMPERATURE. In the
case of a failure, then, two of the LEDs will be illuminated, one indicating the circuit involved
and one showing the specific problem.
The READY LEDs at the top of the panel are used to show the type of failure. If the circuit is
OPEN, the PROBE LED will light. If the circuit is SHORTED, then the EXTERNAL LED will be
on, and if the zone is OVER TEMPERATURE, then the GC LED will be on.
The specific circuits are indicated by the INITIAL, RATE and FINAL LEDs for both the probe
and accessory. A complete list of the locations and corresponding LEDs is on the next page.
For example, if the transfer line had shorted, the PROBE RATE and EXTERNAL LEDs would
both be lighted. If the CLEAN LED and the PROBE LED are both on, then the Pyroprobe
filament circuit is open, probably indicating a broken filament.
Page 3.10
FAILURE CODE LIST
EXT LED means SHORTED

PROBE LED means OPEN
GC LED means OVER TEMPERATURE
CHANNEL CIRCUIT LED USED
1 Spare 5 Probe final

2 Transfer line Probe rate
3 Programmed interface Probe initial
4 Trap Accessory final
5 Auxiliary 1 Accessory rate
6 Spare 6 Accessory initial
7 MFC 1 Dry
8 Probe actual Clean
LED COMBINATIONS
Probe Ready and Clean Probe is OPEN
Probe Final and

External Spare 5 is Shorted
Probe Ready Spare 5 is Open
GC Spare 5 is Over temperature
Probe Rate and

External Transfer line is Shorted
Probe Ready Transfer line is Open
GC Transfer line is Over Temperature
Probe Initial and

External 5150 Interface is Shorted
Probe Ready 5150 Interface is Open
GC 5150 Interface is Over Temperature
Page 3.11
Accessory Final and

External Trap is Shorted
Probe Trap is Open
GC Trap is Over Temperature
Accessory Rate and

External Auxiliary 1 is Shorted
Probe Auxiliary 1 is Open
GC Auxiliary 1 is Over Temperature
Accessory Initial and

Probe Spare 6 is Open
GC Spare 6 is Over Temperature
MICROSWITCHES
Features, options and model designation for the CDS 5000 series Pyroprobes are dictated by
the microswitches on the electronics board. The proper switch configurations for Models 5000,
5150, 5200 and 5250 are shown in the diagram below.
Page 3.12
FLOW DIAGRAMS
1500 INTERFACE
Page 3.13
MODEL 5150
READY
(HEATED OVEN CHAMBER)
TIC TAH TAHH

GC CARRIER IN TALL
RTD
REACTANT GAS OPTION TO GC

(FRONT PANEL) 3 4
CARRIER IN 2 5
1/16"
1 6
8 7
REACTANT GAS PURGE FLOW ADJUST

SV-1
TIC TAH TAHH
TALL
VALVE OVEN
RTD
SWAGEL
TAHH
(LEFT SIDE PANEL) (FRONT PANEL) TALL
TAH
SAMPLE VENT L E G AWS
STATUS
MPV1 DE-ENERGIZED
TIC
INTERFACE REST TEMP
PROBE OFF RTD
INTERFACE
REACTANT GAS OPTION
PROBE
SV-1 DE-ENERGIZED
MODEL 5150
RUN
TIC TAH TAHH

GC CARRIER IN TALL
RTD
REACTANT GAS OPTION TO GC

(FRONT PANEL) 3 4
CARRIER IN 2 5
1/16"
1 6
8 7
REACTANT GAS PURGE FLOW ADJUST

SV-1
TIC TAH TAHH
TALL
VALVE OVEN
RTD
SWAGEL
TAHH
(LEFT SIDE PANEL) (FRONT PANEL) TALL
TAH
STATUS
MPV1 ENERGIZED
TIC
INTERFACE RUNNING
PROBE ON RTD
INTERFACE
REACTANT GAS OPTION
PROBE
SV-1 DE-ENERGIZED
Page 3.14
DIRECT PYROLYSIS MODE
MODEL 5200
PY-GC MODE (REST / LOAD / ACC. INITIAL)
(PURGINGTO VENT)
TIC TAH TAHH
GC CARRIERIN (HEATEDOVEN C H A M B E R )
TALL
RTD
TRAP DESORB TO GC
REACTANTGAS OPTION
(FRONTPANEL) 3 4
CARRIERIN 2 5
1 6
8 7
REACTANTGAS SV-1 SAMPLEPURGE 1/16"

LOWERMPV
TIC TAH TAHH
TALL
VALVEOVEN
RTD
SWAGEL
(LEFT SIDE PANEL) (FRONTPANEL)
SAMPLEVENT L EGAWS
TRAP PY-GC
1 2
5 6
8 7
4 3 1/16"
TAHH UPPERMPV TAHH
TALL TALL
TAH TAH
TIC TIC
RTD RTD
INTERFACE
TRAP
PROBE
Page 3.15
DIRECT PYROLYSIS MODE
MODEL 5200
PY-GC MODE (RUNNING / ACC. RAMP)
TIC TAH TAHH
GC CARRIER IN (HEATED OVEN CHAMBER)

TALL
RTD
TRAP DESORB TO GC
REACTANT GAS OPTION

(FRONT PANEL) 3 4
CARRIER IN 2 5
1 6
8 7
REACTANT GAS SV-1 SAMPLE PURGE 1/16"

LOWER MPV
TIC TAH TAHH
TALL
VALVE OVEN
RTD
SWAGEL
(LEFT SIDE PANEL) (FRONT PANEL)

TRAP PY-GC
1 2
5 6
8 7
4 3 1/16"
TAHH UPPER MPV TAHH
TALL TALL
TAH TAH
TIC TIC
RTD RTD
INTERFACE
TRAP
PROBE
Page 3.16
PYROLYSIS WITH TRAPPING MODE
MODEL 5200
ACCESSORY INITIAL
TIC TAH TAHH

TALL
RTD
TRAP DESORB TO GC
REACTANT GAS OPTION

(FRONT PANEL) 3 4
CARRIER IN 2 5
SAMPLE PURGE
1 6
8 7

LOWER MPV
TIC TAH TAHH
TALL
VALVE OVEN
RTD
SWAGEL

TRAP PY-GC
1 2
5 6
8 7
4 3 1/16"
TAHH UPPER MPV TAHH
TALL TALL
TAH TAH
TIC TIC
RTD RTD
INTERFACE
TRAP
PROBE
Page 3.17
PYROLYSIS WITH TRAPPING MODE
MODEL 5200
ACCESSORY FINAL
TIC TAH TAHH

TALL
RTD
TRAP DESORB TO GC
REACTANT GAS OPTION

(FRONT PANEL) 3 4
CARRIER IN 2 5
SAMPLE PURGE
1 6
8 7

LOWER MPV
TIC TAH TAHH
TALL
VALVE OVEN
RTD
SWAGEL

TRAP PY-GC
1 2
5 6
8 7
4 3 1/16"
TAHH UPPER MPV TAHH
TALL TALL
TAH TAH
TIC TIC
RTD RTD
INTERFACE
TRAP
PROBE
Page 4.1
SECTION 4. PROGRAMMING
All control setpoints for the Pyroprobe 5000 are entered through the Windows based con-
trol software installed on a PC. Installation provides an icon on the desktop, which is
double-clicked to produce the base screen for the Pyroprobe.
This base screen has icons on the left side for the Pyroprobe, the Accessory (interface)
establishing a Sequence of methods and for displaying Isothermal Zones. Across the top
of the screen is a menu bar with selections for:
File
Edit
Tools
Configuration
Communication
View and
Help.
The functions of these menu items, as well as basic setpoint entry, are described on the
following pages.
Page 4.2
FILE MENU
Selecting FILE from the menu bar produces choices for starting a new method, saving the
method, opening a previously saved method, etc., as well as setting up printer parameters.
Selecting New Method will enter zeroes into all fields of the display so that a completely
new method may be created. Methods include all setpoints (both probe and accessory or
interface) and are saved with the extension .m50. Selecting Save Current Method saves
any changes using the existing method name. Selecting Save Current Method AS will
save the current setpoints but allow the use of a new method name.
Page 4.3
EDIT MENU
Selecting EDIT from the menu bar permits the use of typical edit functiions such as cut,
copy and paste. As with other Windows type programs, the entry to be cut or copied must
be hi-lighted before the function is selected.
Page 4.4
TOOLS MENU
Selecting TOOLS from the menu bar provides two selections, the Method Editor and ac-
cess to the PIDs for the various heaters. PID values are set for the heaters at the factory
and under normal conditions require no adjustment by the user.
The Method Editor window presents a screen with all the values needed for a complete
method on one page, and is a convienent way to review and revise methods. Methods
may be programmed, edited and saved using the editor, which is described in detail on
page 4.12.
Page 4.5
CONFIGURATION MENU
The Configuration menu includes selections for Accessory Type, GC Handshaking and is
where the probe Calibration number is entered.
Under Accessory Type, the selection is between the 1500 interface and the 1550 inter-
face. The Model 5000 is usually used with the standard 1500 interaces, which is the
valved box which is mounted on the GC injector. The Model 5150 uses the 1550 interface,
which is the low mass zone located on the 5150 itself, connected to the GC using a trans-
fer line. Although initial, ramp and final zones are presented for each, it is recommended
that the 1500 be used isothermally, since the presence of the valve makes the interface
mass larger than the 1550 zone of the 5150, making it heat and cool more slowly.
Under GC Handshaking, the choices are Look at GC Ready and Issue GC Start. In most
analyses, both of these functions should be checked. This tells the 5000 to wait for a GC
ready signal before pyrolyzing the sample, and to Start the GC when the probe fires.
These commands may be turned off if the user wishes to start the GC manually, if a ready
signal is not available, or if the 5000 is connected to a device other than a GC.
When changing the probe rod, the new calibration number (located on the yellow tag on
the rod itself) should be entered by selecting Probe Cal # in this menu.
Page 4.6
CONFIGURATION MENU - 5200
In addition to the trapping zone, the Model 5200 adds the ability to use the Pyroprobe
directly to the gas chromatograph or to the trap first. Selection of which mode will be used
with the 5200 is made on the configuration page. If the Pyroprobe 5200 is to be used
directly to the GC without trapping, the probe must be located on the right-hand heating
zone, and the Py Mode button selected in the Configuration menu. If the Pyroprobe is to
be used with trapping first, with or without a reactant gas, the probe must be inserted into
the left-hand heating zone, with a packed tube (trap) installed into the right-hand heating
zone, and the “Collect on Trap” button selected in the configuration menu.
NOTE: Changes must be made in the configuration of the 5200 while it is off-line from the
computer, to prevent accidently changing modes while the Pyroprobe is running. The
Operating Mode and Calibration sections will be grayed-out when the Pyroprobe is con-
nected to the computer. To make changes in the configuration, first go to Communications
and select Disconnect, then reconnect after the changes have been made.
Page 4.7
COMMUNICATIONS MENU
The Communications menu provides control of the communication between the PC and the
5000 unit itself. Clicking on the top entry (Connect) establishes communication to the
5000, which is confirmed by a tone at the 5000, at which time the top line changes from
“Connect” to “Disconnect”.
NOTE: INITIAL SET-UP
The first time the Pyroprobe is connected to a PC, the DCI software will read the
microswitches in the Pyroprobe unit to see which features are available. After clicking on
CONNECT, check the CONFIGURATION window to confirm that the proper configuration
has been selected. If a different configuration is required, DISCONNECT, then select the
proper configuration, then click on CONNECT again. The DCI will now store this configura-
tion for future use.
When installing the 5000, the Auto Detect COM Port function may be used to establish the
correct com port used on the PC to communicate with the 5000. In addition, the software
may be set to connect automatically when the program is opened.
Page 4.8
PROGRAMMING THE PYROPROBE FILAMENT
A method includes all parameters for the Pyroprobe filament, the interface zone, the clean
and dry functions and the isothermal setpoints. The screens for setting parameters for
each function are selected by choosing the appropriate icon on the left-hand side of the
window. Selecting Pyroprobe presents the screen for entering the initial, rate and final
setpoints for the filament itself, plus the clean and dry functions.
The filament initial and final temperatures are set in °C, in 1° increments up to 1400°. Time
may be set in seconds or minutes, by selecting either S or MN under UNITS. The heating
rate of the filament may be set in °C per minute, second or millisecond. For pulse experi-
ments a value between 10 and 20°C/ms is recommended.
The Pyroprobe filament fires at the start of the Interface or accessory FINAL step. This
permits adjusting the interface zone temperature before actually pyrolyzing the sample.
Pressing RUN METHOD will start the current method, time the interface, then fire the probe
and start the GC at the accessory final step.
Clicking on CLEAN or DRY on this screen will immediately take the Pyroprobe filament to
the setpoint temperature for the programmed time for those functions.
Start, Dry and Clean may also be activated by pressing the appropriate key on the front
panel of the 5000 unit itself.
Page 4.9
PROGRAMMING THE ACCESSORY (INTERFACE)
The interface zone for the Pyroprobe is also set in °C, with a maximum of 350°C. To pro-
long the life of the rotor used in the 1500 valved interface, a maximum extended use tem-
perature of 300°C is recommended.
Since the 1500 interface uses a valve oven to house the probe, it is suggested that this
interface be used isothermally. This is done by entering the same value for the initial and
final temperatures. As shown above, the interface would stay at 275°C, and when the Run
Method button is pressed, the probe would fire at the start of the Final step, 0.10 minutes
into the run. To make the probe fire immediately, an initial time of 0 may be entered.
NOTE: The interface final time must always be longer than the Total Pyroprobe time. In
addition, when using the CDS 8000 Desorber instead of the 1500 interface, the interface
setpoint temperature must be equal to the “actual” to obtain a ready for the unit, and the
interface Final must be programmed with a time longer than the total Pyroprobe time.
The interface has a rest temperature to be used between runs. The Heater On box must
be checked to heat the interface, and may be unchecked to cool it without changing the
rest temperature value.
The Method may be started by clicking on Run Method from this screen or from the
Pyroprobe screen.
Page 4.10
PROGRAMMABLE INTERFACE ZONE
The Pyroprobe 5150 connects to the GC using a heated transfer line and has the valve in
an isothermal valve oven, so the interface zone for the probe is low-mass and easily pro-
grammable. In the above example, the interface zone rests at 75°C. When Run Method is
pressed, the zone goes to 100°C, then from 100° to 200° at 50°C/minute. When the inter-
face reaches 200° at the start of the Final step, the probe is fired and the GC started. The
interface zone will stay at 200° for five minutes, then return to the 75° rest temperature until
the next run.
Page 4.11
5200 COLLECTION TRAP
When using the trap of the 5200, carrier gas from the probe zone goes through the trap
during pyrolysis, and the collected products are transferred to the GC by desorbing the
trap. This permits slow heating rates with collection of the pyrolysate and the use of a
reactant gas - usually air or oxygen - as the carrier gas without introducing that gas to the
GC.
On the 5200 TRAP page, the reactant gas feature is selected by checking ENABLED in the
Reactant Gas field. The reactant gas time is the amount of time during the interface FINAL
step that the reactant gas is used as carrier. This time must be less than the interface final
time. After that time, the carrier gas is switched to inert - usually helium - to flush the air
from the system before heating the trap to the GC.
On the trap collection page, the desorption parameters for the trap heater are selected. A
rest temperature is entered, which is the temperature at which the sorbent tube will be held
between runs and while the sample is being collected. The desorb parameters - tempera-
ture and time - are used to desorb the collected analytes and transfer them to the GC at
the beginning of the GC run.
If the Pyroprobe is equipped for Cryogenic Trapping, there is also an Initial temperature,
which is subambient, for the trap. For this feature, microswitch # 2 must be ON and switch
# 3 must be OFF. In use, the trap goes from the Rest temperature to the Initial before the
sample is delivered to the trap. The trap stays at the subambient Initial temperature
through the Interface Final time. After collecting the sample, the trap is heated to the GC
using the desorption temperature and time as normal.
Page 4.12
CRYOGENIC REFOCUSER
The Pyroprobe 5150 and 5200 may be equipped with a cryogenic refocuser at the GC
injection port to refocus analytes transferred at low flows, especially when doing splitless
capillary analysis. In these cases, the pyrolysis (in the pyrolysis mode) or the trap desorp-
tion (in the trap mode) products are first frozen onto the column at subambient tempera-
tures, then vaporized at the beginning of the GC run. The Crogenic focuser has a Rest
temperature used between runs to conserve cryogen, an Initial temperature, used to refo-
cus the analytes, and a Final temperature to vaporize the trapped compounds and start the
GC.
The Rest time allows the cryogenic focuser to be chilled with liquid nitrogen before the
sample is transferred to it. The cryogenic focuser must be at its Initial temperature before
the sample is pyrolyzed or the trap desorbed to collect the analytes efficiently. The time for
the Initial step coincides with the time that the interface is on-line in the pyrolysis mode, or
with trap desorption time in the trapping mode. The GC start signal is sent at the beginning
of Final time, which should be long enough to permit vaporization of the trapped analytes
and complete transfer out of the cryogenic focuser and into the GC.
When cryogenic refocusing is not needed, the cryogenic focuser may be “Disabled” by
clicking on the box next to “Enabled”. At that time, the cryogenic focuser automatically goes
to the same temperature as the transfer line and the unit works as a standard 5150 or 5200.
When using the Cryogenic Focuser, Microswitch # 3 must be ON and switch # 2 must be
OFF.
Page 4.13
CREATING A SEQUENCE OF METHODS
Once a sample has been loaded into the 5000 or 5150, it may be analyzed using several
methods sequentially and automatically. Up to eight methods may be used in a sequence,
each one with a pyrolysis and interface program, starting the GC each time. The use of the
5150 low-mass interface zone is especially useful in proceeding through a series of tem-
peratures from low to desorb volatiles and semivolatiles to high for pyrolysis.
In the Sequence Table, double-clicking on a numbered line opens the Select Method
window. Double-clicking any method enters that method with all of its parameters as the
method to be run in that step of the sequence. When the complete sequence has been
defined, it may be saved as a sequence by selecting FILE, then SAVE. The sequence will
be saved with a name and a .s50 extension. To initiate the whole sequence, the RUN
SEQUENCE button is pressed from the Sequence screen. In the above example, a
sample is sequentially heated to 300°, 650°, 750° and then 1000°C, with a GC run each
time. This would provide runs for volatiles and semivolatiles, pyrolysis and then higher
temperature runs to evaluate the completeness of the pyrolysis runs.
Saved sequences may be opened by selecting FILE, then OPEN A SEQUENCE. It is

important to be sure that the GC is also programmed with a sequence so that each run will
be saved and a GC Ready signal will be sent to the 5000, so that it may go to the next
method.
Page 4.14
SETTING ISOTHERMAL TEMPERATURES
The Pyroprobe is capable of controlling up to four isothermal zones. For the 5150, two of
these are pre-set as the valve oven (for the on-line/off-line valve) and the heated transfer
line to the GC. These values are saved as part of the method. Each zone may be turned
on or off by checking the Heater On box displayed in the Iso Zones screen.
Page 4.15
METHOD EDITOR
Selecting Method Editor under the Tools menu presents the screen shown above. This
Method Editor page permits entering all the setpoints for all parameters needed for a com-
plete method. Using the File menu from this page permits opening, saving, saving as, and
so on as for other screens. This is a convenient page for both preparing a complete
method and for reviewing all of the parameters that are saved as an existing method.
Send Method
Methods may be edited and saved using the Method Editor page without changing the
active method used by the Pyroprobe. The Send Method command in the File menu will
load the displayed method to the Pyroprobe, replacing all values with the new ones.
Page 5.1
SECTION 5. OPERATION
The Pyroprobe 5000 Series are very versatile sample introduction instruments. When
using the 5150 or the 5200, with programmable interface zones and automatic valve
switching, it is important to keep in mind that the valve rotates at the beginning of the
interface RATE step. Before that, purge gas is going through the sample chamber and out
to vent. This permits venting volatiles, residuals and contaminants before pyrolyzing the
sample. If transferring the volatiles to the GC (instead of venting them) is desired, the
Pyroprobe must be programmed with that in mind. Examples are shown here of how to
establish different modes of testing by selecting the right Pyroprobe parameters. These
modes include:
Single step pyrolysis (venting volatiles)

Single step pyrolysis after removing semivolatiles
Single step pyrolysis (transferring volatiles to the GC)
Single step desorption (low temperature)
Reactant gas pyrolysis with trapping
Multiple step analysis

Page 5.2
SINGLE STEP PYROLYSIS
The setpoints above wil produce a simple pyrolysis run by heating the filament to 750°C for
10 seconds.
VENTING VOLATILES
This Pyroprobe filament program will start when the Accessory or Interface begins its
FINAL step, after a delay to insure that the interface is at Final temperature and that the
GC carrier has re-equilibrated. Under normal conditions, the interface zone may be kept
cool between runs (using the REST temperature) then programmed to a higher tempera-
ture before the Pyroprobe filament is heated. Using setpoints for the interface zone like the
ones shown below will heat the interface at the INITIAL step before placing it on-line with
the GC at the beginning of the RATE step. In this program, any volatiles produced during
the initial heating will be vented by the purge gas, and the pyrolysate will be transferred to
the gas chromatograph.
This mode may be accentuated by programming an intentional pre-heat and vent step,
using the interface initial temperature and time to remove oils, plasticisers, residuals and so
on before pyrolysis.
Page 5.3
This program heats the interface to 100°C and vents volatiles at that temperature before
placing the interface on-line, heating to 250° and then pyrolyzing.
SINGLE STEP, REMOVING SEMI-VOLATILES
By increasing the INITIAL step parameters, the sample is heated to 200°C and purged to
vent for three minutes before putting it on-line with the GC, and raising the interface zone
to 250°C for pyrolysis.
Page 5.4
SINGLE STEP, TRANSFERRING VOLATILES
To prevent the loss of voaltiles in a single step run, an initial time of zero should be entered,
and the interface heated as quickly as possible. This is programmed by entering a zero for
the heating rate of the interface.
With this program, the valve will rotate immediately, and the interface zone will heat
quickly, but the Pyroprobe filament will not be heated until the interface actually reaches
250°C. The start signal to the GC will coincide with the firing of the probe.
SINGLE STEP, LOW TEMPERATURE DESORPTION
The above approach may be used without pyrolysis to look just at the volatile or semi-
volatile constituents in a sample. By using a zero heating rate for the interface and a low
“pyrolysis” temperature (forexample, 250°C for 15 seconds) the sample will be placed on-
line with the GC, then quickly heated to a desorption temperature, automatically starting the
GC when the filament fires.
Page 5.5
TRAPPING MODES, REACTANT GAS ANALYSIS
When the 5200 is used in the trapping mode, the valve is used to place the Pyroprobe
filament on-line with the trap, and the trap on-line with the GC. The Pyroprobe filament still
fires at the beginning of interface FINAL, so all of the manipulations discussed are avail-
able, but the resulting analytes are trapped first. This trapping step allows the use of air as
a sample gas, permitting oxidative studies without introducing air to the GC, and permits
collection of volatiles at lower temperatures, with trapping for better chromatography. If
equipped for cryogenic trapping, the trap Initial temperature may be subambient during the
trapping step.
The combination of interface and trapping programs shown here would allow the sample to
be placed into the Pyroprobe at 75°, then heated at 50°/minute to 250°, during which it
Page 5.6
would be on-line with the trap. Any volatile compounds would be trapped during the inter-
face program. The Pyroprobe would fire at interface FINAL, so any pyrolysis and oxydation
products would be collected onto the trap. The total interface time is 5.5 minutes. The
reactant gas time is set to 4.5 minutes, so that during the last minute of flow to the trap,
carrier gas is automatically changed to helium to remove the residual air from the trap
before transferring the trap to the GC. Volatiles could be vented by adding an interface
INITIAL time.
MULTIPLE STEP ANALYSIS
A sample may be placed into the Pyroprobe and analyzed multiple times, either repeating
the same parameters or using new ones. This is accomplished by building a sequence of
methods and starting the sequence from the Sequence page. The GC is started each time
the filament is heated for a Pyroprobe 5150 and each time the trap is heated for a 5200 in
the Trap mode. Use of the method editor tool is a convenient way to review and change
parameters for a sequence of methods, to be sure that all the parameters are entered and
the sequence is in the proper order.
It may be desired to cool the sample after each method while the GC is running, but a
different Interface Rest temperature may be used for each step.
Page 5.7
CHANGING FROM TRAP MODE TO DIRECT PY-GC MODE
The Pyroprobe 5200 is equipped with a manual mode select valve on the front of the unit.
The two positions for this valve are TRAP and GC. To switch between going directly to the
GC and pyrolyzing with the trap, simply turn the valve to the desired mode.
Mode select valve
FIGURE 5.1.
5200 mode switching valve.
Page 5.8
SAMPLE PLACEMENT
Decisions concerning the use of a coil or ribbon probe, sample amount, temperature and
time for pyrolysis etc. depend primarily on characteristics of the sample, including its physi-
cal state, organic content, thermal stability, homogeneity and solubility. If a sample may be
dissolved in a suitable solvent, it may be placed onto the element of the ribbon probe
directly using a syringe. Likewise, if the sample has a fairly low melting point, a small piece
may be melted onto the ribbon probe to secure it for pyrolysis. Samples such as powders,
fibers, chips and materials which would be altered by melting should be pyrolyzed in a
quartz tube in the coil element.
For either element type, the sample should be placed at the center of the filament for py-
rolysis. Samples pyrolyzed in a quartz tube should be held in place using small plugs of
quartz wool so that the sample itself is in the center of the coil when the tube is inserted.
It is important to remember that the Pyroprobe electronics controls the temperature of the
filament. The actual temperature of the sample depends on sample size, chemical nature,
and additional mass such as the quartz tube in a coil probe. When using a ribbon probe,
the sample is in direct contact with the filament, but when using the coil probe, the sample
is insulated by the quartz tube. On average, the actual temperature inside the quartz tube
is approximately 100°C lower than the filament temperature.
Proper sample handling plays a very important role in achieving reproducible pyrolysis.
Best results will be obtained by using as small a sample as possible to prevent thermal
gradient effects and to insure that the sample is completely pyrolyzed. In general, optimum
temperature for pyrolysis-gas chromatography is that which is just hot enough to pyrolyze
the sample. Lower temperatures would leave unpyrolyzed material on the probe, while
hotter would produce mostly smaller fragments which may provide less information. The
temperature which provides the most useful fragments for a given sample may be deter-
mined experimentally by pyrolyzing the sample through a series of temperatures at 25 - 50
degree intervals.
It is important to remember that the Pyroprobe is being used as a sample introduction

device for the gas chromatograph and sample size should be consistent with what is gener-
ally injected onto the column. The best reproducibility will probably be obtained using
samples of 10 to 50 micrograms if the material is completely pyrolyzed, slightly more if the
sample is only partly organic or produces considerable char.
Page 5.9
ELEMENT ROD PLACEMENT
THE PYROPROBE MUST BE UNPLUGGED BEFORE ATTEMPTING TO MAKE ANY

ELECTRICAL CONNECTIONS SUCH AS REPLACING THE PROBE FILAMENT.
PROBE FILAMENTS ARE MADE OF PLATINUM WHICH IS EASILY DAMAGED. DO

NOT TOUCH THE FILAMENT WHILE REPLACING THE PROBE ROD.
If the platinum filament becomes damaged or broken, or it is desired to change from a coil
to a ribbon element, the rod containing the filament is removed from the handle. A dam-
aged rod may be discarded or returned to CDS Instruments for refurbishing.
As shown below, the handle of the probe separates into two pieces when the three screws
in it are removed. Inside the handle, the probe element rod is connected by metal screws to
electrical connections, and held steady by a bushing which matches the handle material.
To change an element rod, first unplug the Pyroprobe, then remove the three screws from
the handle. Now remove the screws attaching the probe rod to connections inside the
handle. The rod will now lift out easily, bringing the bushing with it. The connectors on the
probe element rods are configured so that they fit in one direction only. To insert the new
element, simply place it so that the connectors on the rod and those inside the handle
match, replace the screws, and reattach the handle. It is recommended that a spare ele-
ment rod always be kept with the Pyroprobe to eliminate loss of instrument use time due to
a damaged filament.
Page 5.10
USE OF PYREX TUBE FOR DESORPTION
To use the 5200 for thermal desorption from a tube instead of pyrolysis, the PEEK tubing
must be disconnected from the side of the interface zone and attached to the desorption
probe handle to provide carrier flow through the tube. The fitting on the interface zone
must be capped as shown in Figure 5.6.
The desorption tube is secured into the handle using one retainer, and then sealed into the
heater using another, as seen in Figure 5.6. Interface heat desorbes the sample from the
tube and the carrier gas transports it to the trap, where it is collected and then desorbed to
the GC during the trap desorb step.
Retainer used to seal tube into heater. Retainer used to seal tube into probe handle.
Fitting on heater tube must be capped. Tubing goes to union on handle.
FIGURE 5.6. Pyroprobe 5200 used with desorption tube.

Page 5.11
INITIAL START-UP FOR THE CDS PYROPROBE SERIES 5000
When first connecting the CDS Pyroprobe 5000 series to the PC and gas chromatograph, it
is important to verify the instrument configuration, remote start communication and that all
heated zones in the 5000 are properly installed. If any of the heated zones are not con-
nected, the 5000 will sense this condition on start-up and will not connect to the computer
for DCI control. Instead, it will indicate an error by lighting a combination of LEDs on the
front panel.
INSTRUMENT CONFIGURATION
During the initial connection betwen the Pyroprobe and the PC running the DCI software
(by clicking on COMMUNICATIONS and then CONNECT), the exact configuration of the
Pyroprobe (5000, 5150, 5200, 5250, etc.) is detected by reading the position of a series of
microswitches. After the switches have been read, the unit should be disconnected by
selecting COMMUNICATIONS then DISCONNECT. Once the information under CON-
FIGURATION in the menu has been verified (that is, the proper model and options are
checked), CONNECT should be selected again. The microswitches are pre-set at the
factory, and should not be changed in the field. The proper orientation for the
microswitches for each model of Pyroprobe is shown in the diagram below.
REMOTE START
The GC may be started by the Pyroprobe either using a switch closure or TTL. This is
selected by the position of three jumpers (J1, J2, and J3) as shown in the diagram below.
If the GC fails to start when the Pyroprobe sends the start signal, verify the remote start
requirements for the specific GC and adjust the jumpers if necessary.
ERROR CODES
When the Pyroprobe is turned on and all zones are properly connected, the green power
LED at the top of the front panel will blink. If any other condition is present, such as the
interface or transfer line not plugged in, a broken filament or short in a circuit, an error will
be indicated by lighting a combination of the LEDs instead. The Pyroprobe cannot be
connected to the PC for DCI control if any error code is displayed. The error must be
identified and rectified before the unit can be connected to the PC. A complete description
and explanation of the error codes are on the following pages.
Page 5.12
FAILURE CODES
READY LEDs
Probe (used for Open)
External (used for Shorted)
GC (used for Over Temperature)
Probe LEDs
Initial (used for interface)
Rate (used for transfer line)
Final (used for spare 5)
Accessory LEDs
Initial (used for spare 6)
Rate (used for Aux 1)
Final (Used for trap)
Clean LED
(used for probe)
In addition to displaying the operating step and ready status of the Pyroprobe, the LEDs on
the front panel are used to indicate the location of an electrical failure. Various circuits are
monitored, and will be indicated as being OPEN, SHORTED OR OVER TEMPERATURE.
In the case of a failure, then, two of the LEDs will be illuminated, one indicating the circuit
involved and one showing the specific problem.
The READY LEDs at the top of the panel are used to show the type of failure. If the circuit
is OPEN, the PROBE LED will light. If the circuit is SHORTED, then the EXTERNAL LED
will be on, and if the zone is OVER TEMPERATURE, then the GC LED will be on.
The specific circuits are indicated by the INITIAL, RATE and FINAL LEDs for both the
probe and accessory. A complete list of the locations and corresponding LEDs is on the
next page. For example, if the transfer line had shorted, the PROBE RATE and EXTER-
NAL LEDs would both be lighted. If the CLEAN LED and the PROBE LED are both on,
then the Pyroprobe filament circuit is open, probably indicating a broken filament.
NOTE: An OPEN circuit message may just mean that a heated zone, such as the 1500
interface for the Model 5000, is not plugged in, or is plugged in to the wrong socket. Verify
that all heaters are properly connected, especially at initial set-up, before turning the
Pyroprobe on.
Page 5.13
FAILURE CODE LIST
EXT LED means SHORTED

PROBE LED means OPEN
GC LED means OVER TEMPERATURE
CHANNEL CIRCUIT LED USED
1 Spare 5 Probe final

2 Transfer line Probe rate
3 Programmed interface Probe initial
4 Trap Accessory final
5 Auxiliary 1 Accessory rate
6 Spare 6 Accessory initial
7 MFC 1 Dry
8 Probe actual Clean
LED COMBINATIONS
LEDS LIGHTED CONDITION

Probe Ready and Clean Probe is OPEN
Probe Final and

Probe Ready Spare 5 is Open
GC Spare 5 is Over temperature
Probe Rate and

External Transfer line is Shorted
Probe Ready Transfer line is Open
GC Transfer line is Over Temperature
Probe Initial and

External 5150 Interface is Shorted
Probe Ready 5150 Interface is Open
GC 5150 Interface is Over Temperature
Accessory Final and

External Trap is Shorted
Probe Trap is Open
GC Trap is Over Temperature
Accessory Rate and

External Auxiliary 1 is Shorted
Probe Auxiliary 1 is Open
GC Auxiliary 1 is Over Temperature
Accessory Initial and

Probe Spare 6 is Open
GC Spare 6 is Over Temperature
DIAGRAMS SHOWING THE LEDS LIGHTED FOR EACH CASE ARE ON THE FOLLOWING
PAGES.
Page 5.14
Probe Front Panel Error Display
READY
STATUS
PWR/ PROBE
COM
EXT. GC
SYSTEM CYCLE
PYROPROBE
FINAL
RATE
INITIAL
FINAL
RATE
INITIAL
ACCESSORY
DRY START
Hold
CLEAN RESET
RGO/AS CLEAN
DRY
CLEAN
Probe is Open
Interface Front Panel Error Display
READY READY READY

STATUS STATUS STATUS
PWR/ PROBE PWR/ PROBE PWR/ PROBE
COM COM COM
EXT. GC EXT. GC EXT. GC
SYSTEM CYCLE SYSTEM CYCLE SYSTEM CYCLE

PYROPROBE PYROPROBE PYROPROBE
FINAL FINAL FINAL
RATE RATE RATE
INITIAL INITIAL INITIAL
FINAL FINAL FINAL
RATE RATE RATE
ACCESSORY ACCESSORY ACCESSORY
DRY START DRY START DRY START
Hold Hold Hold

CLEAN RESET CLEAN RESET CLEAN RESET
RGO/AS CLEAN RGO/AS CLEAN RGO/AS CLEAN
DRY DRY DRY

CLEAN CLEAN CLEAN
Interface Zone is Shorted Interface Zone is Open Interface Zone is Overtemp.

Page 5.15
Transfer Line Zone Front Panel Error Display
READY READY READY

COM COM COM

FINAL FINAL FINAL

RATE RATE RATE
FINAL FINAL FINAL
RATE RATE RATE
Hold Hold Hold

DRY DRY DRY

CLEAN CLEAN CLEAN
Transfer Line Zone is Shorted Transfer Line Zone is Open Transfer Line Zone is Overtemp
Trap Zone Front Panel Error Display
READY READY READY

COM COM COM

FINAL FINAL FINAL
RATE RATE RATE
FINAL FINAL FINAL
RATE RATE RATE
Hold Hold Hold

DRY DRY DRY

CLEAN CLEAN CLEAN
Trap Zone is Shorted Trap Zone is Open Trap Zone is Overtemp.

Aux. 1 Zone Front Panel Error Display
Page 5.16
READY READY READY

COM COM COM

FINAL FINAL FINAL

RATE RATE RATE
FINAL FINAL FINAL
RATE RATE RATE
Hold Hold Hold

DRY DRY DRY

CLEAN CLEAN CLEAN
Aux. 1 Zone is Shorted Aux. 1 Zone is Open Aux. 1 Zone is Overtemp.
Temperature Zone 5 Front Panel Error Display
READY READY READY

COM COM COM

FINAL FINAL FINAL
RATE RATE RATE
FINAL FINAL FINAL
RATE RATE RATE
Hold Hold Hold

DRY DRY DRY

CLEAN CLEAN CLEAN
Spare Temperature Zone 5 Open Spare Temperature Zone 5 Shorted Spare Temperature Zone 5 Over Temp.
Page 5.17
Temperature Zone 6 Front Panel Error Display
READY READY READY

COM COM COM

FINAL FINAL FINAL

RATE RATE RATE
FINAL FINAL FINAL
RATE RATE RATE
Hold Hold Hold

DRY DRY DRY

CLEAN CLEAN CLEAN
Spare Temperature Zone 6 is Shorted Spare Temperature Zone 6 is Open Spare Temperature Zone 6 is Overtemp.
Page 5.18
TEST TUBE DESORBER
For analyzing larger samples in the trapping mode, the Pyroprobe interface zone may be
removed and replaced with the test tube desorber. Just as with the Pyrex desorption
tubes, the sample is heated in the desorber and the volatiles produced are transferred to
the trap for collection using the purge gas of the 5200. With the test tube desorber, the
purge gas is connected to a tube that goes into the test tube from the top. Purged
analytes travel out the bottom of the desorber into the valve oven of the 5200, then to the
sorbent trap on the right side of the 5200. The height of the purge tube in the test tube
desorber is adjustable by loosening the 1/8” fitting on the top of the desorber.
The test tube desorber plugs into the same socket used for the Pyroprobe interface zone
heater. PEEK tubing is used to bring the Pyroprobe purge gas from the 1/16” bulkhead on
the 5200 (the left bulkhead of the two) to the purge tube of the test tube deosrber using a
Swagelok union. When using the test tube deosrber, neither the standard 1/4” desorption
probe or the Pyroprobe filament rod are used. The Pyroprobe filament should be placed in
the holder on the 5200 and probe temperatures all set to 0°C when using the test tube
desorber.
Union for purge gas
Desorber cover
Thumb wheel
Heater plug for desorber

Plugs into the desorber
heater socket.
Purge flow connects the top of the

test tube deosorber to the
purge flow bulkhead.
FIGURE 5.7. Test tube desorber connected to the 5200 valve oven.
Page 5.19
Test tube desorber purge assembly

PEEK tubing from the 5200 purge flow
Collar
Reducing union (5 micron filter)
Height adjustment fitting
O-ring
Purge tube
Test tube
FIGURE 5.8. Purge tube inside test tube with sealing assembly.
To install the test tube deosrber, turn the Pyroprobe 5200 off and allow heated zones to
cool. Then remove the interface tube from the left side (see Figure 5.3), remove and
unplug the interface heater. The exit tubing of the test tube desorber is connected to the
valve oven using the same thumb wheel and ferrule that were used for the Pyroprobe
interface tube (see Figure 5.9). Plug the test tube desorber into the interface heater
socket.
The cap of the test tube desorber seals using an O-ring and collar. The test tube goes
completely inside the heater, then the cap with the purge tube is sealed on top. The depth
of the purge tube into the test tube may be adjusted using the height adjustment fitting (see
Figure 5.8).
Page 5.20
Exit of desorber connects

to the valve oven using the
thumb wheel on the left
(desorber) side.
FIGURE 5.9. Test tube desorber with cover removed.
VOST TUBE DESORBER
In addition to the standard 1/4” desorption tubes and the test tube desorber, the 5200 may
be equipped to perform desorption of large (“VOST”) tubes, which are wider and longer
than the standard tubes. A specific heater is required for these tubes, which plugs into the
5200 as the test tube deosrber does, and connects using the standard thumb wheels of the
5200. Since the VOST tube is longer than a standard tube, the heater is longer, and the
thumb wheel assembly is moved toward the front of the unit (see Figure 5.10). The heater
fits into slots, and is held in place by the bracket which includes springs. To remove the
heater, the bracket may be moved back, compressing the springs. Instruments which
include the VOST tube desorber option are shipped with an additional mounting bracket for
this application. Switching the 5200 from Pyrolysis mode, to Trapping mode to VOST tube
mode requires changing to the appropriate mounting bracket.
NOTE: When using the VOST tube deosrber, neither the standard 1/4” desorption probe or
the Pyroprobe filament rod are used. The Pyroprobe filament rod must be connected,
however, and should be placed in the holder on the 5200 with probe temperatures all set to
0°C.
Page 5.21
Cover
Heater
Thumb wheel
Rear bracket
Springs
Heater plug
FIGURE 5.10. VOST tube desorber assembly with thumb wheel moved forward to
accomodate longer tube.
FIGURE 5.11. VOST tube desorber with cover removed.

Page 6.1
SECTION 6. PYROPROBE INSTALLATION AND GC INTERFACING
MODEL 1500 GC INTERFACE

INTRODUCTION
The CDS Analytical Pyroprobe 1500 is a valved interface which connects the CDS Pyroprobe
to the inlet of a gas chromatograph. The 1500 includes a valve which permits the user to place
the pyrolysis zone on-line or off-line from the GC injection port. This allows the user to insert
and remove the probe while the GC oven is programming, without disturbing the GC column
flow. With the valve in the LOAD or OFF-LINE position, GC carrier goes directly to the injection
port, bypassing the Pyroprobe entirely. The 1500 includes a separate interface purge flow
which purges the interface zone to vent when the 1500 is off-line from the GC. When the 1500
is placed in the RUN or ON-LINE position, GC carrier is directed through the interface zone to
sweep the pyrolysate onto the GC column.
The 1500 is compatible with packed, wide-bore and narrow-bore capillary columns. When
performing split capillary analysis, the GC injection port pneumatics are used in the standard
way, that is, the injection port pressure or flow and the split flow are all set using the GC injection
port controls as usual.
The temperature of the pyrolysis interface zone and the valve are controlled by the interface
heater control of the Pyroprobe controller. The 1500 connects to the Pyroprobe 5000 controller
by use of a round 7-pin connector, and the setpoint and actual temperatures are displayed on
the Pyroprobe control software Accessory screen.
DESCRIPTION
The CDS 1500 Pyroprobe interface is designed to sit directly above the injection port of the
gas chromatograph, with flow to the GC exiting the bottom of the 1500. With the 1500 oriented
so that the probe enters the front, pneumatic connections and the valve rotation knob are found
on the left side of the interface, which includes two bulkheads for flow connection, the valve knob
and a vent. The two bulkheads are for bringing in GC carrier gas to the valve oven and interface
purge flow. The GC carrier always exits the interface to the injection port, regardless of the
valve position, and the purge flow always exits the vent. The electrical cable to connect the
1500 to the Pyroprobe 5000 controller is found on the rear of the interface.
Page 6.2
Both the valve and the pyrolysis zone are located inside a heated valve oven which is controlled
by the Pyroprobe accessory heater control. Therefore, there is only one connector to attach
to the Pyroprobe 5000 controller, and the temperature for the Pyroprobe interface and the valve
are the same. The electrical cable from the 1500 plugs into the seven-pin socket on the rear
of the 5000 controller labeled AUX HEATER, below the connector marked TRANSFER LINE,
(which is not used in the model 5000) as shown in Figure 6.12.
As with any pyrolysis interface, the 1500 must be inserted pneumatically into the carrier stream
of the GC. This requires connection of the GC carrier to the inlet bulkhead of the 1500 instead
of directly to the injection port of the GC. In addition, another flow, the interface purge, is
connected to permit purging the interface before placing it on-line with the column, and baking
the interface to vent between runs. A “T” fitting and metering valve are provided to permit the
user to add this purge flow to the system.
When properly connected, the left side of the 1500 interface looks like the diagram in the figure
below.
FIGURE 6.1. 1500 interface diagram.

Page 6.3
INSTALLATION
To transfer the pyrolysis products for analysis, the 1500 Interface must be connected
pneumatically to the gas chromatograph. This requires disconnecting the GC carrier flow into
the injection port and connecting it instead to the 1500 interface. The inlet to the injection port
must be capped to prevent all flow from leaking out where the carrier was disconnected. For
convenience, a diverter valve may be installed to permit directing the GC flow either to the1500
interace or back to the injection port (see page 6.11).
When the 1500 is installed, the GC carrier flow is connected to the on-line, off-line valve, which
permits directing flow either to the interface zone of the Pyroprobe and then to the GC, or
straight to the injection port (in the Load position).
Flow is connected from the valve to the injection port using a union inside the valve oven of the
1500, which connects to a tubing assembly held in place by the GC septum retainer. This
permits positioning of the 1500 close to the injection port and the elimination of a cold spot. The
union inside the 1500 attaches to a piece of 1/8" stainless steel tubing which is connected to
the injection port by the septum retainer, as shown in the diagram on the next page. All flow into
the GC injection port goes through this 1/8" tubing, whether the system is being used split or
not. The capillary GC column is brought up through the injection port and into this 1/8" tube. In
operation, the carrier flow which exits the splitter vent goes through the tube around the outside
of the capillary column, into the injection port and out the split vent while the analytical flow goes
through the capillary column. Alternatively, the 1500 interface may be installed using a
traditional needle assembly. In this case, flow goes through the septum via a needle, and the
GC column is left installed in the injector as for standard syringe injections.
MOUNTING TRAY
On some models of gas chromatographs, the tray around the injection ports is too small to
accommodate the 1500 interface. Mounting the 1500 above the tray would produce a cold
spot between the interface and the injection port. To eliminate this problem, CDS Analytical
provides a replacement tray designed with a larger area to permit installation of the interface
directly on top of the injection port. When installing the 1500 therefore, the existing injection port
tray should be removed from the GC and replaced with the new one supplied by CDS
Analytical.
The 1500 is mounted onto the tray using three alignment pins - two on the left or valve knob side
and one on the right side. The interface fits down over the two pins on the left side, and the single
pin on the right screws into the tray through the cabinet of the 1500 as a locking pin. The
replacement tray includes multiple positions for the alignment pins so that the 1500 may be
installed in three orientations - with the probe entering from the front (A) or from the left side (B)
on the front injection port, or from the left side (C) on the rear injection port. The replacement
tray is shown on page 6.6 , which also shows the placement of the alignment pins used to place
the 1550 in position A, B or C. On the diagram, the locking pin is designated with the letter L,
so for position A, pins would be placed in two holes marked A and the locking pin in the position
marked AL.
Page 6.4
CDS ANALYTICAL 1500 INSTALLED ON GC INJECTION PORT

Schematic as seen from the right, with probe inlet (front) to the left.
1500 cabinet
Valve
Purge flow Union connecting valve to

1/8" tubing of septum
retainer adapter, with or
without needle
Probe inlet
Septum retainer adapter
GC septum retainer
"T" fitting
Split vent
GC carrier flow disconnected from
injection port and connected to 1500 Injection port
Capillary column
GC carrier inlet plugged
FIGURE 6.2. Pneumatic configuration.

Page 6.5
INSTALLATION INSTRUCTIONS
BOTH THE GAS CHROMATOGRAPH INJECTION PORT AND THE PYROPROBE

INTERFACE ARE HOT WHEN IN USE. ALLOW THESE PARTS TO COOL BEFORE
HANDLING, INSTALLING OR REMOVING INTERFACE.
Installing the 1500 interface involves three steps:
A. Bringing GC carrier flow into the 1500 instead of directly to the injection port;
B. Adding the adapter to the septum retainer; and
C. Connecting the 1500 to the septum retainer adapter.
A. GC Carrier Flow
1. Disconnect the tubing which goes from the helium filter to the carrier IN position
of the injection port.
2. Cap the end of the tubing connected to the injection port so that flow will not exit
here instead of going to the column. Be sure to use a Vespel ferrule at this plug so that it may
be removed later if it is desired to restore the GC pneumatics to their original configuration.
Alternatively, installing a diverter valve permits switching between the 1500 and using the
injection port as usual, as shown on page 6.11.
3. Attach the 1/16" tubing provided to the outlet fitting of the helium filter.
4. Attach the other end of this tubing to the bulkhead on the 1500 marked Carrier
IN. Now the GC flow or pressure controller is supplying flow into the 1500 instead of into the
injection port of the GC.
5. Install the “T” fitting provided in the helium inlet line to provide purge flow for the
1500.
6. Connect one leg of the “T” to the original helium inlet for the GC to maintain flow
for the GC pneumatics.
7. Connect the tubing for the purge flow metering valve to the other leg of the “T”.
8. Connect the tubing out from the purge flow metering valve to the 1500 bulkhead
fitting marked purge in and secure the metering valve with the supplied bracket to a convenient
position.
Page 6.6
FIGURE 6.3. Mounting for 5890GC.

Page 6.7
MOUNTING PLATE FOR AGILENT 6890
The mounting plate for the Agilent 6890 gas chromatograph attaches to the top tray di-
rectly, using stand-off screws as shown in Figure 6.4. The circular cutout for the septum
retainer adapter should be placed directly over the septum retainer of the injection port to
be used. The mounting plate has two pins and a lock-down screw for stabilizing the 1500
during use. After the mounting plate has been attached to the GC with the pins and lock-
down screw facing up, the 1500 is positioned on top of the plate as shown in Figure 6.4.
The pins align with two holes in the base of the 1500 itself, and the lock-down screw
projects through a hole on the right side of the base, inside the insulated cover. The 1500
is stabilized by attacheing a nut to the lock-down screw, securing it to the mounting plate.
Front of 6890 Septum retainer 1500 mounting plate
Pin
Lock-down screw to fasten 1500 to plate
Stand-off for attaching plate to GC
Lock-down screw to fasten 1500 to plate
FIGURE 6.4. Mounting for Agilent 6890 GC.

Page 6.8
FIGURE 6.5. Pneumatic connection for Clarus 5000.

Page 6.9
B. Adapting the septum retainer
1. Remove the septum retainer and septum from the injection port.
2. Insert the 1/8" tubing of the septum retainer adapter through the septum retainer
so that it protrudes above the top. It may be necessary to enlarge the needle hole in the septum
retainer using a 1/8" drill bit to permit passing the tubing through. All of the tubing should be
above the septum retainer so that the flat disk at the bottom of the adapter contacts the inside
of the septum retainer.
3. Place an o-ring against the flat disk of the adapter so that it is sealed into the
injection port septum well with the adapter on top of it, held in place by the septum retainer, as
shown in the diagram below. The 1/8" tubing will protrude up from the injection port, and the
1500 will be attached to the injection port using this tubing.
NOTE: The 1500 interface may be installed using a needle assembly instead of the tube with
no needle. For this installation, the fitting from the valve still connects to the top of the 1/8" tubing,
but a septum is used with the needle instead of an o-ring. (see figure on page 6.4)
FIGURE 6.6.
Page 6.10
C. Connecting the 1500
1. Decide which orientation (A, B or C) will be used, and screw in the two alignment
pins for the valve knob side of the 1500.
2. Remove the top cover of the 1500 and place the interface over the two alignment
pins so that the 1/8" tubing of the septum retainer adapter passes through the channel and into
the valve area of the 1500.
3. Screw in the third alignment pin, through the corresponding hole in the base of
the 1500, locking the 1500 into place on the mounting tray.
4. If it has not yet been done, attach the carrier flow and purge flow to the
corresponding bulkhead fittings on the 1500.
5. Remove the insulation covering the valve area of the 1500. Bring the inlet of the
capillary column up through the injection port (removing the liner if necessary) and through the
adapter tubing so that it is even with the end of the tubing.
6. Attach the 1/16" tubing from the valve to the adapter tubing using the reducing
union provided.
7. Replace the insulation covering the valve, then the cover, securing it with the
screw at the top.
8. Plug the electrical connection for the 1500 into the AUX heater position on the
back of the Pyroprobe controller (see Figure 6.12).
OPERATION
With the 1500 installed, the Pyroprobe filament rod is inserted into the probe inlet and sealed
in place with the seal in the probe collar.
It is recommended to keep the valve in the OFF-LINE or LOAD position except when actually
making a run. This keeps flow going directly to the injection port, and therefore the column,
while purging the interface area to vent. After a sample has been placed on the ribbon or inside
the coil, insert the probe into the probe inlet and seal. Allow a short time for the air in the system
to be purged out the vent, then turn the valve to the ON-LINE or RUN position. Now the probe
is on-line with the GC column. When the Pyroprobe START key is pressed, the sample is
pyrolyzed, and the pyrolysate is carried through the valve to the column inlet, and onto the
column. After the sample has been pyrolyzed, the valve may be turned to the OFF-LINE
position and the probe removed for cleaning and preparing the next sample.
Page 6.11
INSTALLATION WITH DIVERTER
The installation of a diverter valve on the GC carrier flow line simplifies converting the GC from
use with the Pyroprobe interface back to the standard injection port. As shown below, the
carrier gas may be directed to the interface in one position of the diverter valve, or back to the
injection port in the other direction. Converting the GC back to standard operation, then, only
requires removing the interface needle adapter, replacing the standard injection port septum
retainer, and turning the diverter valve to the GC direction.
HP 5890/6890 SPLIT/SPLITLESS INJECTOR

INJMOD
NEEDLE OR NEEDLELESS CONNECTION
OPTIONAL:
IDENTIFY INLET OUTLET LINES MODIFY LINES TO ADD IN CDS INTERFACE ADD 3 WAY DIVERTER FOR CONVENIENCE
SEPTUM PURGE LINE SEPTUM PURGE LINE SEPTUM PURGE LINE
SPLIT FLOW LINE SPLIT FLOW LINE SPLIT FLOW LINE

EL
EL
EL
AG
AG
AG
SW
SW
SW
FLAT SIDE FLAT SIDE

CUT SEVERAL INCHES FROM
THE INJECTION PORT
> 2 INCHES FLAT SIDE
FLOW
EL
FLOW
AG
SW
ROUTE TO "GC CARRIER INPUT"

SWAGEL
ON "CDS" DEVICE BEING ADDED

SWAGEL
SWAGEL
CAP THIS END

INLET IS FLAT SIDE OF NUT
(ACTUALORIENTATION
M A Y VARY) ADD 1/16" UNION SWAGEL
TOTAL FLOW LINE

3 WAY
SWAGEL
ROUTE TO "GC CARRIER INPUT" DIVERTER
SWAGEL
SWAGEL
SWAGEL
ON "CDS" DEVICE BEING ADDED
X4
CDS PART NUMBER
FLAT SIDE 3 WAY BRASS DIVERTER 2460-0032
FIGURE 6.7.
Page 6.12
INSERTS AND LINERS
Glass Insert Tube
It is not necessary to remove the 1500 interface from the GC to make syringe injections of
liquid standards. The 1500 comes equipped with a septum retainer which attaches to the
probe inlet for this purpose. To reduce dead volume in the 1500 interface when making
syringe injections, a glass insert is placed into the interface (instead of the Pyroprobe) and
the opening is capped with the septum retainer. This glass insert is thick-walled, with just a
narrow passage in the center for the syringe needle. As with pyrolysis, the valve must be in
the RUN position when making syinge injections to the GC.
USING THE 5000 WITH A CDS 8000 SAMPLE CONCENTRATOR
The Probe of the Pyroprobe 5000 is configured to be compatible with the thermal desorber of
the CDS 8000 Sample Concentrator. This permits the trapping of volatiles resulting from
programmed heating rates, and the use of air as a carrier gas with the reactant gas feature of
the 8000. When using the 8000 instead of the interface accessory of the Pyroprobe, the 5000
filament is still controlled by the software of the 5000, which means that the 8000 will start the
interface program of the 5000, and the probe will still fire at interface final. Therefore it is still
necessary to enter an interface or accessory final time longer than the total Pyroprobe time for
the probe to fire. In addition, if the accessory or interface of the 5000 has been unpluggged
from the unit, a replacement or "dummy" plug must be used in order to get a "ready" for the
5000. The dummy plug generates an actual temperature for the accessory, and the setpoint
temperature must be set to equal that "actual" temperature for the probe to fire.
Page 6.13
PYROPROBE 5150 AND 5200 INTERFACING

HEATED TRANSFER LINE
The Pyroprobe Models 5150 and 5200 incorporate a low mass, programmable interface
zone for the probe into the body of the Pyroprobe itself. The on-line/off-line valve is housed
in a separate valve oven, also part of the Pyroprobe unit. Connection to the gas chromato-
graph is made via a heated transfer line. The valve oven and the transfer line are separate
isothermal zones controlled through the isothermal window of the Pyroprobe control soft-
ware, while the interface zone for the probe is programmable and is controlled using the
accessory programming window of the Pyroprobe.
The on-line/off-line valve of the 5150 or 5200 is controlled automatically by the Pyroprobe.
The sample (or trap) is placed on-line with the GC during the interface (accessory) RAMP
step (or trap heating step). This permits pre-treatment of the sample to vent during the
initial step, if desired. To have the sample pyrolyzed without pre-treatment, simply enter the
same temperature for both the initial and final steps of the accessory, with a 0 time for the
initial. In this case, the Pyroprobe will go directly into Accessory Final, rotate the valve and
fire the probe. To permit equilibration of the GC carrier gas, there is a 10 second delay
after rotating the valve before the Pyroprobe filament is heated. The GC start signal is sent
when the probe is heated.
Connection to the GC is made using a heated transfer line which terminates with a needle
that goes through the septum of the GC. The standard transfer line uses tubing which is
attached to the injection port with a needle adapter (in the same way as the 1500, shown
on page 6.9). The union used to connect the tubing to the needle assembly goes up into
the socket of the transfer line to keep it hot in use, as shown on page 6.15.
A quick connection transfer line is also available, which has the needle already attached. In
use, the needle of this transfer line is just pushed through the GC septum to make the
connection. The end of the transfer line at the GC is stabilized using two screws to secure
it to the GC injection port as shown in Figure 6.10. When inserting the quick conect trans-
fer line, turn the diverter valve so that GC carrier flow is going through the transfer line
before inserting the needle through the septum. This will help prevent coring the septum
and plugging the needle.
As with the 1500 interface, the 5150 and 5200 require connection of the GC carrier gas to
the valve oven of the Pyroprobe to transfer the pyrolysate from the probe (or trap of the
5200) to the GC injector (see Figure 6.6 on page 6.9, and Figure 6.7). Figure 6.8. is a
diagram of how the GC pneumatics should be modified to direct carrier flow to the
Pyroprobe and then back the the GC through the transfer line. A separate connection is
provided for purge gas in the Pyroprobe, which is controlled by the flow controller on the
front of the unit. This gas purges the interface zone to vent when the unit is off-line and
transfers analytes from the probe to the trap in the 5200.
Page 6.14
FIGURE 6.8. Typical pneumatics of GC (top), and modified to connect the Pyroprobe
transfer line using a diverter valve (bottom).
Page 6.15
Transfer line
Diverter valve
Socket for union
Transfer tubing
Union
1/8" tubing of needle adapter
Septum cap
Needle
FIGURE 6.9. Standard transfer line with needle adapter.

Page 6.16
Transfer line from 5150
Cup goes over septum retainer
Needle goes through septum
Retaining screws secure the transfer line to the septum cap.
FIGURE 6.10. Quick connect transfer line at GC injection port.

Page 6.17
5150 AND 5200 MODULES
The 5150 and 5200 are shipped with the interface or pneumatic section removed from the
electronics section. To assemble, the interfacing section, which includes the valve, must
be placed onto the main unit, aligned with two pins and locked with a screw. Depending on
the model, up to four electrical connections must be made, two for the heaters, one for the
fan (2 pins) and one for the valve actuator (4 pins).
Valve oven Electronic module
Interface module
Alignment pins Holes for alignment

Pins
Connectors
Tube heater
Fan
Interface heater
Valve
Threaded hole for screw
FIGURE 6.11. 5200 Modules.

Page 6.18
To assemble, place the pneumatics module onto the base, plug in the cables, align the top
using the two pins at the rear, and secure using the screw on the side, as shown in Figure
6.11. The interface module must be plugged into the rear of the unit, and the purge gas
connected from the base to the side fitting, marked Purge.
Purge Gas
from base
Carrier from
GC IN
Securing screw
Pneumatic
Connection for
Transfer Line Reactant Gas IN
Transfer line socket
AUX Connector Purge gas

For Interface From base
Module To interface
Or 1500 Interface
For Model 5000
Purge, and
carrier to the
trap of the
5200 IN
FIGURE 6.12 Assembled 5200

Page 6.19
INSTALLATION TO GC OF 5150 OR 5200
1. Install the Swagelok diverter as shown in Figure 6.7 on Page 6.11.
2. Connect the GC Carrier from the diverter to the 1/16 inch bulkhead on the side of the
5150or 5200 marked GC, shown in Figure 6.12.
3. Connect a supply of purge gas (Helium, 100 psi maximum) to the 1/8 inch bulkhead
marked CARRIER IN on the rear of the 5200,or to the 1/16" fitting on the side of the
5150 marked SAMPLE PURGE.
4. Attach the 5150 or 5200 end of the transfer line inside the valve oven of the Pyroprobe
using the 1/16" Swagelok nut, a Vespel ferrule and the bulkhead fitting on the L-
bracket to the left of the valve (see Figure 6.12).
5. Place the GC end of the transfer line (with the needle) through the septum of the GC
(Figure 6.10), or install the standard needle assembly as shown in Figure 6.9.
CAUTION! The needle is permanently attached and sharp. Handle carefully.
6. Slide the GC end of the transfer line all the way down so that the recessed cup fits over
the septum retainer.
GC flow and pressure are adjusted at the GC as for any other analysis. The 5150 is just
inserted as a sample delivery loop upstream of the column. Purge gas should be set with
the flow controller to 10 - 20 ml/minute, measured at the vent on the front of the 5150.
Valve oven
Purge flow Purge flow

Control
GC flow IN
Carrier gas
Tubing
FIGURE 6.13. Pyroprobe 5150, side view.

Page 6.20
ELECTRICAL CONNECTIONS
Electrical connections to the 5150 are made on the rear of the unit, as shown in Figure
6.14. The valve oven and transfer lines must be plugged into the corresponding sockets.
Remote start connections are made at the upper connector. The serial cable from the
computer to the 5150 attaches to the right of the main power switch. The main power fuse
for the unit is located inside of the power entry module. On the right hand side of the 5150
rear panel is an additional fuse for the supply voltage of the filament itself.
Replacing Fuses
The fuse holder of the power entry module is removed by opening the black cover of the
module, which is hinged at the bottom (see Figure 6.15). The fuses slide into the sides of
the fuse holder, which is then reinserted into the cavity of the entry module. The fuses must
be inserted toward the rear of the holder, as shown in Figure 6.15 and the holder replaced
with the two blades at the top.
CAUTION: Disconnect the instrument from its power source before removing the cover
for access to fuses.
Individual zone fuses are located inside the electronics cabinet of the Pyroprobe, arranged
as shown in the diagram below.
NOTE: Fuse number and locations depend on specific Pyroprobe model according to the
following chart.
Model F1 F2 F3 F4 F5 F6 F7 F8
220v 115 v
5000 2A 4A 2A
5150 2A 4A 2A 2A
5200 2A 4A 2A 2A 0.5A 2A
R11 R14 R17 R20 R23 R26
R5 R8
U1 U2 U3 U4 U5 U6
R9 R12 R15 R18 R21 R24
J1
J3
TR3 TR4 TR5 TR6 TR7 TR8
U7 U9
R3 R6
TP1
SEE JUMPERS
E1
TR1 TR2 R10 R13 R16 R19 R22 R25
J2 R1
! F1 ! F2 ! F3 ! F4 ! F5 ! F6 ! F7 ! F8
E2
R4 R7 K1
D1
U9
!
C1 E3 REFER TO MANUAL FOR
FUSE VALUES AND TYPES
Q1
J4 R2
L2 L1
WARNING: DANGEROUS VOLTAGES N H
DISCONNECT AC POWER CORD
BEFORE SERVICING
CDS ANALYTICAL,
INC. 6A0053 J5 J6
Page 6.21
Remote I/O
For remote start
Transfer line
Valve oven
Computer connection
Power entry Primary and

With main fuse Secondary
Fuses for
Filament
Power
FIGURE 6.14. Rear of 5150.
Two blades - TOP
Cover, opens from the top Fuse holder Fuse
FIGURE 6.15. Fuse holder in power entry module.

Page 6.22
MODEL 5200
PY-GC MODE (REST / LOAD / ACC. INITIAL)
(PURGINGTO VENT)
TIC TAH TAHH
GC CARRIERIN (HEATEDOVEN C H A M B E R )
TALL
RTD
TO GC
REACTANTGAS OPTION
(FRONTPANEL) 3 4
CARRIERIN 2 5
1/8"
1 6
8 7
REACTANTGAS SV-1 SAMPLEPURGE
TIC TAH TAHH
TALL
VALVE OVEN
RTD
TAHH TAHH
SWAGEL
TALL
(LEFT SIDE PANEL) (FRONTPANEL) TALL
TAH
TAH
SAMPLEVENT
STATUS
L E G AWS
MPV1 ENERGIZED TIC

TIC
INTERFACE REST
PROBE IDLE
TRAP REST TEMP RTD RTD
INTERFACE
TRAP
REACTANTGAS OPTION
PROBE
SV-1 DEENERGIZED
MODEL 5200
PY-GC MODE (RUNNING / ACC. RAMP)
TIC TAH TAHH
GC CARRIER IN (HEATEDOVEN CHAMBER)

TALL
RTD
TO GC
REACTANT GAS OPTION

(FRONT PANEL) 3 4
CARRIER IN 2 5
1/8"
1 6
8 7
REACTANT GAS SV-1 SAMPLE PURGE
TIC TAH TAHH
TALL
VALVE OVEN
RTD
TAHH TAHH
SWAGEL
(LEFT SIDE PANEL) TALL

(FRONT PANEL) TALL
TAH TAH
SAMPLE VENT
STATUS
L E G AWS
MPV1 DE-ENERGIZED TIC

TIC
INTERFACE RUNNING PROGRAM
PROBE RUNNING PROGRAM RTD RTD
TRAP REST TEMP

INTERFACE
TRAP
REACTANT GAS OPTION
PROBE
SV-1 DE-ENERGIZED
FIGURE 6.16. Flow diagrams.

Page 6.23
Cryogenic Option
The CDS 5150 and 5200 may be equipped to provide subambient temperatures using liquid
nitrogen as a cryogenic fluid. The cryogen is supplied by a suitable liquid nitrogen tank at
the 1/4” bulkhead on the cryogenic module of the Pyroprobe. The cryogenic focusing option
allows for sample refocusing at the GC injection port, while the cryogenic trapping option permits
use of the trap at subambient temperatures.
NOTE: When using the cryogenic option, provide appropriate ventilation for
the nitrogen gas which can displace oxygen in the room air.
Cryogenic temperature set points are selectable in 1oC increments. To select a temperature
setpoint below 0oC, use the negative (-) key before entering numeric values. When the CDS
Pyroprobe is equipped with the cryogenic option, additional parameters are used when
generating operating methods. Three temperatures are used with the cryogenic options, REST,
INITIAL, and FINAL. The REST parameter is active between runs and allows the cooled zone
to heat to ambient (or higher) temperatures when the instrument is idling. This prevents exces
sive amounts of liquid nitrogen coolant from being consumed when the unit is inactive. The
INITIAL temperature is the actual subambient value needed for the method. This is the tempera-
ture at which the analytes are focused before starting the GC run. The FINAL temperature is the
GC injection temperature when using cryogenic focusing.
Cryogenic focusing at the GC injection port is useful with narrow bore capillary columns. When
the adsorbed sample is backflushed and desorbed from the trap of the 5200 to the GC, the trap is
on-line with the GC column, and sample transfer takes place at the GC carrier flow rate. Using
normal split ratios, or sufficiently wide-bore capillary columns, enough flow is usually maintained
to transfer the analytes efficiently. When the Pyroprobe is interfaced with a narrow-bore splitless
capillary, GC carrier flow may be as low as 1 ml/min. Pyrolysis, sample desorption or desorption
from the trap at such low flow rates causes peak broadening. Cryogenic focusing helps maintain
peak shape integrity when these low flows are used.
The CDS Cryogenic Focuser installs on the injection port of the GC and provides a focusing
zone to recollect the organic analytes. Cryogenic focusing may be done on a piece of uncoated
fused silica (which is attached to the capillary column inside the GC oven), or directly onto the
column itself. Because of its unique design, the CDS cryogenic focuser still permits pyrolysis to
the GC in the normal split mode when cryogenic focusing is not required. When the cryogenic
focuser is disabled, and at transfer line temperature, and the GC injection port splitter is open,
sample flow passes through the transfer line of the Pyroprobe to the tip of the fused silica
column in the focuser (see Figure 6.17 ). With the split vent open, most of the carier gas
passes around the column, through the 1/8" stainless steel adapter tubing and out the injection
port vent. The analytical flow proceeds through the column as usual for a split capillary injection,
but the split point is now inside the fitting at the top of the cryogenic focuser instead
of inside the insert of the injection port. For true splitless analyses, with cryogenic refocusing, the
split vent is closed and the cryogenic focuser is cooled before sample transfer. In this case, all
of the flow from the transfer line passes through the fused silica tubing, where the analytes
are collected, then revaporized by heating at the beginning of the GC run.
Page 6.24
Installation of the Cryogenic refocuser
Cryogenic refocusing with the Pyroprobe requires a tank of liqiud nitrogen, the cryogenic
focuser, and a cryogenic fluid control solenoid valve. The cryogenic focuser is mounted
directly onto the injection port of the GC, with the cryogenic fluid solenoid box located no more
than 12 inches away from it. Liqiud nitrogen flows from the tank to the solenoid box IN fitting,
then from the solenoid OUT fitting to the focuser IN fitting. In use, nitrogen gas is then vented
from the cryogenic focuser from the Out fitting. Because large amounts of nitrogen gas are
produced as the liquid nitrogen vaporizes, the cryogenic focuser Out fitting must be vented
away from the room (through a hood or other suitable vent) to prevent displacement of
oxygen in the room. CDS supplies insulated tubing and all the necessary fittings to connect
the liquid nitrogen from the tank to the solenoid, from the solenoid to the cryogenic focuser and
from the focuser to a vent.
The cryogenic refocuser is positioned on the injection port of the GC using the cryogenic
adapter, as shown in Figure 6.17. When using the cryogenic focuser, therefore, the adapter
does not have a needle on the bottom (as the universal needle adapter does) but is open to
permit the fused silica tubing to pass through it to the fitting at the top of the refocuser. To install
the cryogenic refocuser, the adapter is attached to the GC injection port using the septum re-
tainer, as shown in Figures 6.18 to 6.21. The adapter is a piece of 1/8" stainless steel
tubing which extends all the way through the cryogenic focuser and attaches to the silcosteel of
the transfer line using a 1/8" to 1/16" reducing union. The bottom of the adapter is a disk which
goes between the septum retainer and the septum to seal it to the injection port. The septum
used must have a hole in the center large enough for the fused silica to pass through easily and
for carrier gas to pass through around the fused silica when the unit is used in the split mode.
Once the adapter tube is screwed onto the injection port, the cryogenic focuser itself is slid down
over the tube so that it rests on the GC septum retainer, and the top of the adapter tube
extends above the top of the cryogenic focuser. The fused silica from the GC oven is brought all
the way through the focuser adapter tube, into the reducing union, and, if it is narrow enough,
should extend about one inch into the silcosteel tubing of the transfer line. The transfer line
tubing is attached to the 1/16" side of the reducing union, and the adapter tube to the 1/8"
side of the reducing union, then the transfer line end is slid down over the reducing union
to keep it hot.
Liquid nitrogen from a low pressure tank (one atmosphere) is connected from the tank Liquid
fitting, using the adapter supplied, to the inlet of the cryogenic solenoid box, using 1/4" copper
tubing with foam insulation. Flow from the solenoid to the cryogenic focuser inlet and from the
cryogeinc focuser outlet to vent also uses insulated 1/4" tubing. The cryogenic focuser electric
cable is attached to the Pyroprobe using a 7-pin connector at the socket labeled “Cryofocuser”.
The cryogenic solenoid box is attached to this cable at the focuser end using a 2-pin Molex
connector.
In programming the Pyroprobe, the cryogenic focuser may be "Enabled", for cryogenic use,
or "Disabled" if cryogenic focusing is not required.If Disabled is selected, the cryogenic focuser
will automatically go to the transfer line temperature to prevent a cold spot.
Page 6.25
1/8" O.D. S S T R A N F E R LINE
SPLIT POINT
END OF COLUMN
FROM CONCENTRATOR
COLUMN FOCUS JACKET
IN
COOLINGJACKET
C D S M O D I F I E DF O C U S O R
M O D I F I E DU N I V E R S A L
NEEDLE ASSEMBLY OUT
R E T A I N E RA D A P T E R
TOP OF GC
SEPTUMRETAINER
T O S P L I T T E RV A L V E
I N J E C T I O NP O R T H E A T E R A S S E M B L Y
OVEN INSULATION
GC OVEN
COLUMN
FIGURE 6.17. Cryofocuser on GC injection port.

Page 6.26
1 NEEDLELESS CONNECTION SEPTUMRETAINERNUT
1
DEPENDINGON THE GC, IT IS 2A ASSEMBLYSHOULD LOOK LIKE THIS
NECESSARYTO EITHER
REMOVETHE CENTER INSERT
OUT OF THE RETAINEROR
DRILL IT THRU WITH THE #12 COLUMN UP THROUGHTUBE
DRILL PROVIDED.
THIS IS TO ALLOW THE

COLUMNADAPTERTUBE COLUMNADAPTERTUBE
TO BE INSERTEDINTO THE
COLUMN
RETAINER. THIS TUBE
ALLOWS US TO EXTEND
THE INJECTIONPORT UP
INTO THE 1500 OVEN.
SEPTUMWITH CENTER HOLE COLUMNADAPTER
SHOWN IN PLACE
GC SPLIT ADAPTERTUBE
FLOW ADJUST SOL GC INJECTIONPORT
RETAINER
SEPTUM W/ CENTER HOLE
GC INJECTIONPORT
GC SPLIT GC CARRIERINLET
FLOW
2 SOLENOID
LEAVE BOTTOMINJECTIONPORT GC CARRIERINLET
FITTINGLOOSE UNTIL THE END OF
THE INSTALLATIONOF THE
COLUMN
GENTLYSLIDE COLUMN UP
THROUGHINJECTIONPORT,
SEPTUM,ADAPTERTUBE, AND,
FINALLY,OUT THROUGHTHE
RETAINER.
NOTE: FITTINGSTILL LOOSE

IF INJECTIONPORT HAS A LINER
IN IT THAT PREVENTSTHE
COLUMNFROM GOING
THROUGH,THEN THE LINER
MUST BE REPLACED OR
REMOVED.
FIGURE 6.18. Needle connector for cryogenic focuser.

Page 6.27
FIGURE 6.19. Positioining cryogenic focuser.

Page 6.28
FIGURE 6.20. Attaching transfer line tubing.

Page 6.29
FIGURE 6.21. Completed installation of the cryogenic focuser.

Page 6.30
Cryogenic Trapping
The trapping zone of the Pyroprobe 5200 may also be used with cryogenics to lower the
collection temperature below ambient. Only one cryogenic zone may be used at a time, so
when using cryogenic trapping, microswitch #2 must be in the ON position and #3 (for the
cryogenic focuser) in the OFF position.
To use cryogenic trapping, the standard trap heater must be replaced with the cyrogenic
version, which includes the heater and the well for liquid nitrogen, plus the fittings for entry
and exit of the liquid nitrogen (see figure 6.22 and the diagram below). The solenoid for
the liquid nitrogen, and the trap heater both connect to a plug which goes into the top
socket on the rear of the Pyroprobe. The existing trap heater (for ambient traps) may be
placed to the side of the unit, but does not need to be unplugged from the Pyroprobe.
During trap heat, only the cryogenic version will heat if switch #2 is turned ON (see Figure
6.23).
Because of the volume for the liquid nitrogen, and the added insulation, the cryogenic trap
heater assembly is considerably wider than the standard trap heater, so care must be
taken when installing it into the trapping zone of the Pyroprobe. Once installed, the system
requires that the liquid nitrogen supply be attached to the inlet of the solenoid box. The
outlet of the solenoid box must be connected to the IN tubing of the cryogenic trap itself,
and the flow OUT tube for the liquid nitrogen should be vented to prevent displacement of
oxygen from the room.
Page 6.31
Figure 6.22. Cryogenic trapping assembly.
Figure 6.23. Microswitches for Pyroprobe options.

Page 7.1
SECTION 7. ALTERNATIVE PROBES
DIRECT INSERTION PROBES (DIP)

FOR MASS SPECTROMETRY
THERMOCOUPLE PROBES
1/2 INCH PROTECTED COIL PROBE
DIRECT INSERTION PROBES FOR MASS SPECTROMETERS
The Pyroprobe may be used to provide direct Pyrolysis-Mass Spectrometry by using a direct
insertion probe. The DIP is made as a direct replacement for the solids probe supplied by the MS
manufacturer, and is only available for mass spectrometers which have a solids probe port. In use,
the Pyroprobe controls the sample temperature while it is inserted into the mass spec, permitting
rapid heating to elevated temperatures as well as slow, programmed heating to study the thermal
behavior of materials.
DIPs are available only in coil models, and exact information regarding the make and model of the
mass spectrometer is essential to insure compatibility.
Page 7.2
PYROPROBE 5000 LEAD CONNECTIONS FOR DIRECT INSERTION PROBE
THE PYROPROBE MUST BE UNPLUGGED BEFORE ATTEMPTING TO MAKE ANY ELEC-

TRICAL CONNECTIONS SUCH AS REPLACING THE PROBE FILAMENT.
PROBE FILAMENTS ARE MADE OF PLATINUM WHICH IS EASILY DAMAGED. DO NOT

TOUCH THE FILAMENT WHILE REPLACING THE PROBE ROD.
The direct insertion probe for the Pyroprobe terminates in one connector which is attached to both
the red and black wires in the handle, and a return strap which is connected to the combined green
and white wires. When changing from a standard (GC or FT-IR) probe to a direct insertion probe
for MS work, the red and black wires must be connected together at the center fitting in the handle
before attaching the probe, as shown in drawing 1 below. Alternatively, the connections may be
made using the jumper supplied, as shown in drawing 2. In addition, the ballast resistor located
inside the control module must be changed according to the directions on page 7.5.
When changing from a direct insertion probe to a standard GC or FT-IR probe, the red wire
must be moved to the top connector in the handle, as shown in the drawing on page 7.3.
Drawing 1. Wires joined at

center position.
Drawing 2. Jumper
used to connect
wires.
FIGURE 7.1
Page 7.3
PYROPROBE LEAD CONNECTIONS FOR GC OR FT-IR PROBES


The standard GC or FT-IR probe terminates in a return strap, which is connected to the combined
green and white wires in the Pyroprobe handle, and two wires. The smaller wire on the probe is
connected to the red wire at the top connector in the Pyroprobe handle, and the larger wire is
connected to the black wire at the center connector. When changing from a direct insertion probe
to a standard probe, the red wire in the handle must be moved to the top connector as shown in
the drawing below.
When changing from a standard GC or FT-IR probe to a direct insertion probe for mass
spectrometry work, the red wire must be combined with the black wire as shown on page 7.2. In
addition, the ballast reisitor must be changed according to the instructions found on page 7.5.
FIGURE 7.2.
Page 7.4
PYROPROBE 5000 LEAD CONNECTIONS FOR THERMOCOUPLE PROBE


The Thermocouple probe for the Pyroprobe terminates in one connector which is attached to both
the red and black wires in the handle, and a return strap which is connected to the combined green
and white wires. When changing from a standard (GC or FT-IR) probe to a thermocouple probe,
the red and black wires must be connected together at the upper fitting in the handle before
attaching the probe, as shown in the drawing below, making sure that none of the connectors touch
the stainless steel feed-through tubing or the 1/16" union used to secure the thermocouple.
FIGURE 7.3.
Page 7.5
IMPORTANT NOTE CHANGING BALLAST RESISTOR
Internal ballast resistor must be changed before using DIP probe or severe probe
damage could occur.
To change the ballast resistor:
1) Unplug Pyroprobe.
2) Remove left hand side Pyroprobe cover.
3) Locate terminal strip on the board, see Figure 7.4.
4) Loosen screws just enough to remove ballast resistor which is connected to termi-
nals B and E of the terminal strip.
5) Replace with the other ballast resistor provided.
CAUTION: The longer ballast resistor can only be inserted in one direction (see drawing).
ALSO: The ballast resistor should not be touching any wires, the chasis, or the probe storage
tube after it is in place.
DIP probe -- short ballast resistor
Standard probe -- long ballast resistor
6) Replace the cover on Pyroprobe.
7) Plug unit in and resume normal operation.

Page 7.6
Ballast Resistor
FIGURE 7.4.
Page 7.7
PROTECTED COIL PROBE
A ruggedized version of the coil Pyroprobe is available as the 1/2 inch protected coil probe. In this
probe, the platinum coil is wrapped around the outside of a permanent quartz tube. Samples are
placed into a smaller quartz sample tube,which then slides into the tube which is a part of the probe.
This prevents the sample tube from disrupting the platinum coil when samples are placed into the
probe for pyrolysis.
The protected coil probe requires a 1/2 inch Interface for connecting to the gas chromatograph.
Because the sample is held inside of a tube within a tube, the heating rate of the sample is
dampened, and it is advisable to increase the pyrolysis time to compensate for the double
thickness of quartz. The maximum setpoint for the protected coil probe is 1300°C.
The "permanent" or larger of the quartz tubes, which protects the platinum coil, is held into the probe
by a threaded cap. This tube may be changed for cleaning, or if it becomes damaged. To remove
the protective quartz tube, unscrew the retaining cap which holds it in place, as shown in Figure
7.5.
Platinum coil Protective tube Retaining cap Sample tube
FIGURE 7.5.
Page 7.8
The Protected Coil Pyroprobe is connected to the black Pyroprobe handle in the same way that
the standard GC and FT-IR Pyroprobe filament rods are connected, as shown in Figure 7.6.
FIGURE 7.6
Page 7.9
1/2 INCH COIL PROBE
Because the interface zone heater for the 1/2" coil probe is larger and longer than the standard
1/4" probe, the mounting bracket is different. As shown in Figure 7.7, the 1/2" bracket is split, with
a spring loaded section for the larger heater on the 1/2" pyrolysis side. The trap mounting for the
5200 is the same. The 1/2" coil probe also uses a different ballast resistor than a standard 1/4"
probe. If a 1/2" 5200 is to be converted to a standard 1/4" model, the interface tube, heater, probe
and ballast resistor must all be changed.
Trap heater
Trap bracket side
1/2" Interface heater
1/2" heater bracket side
Carrier in
Probe seal for

1/2" probe
Standard bracket
for 1/4" probes.
FIGURE 7.7. Bracket for using 1/2" coil probe (top) and standard 1/4" probe (bottom).
Page 8.1
SECTION 8. FT-IR INTERFACING, THE BRILL CELL
INTRODUCTION
Use of the CDS Analytical Brill Cell and the Pyroprobe 5000 permits the analysis of solid materials
by the combined technique of Pyrolysis-FT-IR. The Brill Cell is designed to fit into the sample
compartment of a standard FT-IR bench, and thus places the filament of the Pyroprobe directly in
the light path, for immediate acquisition of spectral data. Samples may be placed directly onto the
surface of the ribbon probe, or held in a quartz boat for use of the coil probe. With the filament
positioned just below the light path, the sample may be heated rapidly for a single spectrum
analysis of the material, or slowly with multiple scans recorded for time/temperature studies.
The Brill Cell is mounted into the sample compartment of the FT-IR by attaching a base plate, as
with other FT-IR accessories. To permit easy insertion of samples, a replacement cover is
required, with an access hole for the probe rod of the Pyroprobe. This allows the sample to be
placed into the Brill Cell without disturbing the optics purge of the bench. An additional purge and
flow controller is supplied for the cell itself, including an on/off valve. This flow may be used to purge
the cell between runs, to purge the cell continuously during a long, programmed run, or to supply
an atmosphere inside the Brill Cell different from the nitrogen used to purge the bench optics.
Pyrolysis FT-IR may be used to support and confirm data obtained by Pyrolysis-GC or Pyrolysis-
MS, to screen samples rapidly for identification, for quality control of polymeric materials, to
provide FT-IR information on opaque, filled or complex materials, or to study thermal processes
with the immediacy of in-beam sampling. The Pyroprobe 5000 may be used for gas chromatog-
raphy, mass spectrometry or FT-IR simply by changing the probe rod and using the appropriate
interface.
DESCRIPTION
The CDS Analytical Brill Cell is a sampling attachment using standard windows (25 mm diameter,
4 mm thick) which permits the positioning of the Pyroprobe filament into the sample compartment
for direct Pyrolysis-FT-IR. It includes fittings for inlet and outlet of a purge gas, a mounting plate,
a vertical support tower, seals, gaskets, two sets of windows, and a pneumatics module which
incorporates the cell purge gas flow controller, on/off valve and fittings. The Brill Cell includes a
heater for the cell body, which is controlled by the accessory heater control of the Pyroprobe.
Page 8.2
The windows are held in an easily removable retainer which is threaded to permit cleaning and
replacement of the windows without disturbing the cell body. The Brill Cell comes supplied with
one set of KBr windows and one set of ZnSe windows, and all the necessary gaskets to seal the
windows into the cell body.
Brill Cells are configured and supplied for installation into specific FT-IR benches from major
manufacturers. Because the sample compartment dimensions, beam height above the sample
compartment floor, focal point and cabinetry differ from one manufacturer to another, the specific
mounting plate, positioning of inlets, cover, etc. will change from one instrument to another. The
installation instructions included here are general, and use diagrams which are typical, but may
differ from the actual unit being installed. Figure 8.1 shows a side view and an end view of a typical
Brill Cell, indicating the positioning of the various parts. The window retainers screw into the cell
body, which is held in place by the vertical tower, which is mounted into the base plate. The base
plate has several grooves cut into it to receive the vertical tower. This is to permit correct
positioning of the cell with regard to the beam height and focal point configuration of the FT-IR
bench concerned. In all cases, the Brill Cell must be positioned so that the FT-IR beam passes
directly through the cell and over the filament of the Pyroprobe. Holes in the base plate are provided
which align with threaded holes in the floor of the FT-IR sample compartment to anchor the entire
sampling module.
A replacement cover for the FT-IR is available to provide easy access for the probe rod, and
mounting for the additional pneumatics. Figure 8.2 shows the pneumatic module for the Brill Cell,
including the purge gas fittings, flow controller and on/off valve.
INSTALLATION
Complete installation of the Brill Cell for pyrolysis FT-IR involves the correct positioning of three
main parts: the Brill Cell proper, the replacement cover for the FT-IR bench, and the pneumatics
module for the cell purge gas. The cell may be used without replacing the cover and installing the
pneumatics, but this would require leaving the original cover of the FT-IR open for probe access,
interrupting the optics purge. Alternatively, the original instrument cover may be modified with a
probe insertion port by the user, or delivered to CDS for modification. In the following instructions,
specific parts will be mentioned as they are shown in Figure 8.1. The number in parentheses after
the part name is the item number as it is used in the diagram.
THE CELL BODY
When the Brill Cell is ready to be placed into the sample compartment of the FT-IR, it resembles
the one shown in Figure 8.3. The cell body is held in the vertical tower (7), which fits into the cell
base (8). The cell base is attached to the bottom of the FT-IR sample compartment using screws
through holes in the base which align with mounting holes in the FT-IR. For this reason, it is
necessary to specify the make and model of the FT-IR used when purchasing the Brill Cell, and may
be necessary to purchase additional cell bases to interface to other FT-IR benches. The cell body
is held in the vertical tower (7) by tightening a screw (14) at the top of the tower.
Page 8.3
WINDOWS
The cell windows (5) are held in a large threaded nut (3) which screws into the cell body. The
window should have an o-ring (4) on either side of it, and is held into the nut with a window retainer
(6). The assembled nut (3) is screwed into the cell body, using a larger o-ring (2) to seal it into place.
To replace windows, a window retainer tool (15) is provided.
INSTRUMENT COVER
To permit access for the Pyroprobe and mounting for the cell purge pneumatics, a replacement
cover for the FT-IR bench is available for use with the CDS Brill Cell. In general, the original cover
for the bench is hinged at the top, back, and is designed to cover both the top and front of the sample
compartment. The typical replacement cover hinges at the same location and is constructed to
cover the top and front, and has an access hole for the probe. The modified instrument cover must
also include two Swagelok bulkheads for cell flow in and out, and the electrical fitting to connect
the Brill Cell heater to the Pyroprobe controller. The original cover should be removed at the hinge,
and the new cover attached in the same way.
In some instruments, the original cover will have replaceable panels, and the access hole and
pneumatics have been configured on new panels intended to replace these. These may be held
in place either with retainers or magnets, and the new panels attach in the same way used for the
original panels. In all cases, the probe inlet tube (11) should project through a hole in the cover or
panel, using the cover gasket to prevent air intrusion.
PNEUMATICS MODULE
The Brill Cell is purged using a flow controller which is provided in a pneumatics module, together
with fittings for connecting the purge gas, and an on/off valve . Flow is attached from the inlet
bulkhead to the flow controller then to the on/off valve . From here it proceeds to the inlet fitting
of the cell body, purges the cell and exits the top fitting which is connected to the cell vent bulkhead
on the panel. The diverter valve has three positions: ON, in which the purge gas, controlled by the
flow controller proceeds tothe Brill Cell; OFF, in which there is no purge flow; and PURGE, in which
a high volume of purge flow bypasses the flow controller and goes to the cell to purge it rapidly after
use.
PYROLYSIS USING THE BRILL CELL
Once the Brill Cell has been installed in the sample compartment of the FT-IR, the cover replaced
and the optics purged, samples may be pyrolyzed using either the ribbon or coil filament of the
Pyroprobe. Samples should be placed directly onto the surface of the ribbon probe, in the center
of the platinum filament. When heated, the ribbon expands, and should deflect down, away from
the FT-IR beam. This can be verified by examining the position of the filament using the “clean”
function of the Pyroprobe. When using the coil probe, the sample should be held in a quartz boat
which permits the sample volatiles to go directly into the light path.
Page 8.4
It is generally necessary to use a larger sample for analysis by Pyrolysis-FT-IR than is used for
Pyrolysis-GC. For gas chromatography, 10-100 micrograms is generally sufficient while for FT-
IR work, 100-200 microgram samples are typical. This, of course, depends on the organic content
of the sample and the kind and sensitivity of detector used. The cell purge gas may be left on during
analysis, or used to flush the cell between runs. Since the purge gas for the cell is isolated from
the rest of the FT-IR instrument, a gas other than nitrogen may be used, including air or oxygen for
oxidation studies.
The cell heater for the Brill Cell is intended to reduce condensation of pyrolysate, especially on the
windows. It should be operated at a temperature sufficient to keep the pyrolysis volatiles in the
vapor phase so that they may be flushed from the cell. The heated cell may be used at ambient
temperatures with standard o-rings, or at elevated temperatures, using high temperature o-rings
(2,4) to seal the windows (5) and window nuts (3).
USE OF THE BRILL CELL WITH THE PYROPROBE 5150 0R 5200
The Brill Cell for Pyrolysis-FT-IR is intended to be used as an isothermal interfacing zone, similar
to the Pyroprobe 1500 GC interface. These interfaces are generally used with the Model 5000
Pyroprobe. The Pyroprobe 5150 and 5200 incorporate low-mass interface zones which are
programmable and placed on-line and off-line with the GC automatically by an 8-port valve. Since
these functions are not needed when using the Brill Cell for Py-Ft-IR, the 5150 and 5200 models
may be set to perform like a standard 5000 by changing switches on the board in the electronics
section of the Pyroprobe. The switches are located at the top of the board behind the one
containing the fuses, in a red component. As shown below, for use with an isothermal interface like
the Brill Cell (5000 mode), only switches #1 and #7 should be turned on, and all others should be
off. The Brill cell is plugged into the Aux Heater socket on the rear of the unit, instead of the standard
GC interface module.
Page 8.5
FIGURE 8.1. BRILL CELL

Page 8.6
Purge flow module, front view
Diverter valve Flow controller
Purge flow module, rear
Bulkheads for flow in from tank and flow out to Brill Cell
FIGURE 8.2. PNEUMATICS MODULE FOR BRILL CELL

Page 8.7
Cell Body Mounting Tower
Baseplate
Reducing union for

connecting purge flow
Bulkheads for flow Shaft for probe access

in and out of Brill Cell to Brill Cell
Electrical connection
for heater, connects to
Pyroprobe controller
Probe Inlet
FIGURE 8.3. BRILL CELL AS SEEN FROM TOP IN INSTRUMENT.

Page 8.8
UNIVERSAL MOUNTING FOR BRILL CELL
When the Brill Cell is supplied for a specific make and model of FT-IR, the mounting plate is
configured to match accessory installation holes for correct positioning of the cell within the sample
compartment. Alternatively, the cell may be provided with a “universal” mounting arrangement
which permits installation into a variety of FT-IR makes, permitting use in multiple instruments.
Instead of a solid mounting plate with pre-drilled holes, the bottom of the cell is equipped with
movable brackets. These brackets should be positioned inside the sample compartment so that
they are alligned with the mounting holes in the bottom and the cell is held in the correct position
relative to the center of focus.
To adjust the hight of the Brill Cell to match the beam height of the FT-IR, the “tower” is also slotted,
permitting the cell to slide up and down. When the proper height has been reached, the cell should
be held in place using the screws which extend through the slots and into the body of the cell.
Page 8.9
ELEVATED PRESSURE OPTION FOR THE BRILL CELL
The Brill Cell may be equipped with pressure control, which connects to the outlet of the cell, for
operation at elevated pressures. The Pressure Control Option is supplied in a pneumatics
module which includes a back pressure control knob, a diverter valve and a pressure gauge. This
back pressure module is used in conjunction with the Brill Cell pneumatics which supply carrier flow
into the cell.
INSTALLATION
When connecting the Brill Cell Elevated Pressure Option module, be sure that the standard Brill
Cell purge pneumatics are already installed according to instructions in this manual. The standard
purge pneumatics provide a flow controller (metering valve for elevater pressure operation) to
deliver carrier gas to the cell, a diverter valve to direct the purge gas and a cell vent fitting. The
Elevated Pressure pneumatics module is connected to the outlet of the Brill Cell at the vent fitting.
On the rear of the Elevated Pressure module are two fittings, marked "From Brill Cell" and "Vent".
Pressure inside the Brill Cell is controlled by connecting the outlet vent from the Brill Cell
pneumatics to the fitting marked "From Brill Cell" on the back of the Elevated Pressure module.
The vent for the entire cell system is now the fitting marked "Vent" on the back of the Elevated
Pressure module. A pneumatics diagram for the connection of the Elevated Pressure option to
the Brill Cell outles is shown in Figure 8.4.
OPERATION OF THE BRILL CELL AT ELEVATED PRESSURES REQUIRES CARE TO

REDUCE PRESSURE BEFORE REMOVING PROBE, AND TO INSURE THAT THE ZnSe
WINDOWS ARE SERVICEABLE, AS DESCRIBED ON THE NEXT PAGES.
Page 8.10
RV
BH RV
ON BACK OF
MODULE
BH
H3V
PG
ON FRONT OF MODULE
FIGURE 8.4 ELEVATED PRESSURE OPTION PNEUMATICS DIAGRAM.

Page 8.11
OPERATION
The front panel of the Elevated Pressure Option module includes a pressure gauge, a diverter
valve and a vent, arranged as shown in the diagram below.
Once the Elevated Pressure Option module has been connected to the outlet of the Brill Cell,
pressure inside the cell may be regulated by adjusting the back pressure control knob, which is
located on the back of the pressure module. System pressure is displayed on the pressure gauge
located on the front panel of the Elevated Pressure module. When the diverter valve is turned to
the "PRESSURE" position, purge gas from the cell is directed to the back pressure controller
before being vented from the system outlet vent located on the rear of the Elevated Pressure
module. If the diverter valve is in the "VENT" position, flow from the cell goes immediately out the
vent on the FRONT panel of the Elevated Pressure module. (Refer to the diagram in Figure 8.4,
in which the diverter valve is marked H3V, Vent is immediately adjacent to it, and SYSTEM
OUTLET VENT is on the rear of the module, after the back pressure controller.)
To set a pressure in the Brill Cell, be sure that the metering valve and diverter valve upstream of
the cell in the purge gas control module are ON,and that the probe is secured into the Brill Cell, then
put the diverter valve of the Elevated Pressure module to the PRESSURE direction. Now select
the desired pressure on the pressure gauge by turning the back pressure control knob on the rear
of the pressure control module.
Pressure Gauge Diverter Valve
VENT PRESSURE
Vent from diverter valve
ELEVATED PRESSURE MODULE FRONT PANEL

Page 8.12
To control the probe rod when removing it from the cell after an analysis, always be sure to
depressurize the cell before loosening the probe connection to the Brill Cell. To depressurize,
turn the diverter valve on the elevated Pressure module to the VENT position, reduce the pressure
setting, or both.
SAFETY
The Elevated Pressure module includes a factory set pressure relief device which limits the system
pressure to 500 PSIG. If system pressure exceeds this limit, the relief valve will open and vent the
system through the SYSTEM OUTLET VENT on the back of the Elevated Pressure module.
When operating the Brill Cell at elevated pressures, be sure that the ZnSe windows used in the cell
are not scratched, cracked or otherwise incapable of withstanding the pressure used. Use of KBr
windows, or imperfect ZnSe windows could permit fracturing of the window, throwing
fragments into the optics of the FT-IR. Also be sure that the Pyroprobe rod is secured firmly into
the Brill Cell before increasing system pressure. To protect the windows from sudden pressuriza-
tion, increase the back pressure in the Brill Cell gradually to the operating level. Exercise caution
when turning the diverter valve of the Elevated Pressure module to the VENT position when the
system is at elevated pressure, since this causes the pressurized cell gas to vent rapidly from the
front of the module.
CHANGING THE OPERATING PRESSURE RANGE
The Elevated Pressure module for the Brill Cell comes with two interchangeable pressure control
springs to change the operating range. The BLUE spring covers pressures ranging from 50 to 350
PSIG, and the YELLOW from 350 to 750 PSIG (although the system is preset at the factory not to
exceed 500 PSIG). To change the spring, turn the pressure setting knob all the way counterclock-
wise until the knob unscrews from the unit. The spring may now be removed, and replaced with
the other one to change the operating range. Insert the new spring and screw the knob back onto
the unit.
Page 9.1
SECTION 9. SAMPLE HANDLING KIT
Contents:
One pair of sample tweezers

One blade and handle
Plunger for inserting samples and quartz wool
Quartz wool and tubes
Reference polymers;
Kraton 1107 (Styrene/isoprene copolymer)
Nylon 6.6
Polyethylene (Low density)
The CDS Analytical Sample Handling Kit provides small tools to help prepare samples
for pyrolysis using the Pyroprobe. For suggestions concerning sample size, tempera-
tures and other parameters, please refer to the guide “Getting Started Is Easy” which
may be found in the binder pocket of this manual.
To help evaluate the functioning and interfacing of the Pyroprobe, analyses of the
three reference materials included in the kit are provided on the following pages, both
by GC-MS and FT-IR.
CDS Analytical offers many one-page application notes demonstrating the analysis of
materials using pyrolysis. These may be obtained directly from CDS by contacting the
office at 800 541 6593, or they may be downloaded from our web page,
www.cdsanalytical.com.
Page 9.2
Page 9.3
Page 9.4
Page 9.5
Page 9.6
Page 9.7
Page 10.1
SECTION 10. AS-5250 PYROLYSIS AUTOSAMPLER
INTRODUCTION
The AS-5250 Pyrolysis Autosampler is an instrument which provides automatic multiple sampling
for pyrolysis using the CDS Analytical Pyroprobe® 5000. Samples are loaded into quartz tubes,
which are placed vertically in a carousel. The quartz tubes are dropped sequentially into the pyroly-
sis zone, pyrolyzed, then the spent tubes are dropped out the bottom into a collection tray. Pyrolysis
parameters of temperature, rate and time are set using the controller of the Pyroprobe® 5000 as
usual. The probe settings of the 5000, however, control the built-in coil of the autosampler, and the
va/ve oven control sets the temperature of the pneumatics oven. Communication among the
autosampler, the Pyroprobe® controller and the gas chromatograph permits complete automation
of the pyrolysis-GC process, with remote-start of the GC, and wait-for-ready intelligence.
The 5250 Autosampler may be installed directly onto the GC injection port, or mounted on the 5000
series controller and connected to the GC using a transfer line, as for Models 5150 and 5200
Pyroprobe.
PRINCIPLE OF OPERATION
Figure 10.2 shows a schematic of the AS-5250, as well as a plumbing diagram for the 8-port valve
controlling the GC carrier gas and purge gas flows through the autosampler. Sample tubes are
placed into the carousel which fits at the top of the autosampler. As the carousel rotates, a tube is
dropped into the loading chute, and stops at the top loading valve (C).
Autosampler mounted on GC AS-5250 Autosampler mounted on

Using rear-discharge tray Pyroprobe 5000 series controller with tube
front-discharge chute and tray
FIGURE 10.1.
Page 10.2
FIGURE 10.2. AUTOSAMPLER AND PLUMBING DIAGRAM OF 8-PORT VALVE.

Page 10.3
PYROLYSIS
To complete a pyrolysis run, the following steps are employed:
The carousel rotates to drop in the first sample tube;
The top loading valve (C in the diagram) opens, and the sample tube drops into the pyrolysis
chamber;
Valve C closes and the chamber is purged to vent to remove air before pyrolysis;
The 8-port on-line/off-line valve (E in the diagram) is energized to put the pyrolysis chamber
on-line with the GC injection port, and a delay time permits re-establishment of GC flow and pres-
sure;
The sample is pyrolyzed, using the platinum coil surrounding the pyrolysis chamber, a start
signal is sent to the GC, and a post pyrolysis delay permits sweeping the pyrolysate onto the GC
column;
The pyrolysis chamber is taken off-line from the GC by de-energizing the 8-port valve;
The sample discharge valve (D in the diagram) is opened, permitting the spent tube to drop
into the collection tray;
If selected, the pyrolysis chamber is cleaned to by heating the platinum coil a second time, to
the "clean" setting of the Pyroprobe® 5000.
After the above process, the discharge valve is closed, and the autosampler waits for a "GC Ready"
signal before advancing the carousel to the next sample.
Tube funnel
Tube input valve

On-line/off-line valve C in diagram
E in diagram
Pyrolysis coil
Tube discharge valve

Connection to injection D in diagram
port of GC
or to heated
transfer line
Tube discharge chute to
Vent collection tray
FIGURE 10.3.
Page 10.4
SENSORS
The autosampler control is simple because most of the information needed for operation is supplied
by amplified reflective photomicrosensors. A total of five sensors is used to provide various pieces
of information concerning the mode, status and position of the autosampler. Specifically, these are
as follows:
1. A "carousel in place" sensor, which tells the autosampler whether or not a sample tray
has been loaded. If the carousel is in place, the autosampler proceeds in the automatic mode,
and if it is not, the autosampler is in the manual mode, for the analysis of one sample tube;
2. The "home" sensor, which guarantees that the carousel is in the proper orientation at
the beginning of a run;
3. A position sensor which tells the autosampler which sample location is being run, and
displays the sample position on the message center screen;
4. The tube sensor which counts and locates each sample tube in the carousel; and
5. A tube discharge sensor which checks to see that the spent tube has dropped out of
the pyrolysis chamber before another is allowed in.
The sample tube sensor recognizes both the presence and position of the sample tubes, so there is
no need to load the carousel in any particular way. As the carousel rotates, the sensor tells the
autosampler which positions have samples in them, and the carousel stops only at those positions,
skipping any empty slots.
Never add, remove or change the position of tubes once they have been past the tube
sensor. This would invalidate all position information and cause misfeeding of the tubes.
Depending on the information from the sensors, messages may be displayed in the Pyroprobe DCI
window indicating appropriate action. When the tray is first installed, the message "rotate tray to
home", will indicate that the carousel is not in the home position. When this is corrected, the
autosampler will automatically continue the run. If the tube discharge sensor does not register that
the tube has dropped out of the pyrolysis chamber, the message "no discharge" is shown and the
unit will not advance until the operator guarantees that the sample path is clear.
Page 10.5
Pyrolysis Autosampler
Tube sensor Short Alignment Pin Carousel HubTall Alignment Pin
Automatic/Manual sensor Home sensor Position Sensor
FIGURE 10.4. Autosampler seen from the top with the carousel removed to show alignment pins
for the carousel and sensors.
Page 10.6
Autosampler tube carousel Hole for tall alignment pin
Cover for zone

past tube sensor
Notch in carousel for tube sensor
Notch in carousel must

be aligned with the tube
sensor when placing the
carousel onto the autosampler.
FIGURE 10.5. Autosampler carousel.

Page 10.7
OPERATION
PROGRAMMING THE 5250 AUTOSAMPLER
The Pyroprobe autosampler is controlled using the DCI Software window just as for the other 5000
series Pyroprobes. For detailed explanation of the menus and programming, please see section 4
of this manual. Under Configuration, Accessory type, “Autosampler” must be selected. When in-
stalled, the 5250 adds a list of tube positions to the Sequence programming window so that it looks
like this:
When the Autosampler is started by pressing the RUN SEQUENCE button, the tubes are delivered
to the pyrolysis coil in order and each is processed using the Pyroprobe method entered for that
tube number. Double clicking on the Method Name space for each tube will bring up a table of
stored methods for easy programming. Under CLEAN for each tube, one of three selectiona may
be made. Clean to Vent uses the Pyroprobe Clean settings to clean the chamber before the next
tube is inserted. Clean to GC puts the 5250 back on-line with the GC when it is ready, heats the
chamber to the clean temperature and produces a GC blank run. No Clean skips the cleaning step
and moves the unit to the next method in the sequence.
Page 10.8
Just as the Model 5000 may be programmed to to multiple runs per sample, the 5250 may as well.
By clicking on EDIT, then INSERT ROW at any tube number, additional methods may be added for
that tube. In the CLEAN space, it is advisable to select NO CLEAN when performing multiple runs
per sample so that the sample in the tube is not heated to the clean settings before the next analytical
run.
In operation, the Autosampler will perform all runs associated with a specific tube number before
dropping the tube out to the discharge chute and loading the next tube. The final method for a tube
should include a CLEAN TO VENT or CLEAN TO GC step to clean the chamber before introducing
the next sample tube.
The NOTES field in the Autosampler sequence window permits adding a notation about each method
for each tube to record sample name, conditions, operator, etc.
Page 10.9
In the Autosampler sequence below, a total of five runs would be performed on three tubes. Tube
1 is just a single pyrolysis, but tube 2 is heated to 150°, and then at 250°C for desorption, prior to
a final run for pyrolysis at 700°C.
NO CLEAN has been entered after the first two runs of tube 2 in the sequence, then CLEAN TO
VENT after the pyrolysis, before the run on tube 3.
A GC sequence must be created with enough runs to accomodate all of the Autosampler runs.
Even though there are only three tubes being analyzed, a total of five chromatograms will result, so
the GC sequence must allow for five runs for all of the data. In operation, the 5250 will wait until
the GC is ready for the next run before either advancing to the next tube or performing the next run
in a series on the same tube.
Page 10.10
CAROUSEL
SAMPLE LOADING
Samples for analysis using the autosampler must be placed into a quartz tube and positioned verti-
cally in the carousel. The autosampler quartz tubes are fire-polished on one end and it is important
that the fire-polished end is placed down, to prevent tubes from jamming in the loading valve. Samples
may be positioned in the tube with either quartz wool as for traditional Pyroprobe® tubes, or by using
a quartz placement rod, or a combination. Samples may be placed near the top of the tube since the
top end of the tube is within the pyrolysis coil during heating. Attention should be paid to samples
which will melt during the early stages of pyrolysis heating, since the tube is positioned vertically
during pyrolysis, and melted sample will run down the tube. A generous plug of quartz wool below the
sample, and placement at the top portion of the tube will help maximize pyrolysis. In all cases, as
with the standard Pyroprobe®, it must be remembered that the sample being pyrolyzed goes di-
rectly to the column inlet, and therefore, the sample size must be compatible with the gas chromato-
graph. In general, samples should be smaller than 1 mg, with sizes of 10 to 100 µg being preferred.
This is especially important when using sample materials which produce significant amounts of
high-boiling products and residues during pyrolysis. The use of samples which are too large will
FIGURE 10.6. Sample placement in quartz tube.

Page 10.11
result in plugging the 8-port valve and the vent line of the 5250. If the vent line becomes completely
plugged, the pyrolysis chamber will be pressurized to tank regulator pressure, which will cause the o-
rings to distort and fail. For this reason it is recommended that sample size not exceed 100 µg and
that the vent flow be monitored frequently. If the vent flow decreases, it may indicate plugging of the
valve or vent line. Call CDS service for assistance.
POSITIONING CAROUSEL
The autosampler carousel fits onto the top of the autosampler over the carousel hub. The carousel
has a small hole near the hub for a tall alignment pin, a hole on the bottom for the short alignment pin,
and a notch for the sample tube sensor. The carousel should be placed over the tall alignment pin
and hub first, then rotated so that the sensor notch lines up with the sensor. As the carousel slides
down the hub, with the notch going over the sensor, the short alignment pin and corresponding hole
should engage, and the carousel should be in the "home" position. If it is not, a message will appear
in the DCI window when the start button is pressed.
STARTING A RUN
Once the carousel is loaded and in position on the autosampler, and the Pyroprobe® is programmed
with the desired pyrolysis, clean and interface (pneumatics oven) setpoints, the run is initiated by
clicking the "START SEQUENCE" button.
If the GC is not ready, the message will display "GC not ready". If the GC is ready, the autosampler
will begin its run. If the carousel is not in the "home" position, "rotate tray to home" will be displayed
after the start button is pressed. If this is displayed, slowly rotate the tray to the home position (notch
directly at sensor). As soon as the unit senses that the carousel is in the home position, the carousel
motor will engage and drive it clockwise, then reverse to insure homing, then rotate the carousel to
the first sample position, and begin the run.
NOTE
OCCASIONALLY A QUARTZ TUBE MAY BECOME BROKEN INSIDE THE PYROLYSIS ZONE OF
THE 5250 AUTOSAMPLER. TO REMOVE A BROKEN TUBE, FOLLOW DIRECTIONS FOR RE-
MOVING AND REPLACING THE VALVE ROTORS, ON PAGE 10.20, AND BE SURE THAT ALL
FRAGMENTS ARE CLEARED FROM THE UNIT BEFORE CONTINUING.
Page 10.12
IMPORTANT NOTE!
SEQUENCING GC RUNS WITH THE CDS ANALYTICAL 5250
In addition to programming the CDS 5250 for multiple runs, the gas chromatograph data station
must also be programmed to sequence the resulting data files. This prepares the GC to save each
run as a separate file for subsequent analysis. When the GC sequence has been programmed and
initiated, the CDS 5250 will step through its program, sending a start signal to the GC for each
separate run.
For the HP Chemstation software, a sequence is programmed using the following steps.
Click on VIEW and then select TOP.
From the TOP menu, select SEQUENCE.
In the SEQUENCE menu, select EDIT SAMPLE LOG TABLE.
In the log table window GC methods, data file names, sample names and types are selected for
each run in the sequence. This sequence may be named and saved by selecting SEQUENCE
SAVE in the SEQUENCE menu.
When ready, the GC sequence is initiated by clicking on SEQUENCE, then RUN.
A window will appear indicating that the GC is waiting for a start. At this time, the 5250 should be
started, and it will start the GC when the sample is pyrolyzed.
Additional information is available through the HELP screens of the Chemstation.

Page 10.13
INSTALLATION
Just as the standard GC interface (see section 6 of this manual) the Autosampler must be connected
pneumatically to the gas chromatograph. This requires disconnecting the GC carrier flow into the
injection port and connecting it instead to the autosampler. The inlet to the injection port must be
capped to prevent all flow from leaking out where the carrier was disconnected.
As with the Pyroprobe Models 5150 and 5200, the GC carrier flow is connected to the on-line, off-
line valve, which permits directing flow either to the pyrolysis chamber of the autosampler or straight
to the injection port.
Flow is connected from the valve either directly to the injection port, if the 5250 is mounted on top of
the GC,or through a heated transfer line, using a union inside the pneumatics oven of the autosampler.
When installed on top of the GC, the union inside the pneumatics oven of the autosampler attaches
to a piece of 1/8" stainless steel tubing which is connected to the injection port by the septum re-
tainer, as shown in the diagram below. The 1/8” tubing may end in a needle, in which case, the
column is installed as usual, or it may be open, in which case the column is brought up through the
tubing and into the oven of the 5250 to reduce dead volume. In that case, the carrier flow which exits
the splitter vent goes through the tube around the outside of the capillary column, into the injection
port and out the split vent while the analytical flow goes through the capillary column.
When the 5250 is mounted on the 5000 module, the connection is made using a heated transfer line,
as described in section 6 of this manual for Models 5150 and 5200.
FIGURE 10.7. Connecting flow to the injectionport with and without the needle.
Page 10.14
INSTALLATION INSTRUCTIONS
Installing the pyrolysis autosampler involves three steps:
A. Bringing GC carrier flow into the autosampler instead of directly to the injection port;
B. Adding the adapter to the septum retainer; and
C. Connecting the autosampler to the septum retainer adapter.
A. GC Carrier Flow (Please refer to the diagram on the next page.)
1. Disconnect the tubing which goes from the helium filter to the “carrier in” position of the
GC injection port.
2. Cap the end of the tubing connected to the injection port so that flow will not exit here
instead of going to the column. Be sure to use a Vespel ferrule at this plug so that it may be removed
later if it is desired to restore the GC pneumatics to their original configuration.
3. Attach a piece of tubing to the outlet fitting of the helium filter.
4. Attach the other end of this tubing to the bulkhead on the autosampler marked GC
Carrier. Now the GC flow or pressure controller is supplying flow into the autosampler instead of into
the injection port of the GC.
5. Install a "T" fitting in the helium inlet line to provide purge flow for the
autosampler. (Or simply connect a separate supply of purge gas.)
6. Connect one leg of the "T" to the original helium inlet for the GC to maintain flow for the
GC pneumatics.
7. Connect the tubing for the purge flow to the autosampler bulkhead fitting marked Cham-
ber purge Inlet.
B. Adapting the septum retainer
1. Remove the septum retainer and septum from the injection port.
2. Insert the 1/8" tubing of the septum retainer adapter through the septum retainer so
that it protrudes above the top. It may be necessary to enlarge the needle hole in the septum
retainer using a 1/8" drill bit to permit passing the tubing through. All of the tubing should be above
the septum retainer so that the flat disk at the bottom of the adapter contacts the inside of the septum
retainer.
3. Place an o-ring against the flat disk of the adapter so that it is sealed into the injection
port septum well with the adapter on top of it, held in place by the septum retainer, as shown
in Figure 10.7. The 1/8" tubing will protrude up from the injection port, and the autosampler will be
attached to the injection port using this tubing.
Page 10.15
Autosampler helium supply diagram
Autosampler
Chamber Purge Inlet
GC Carrier fitting
8-port
Valve
Helium supply “T” fitting GC flow controller Plug Injection port

or pressure regulator
FIGURE 10.8.
Carousel Valve oven cover
To access valves, remove carousel from autosampler,

then slide valve oven cover straight up to remove,
then remove insulation jacket.
FIGURE 10.9.
Page 10.16
Manual switches for valves
Sensor indicators
Connector for main communications cable from

autosampler controller
Purge flow adjust
Chamber Purge flow bulkhead
GC carrier IN from GC
Pyrolysis filament connection from

Pyroprobe® 5000
Oven heater
Connects to valve oven heater
control of Pyroprobe® 5000
Cable from Autosampler to

Controller
FIGURE 10.10. Rear of 5250 Autosampler.

Page 10.17
C. Connecting the Autosampler
1. Decide which orientation will be used, and place the autosampler above the chosen
injection port.
2. Remove the front cover of the autosampler and place it so that the 1/8" tubing of the
septum retainer adapter passes into the valve area of the autosampler.
3. If it has not yet been done, attach the carrier flow and purge flow to the corresponding
bulkhead fittings on the autosampler. Adjust purge flow to 10-20 ml/min using the purge flow adjust
needle valve (see Figure 10.10). NOTE: The purge flow may be shut off when the unit is not in use
by closing the manual shut-off valve next to the purge flow adjust, and to the left of the bulkheads.
4. If using the injection port adapter without a needle, bring the inlet of the capillary col-
umn up through the injection port (removing the liner if necessary) and through the adapter tubing so
that it is even with the end of the tubing. If using the adapter with a needle, leave the column as
installed for standard GC injections. If using the heated transfer lilne, attach the end as shown in
Section 6 of this manual.
5. Attach the 1/16" tubing from the valve to the adapter tubing (or to the transfer line
tubing) using the reducing union provided.
6. Replace the insulation covering the valve area, then slide the cover back into place.
7. Plug the electrical connection for the autosampler pneumatics oven into the valve oven
heater position on the back of the Pyroprobe® controller.
8. Connect the round black cable usually attached to the handle of the Pyroprobe® probe
rod to the connector on the left side of the autosamplerusing the green/white, black and red wires.
9. Connect the cable from the Pyroprobe control module to the back of the
autosampler above the bulkheads.
Page 10.18
MAINTENANCE
Valves
The 5250 autosampler incorporates an auto-maintenance function to exercise the input and dis-
charge valves periodically. When not conducting sample runs, the autosampler is programmed to
rotate each of the valves periodically. This function helps prevent the valves from sticking during
periods in which the instrument is not being used.
When first heating the autosampler, when resuming use after an idle period, or when increasing the
valve oven temperature, the input and discharge valves should be rotated several times. Especially
when connecting the autosampler and heating the valve oven from cold or room tempera-
ture, it is important to ensure free valve rotation until the oven has reached operating tem-
perature. This is done automatically using the valve break-in mode. To activate this, turn off power
to the autosampler, then hold in the green START button on the front panel and turn power back on.
Continue to hold the button in until the valves rotate and the Dry and Clean LEDs begin to blink. To
exit this mode, press the RESET key on the front panel.
Before initiating a sample carousel run, ensure that the tube path is completely clear by allowing a
quartz tube to drop through both valves. To do this, place a tube into the tube funel manually, then
press the INPUT valve toggle to the down position and leave it there. Next place the DISCHARGE
valve toggle in the down position. The tube should drop out of the autosampler, go into the tube
collection tray and you should hear the discharge sensor beep. (If you do not, please follow the
directions for clearing the sample path.) After the tube has dropped through, return the INPUT valve
toggle to the center position (which deenergizes the valve) and then return the DISCHARGE valve
toggle to the center position.
Manual valve rotation toggle switches.
Center position is CLOSED.
Press DOWN to OPEN.
Note order -
Top - Input
Discharge
On-line (8-port)
Bottom - Carousel
FIGURE 10.11.
Page 10.19
MAINTENANCE
Valve sticking
Occassionally, especially at very high valve oven temperatures, a valve may become stuck in the
closed position. When this occurrs, tubes will not drop through the pyrolyzer, so the display will show
NO DISCHARGE after the run. This condition is usually associated with a chattering sound made by
the valve as it tries to rotate either manually or automatically.
To free a stuck valve, it is usually adequate to reduce the valve oven temperature and use the toggle
switch on the rear of the autosampler to rotate it manually. Set the valve oven temperature to 100°C,
and when it has cooled to this temperature, manually rotate the valve until it moves smoothly. When
increasing the valve oven temperature to the working state, remember to rotate the input and dis-
charge valves using the VALVE BREAK IN mode described on page 10.18 to keep them free
during the temperature change.
If the stuck valve does not respond to this method of freeing it, it may be necessary to remove the
valve seat and replace it, as described on the next page.
No tube discharge
When the autosampler displays NO DISCHARGE, it is likely that the quartz tube did not pass the
DISCHARGE valve and is still in the pyrolyzer. The autosampler is programmed to rotate the carou-
sel back to the HOME position and open both the INPUT and DISCHARGE valves in this case,
waiting for tube removal. To remove a stuck tube, execute the following steps:
The input and discharge valves are already open. Gently insert a cotton pipe cleaner through
the tube funnel. If the tube is stuck at the top, it can be withdrawn using the pipe cleaner;
If the tube is not in the top portion of the pyrolyzer, gently insert the pipe cleaner further into the
autosampler to dislodge the tube through the bottom valve. You shoud be able to pass the pipe
cleaner all the way through the input valve, pyrolysis zone and discharge valve to clear the unit;
Remove the pipe cleaner and insert the alignment rod through the tube funnel. If the tube is
cleared, the tool will pass all the way through the unit to the discharge sensor, stopping when it
contacts the discharge tray, and making the sensor sound;
NOTE
IF YOU CANNOT REMOVE THE QUARTZ TUBE OR ALL FRAGMENTS OF A CRUSHED TUBE
FROM THE PYROLYSIS CHAMBER, CONTACT CDS SERVICE BEFORE PROCEEDING, AT:
800 541 6593
Remove the alignment tool, turn the 5250 off, then turn it on. The valves will automatically be
placed in the correct orientation.
Page 10.20
MAINTENANCE
VALVE ROTOR REPLACEMENT
The valve seat rotors on all three of the valves in the autosampler are replaceable, and the same
technique is used for all. Before attempting to replace a valve seat, it is essential that the valve
oven be turned OFF and that the valves be cool.
Valve Body
Valve Seat Retainer
FIGURE 10.12.
The valve seat rotor is held in the valve body by the valve seat retainer, which screws into the
valve body and has a central tension adjustment part which accepts an allen wrench. To remove
the seat, the entire seat retainer is unscrewed from the body. This retainer is knurled on the 8-
port valve and smooth on the input and discharge valves.
Valve seat rotor Seat retainer removed from

valve body
Alignment tab
FIGURE 10.13.
Page 10.21
When replacing the valve seat rotor in the inlet and outlet tube valves, it is important that the seat be
oriented properly so that the tubes may drop through in the “open” position. The tab on the valve seat
inserts into a slot in the valve which rotates, turning the seat. Be sure that the valve is in the closed
position (using the toggle switch) before replacing valve seat. With the valve in the closed position,
the allignment slot is horizontal. The rotor itself has an oval position indicator between the two holes.
With the valve seat slot horizontal, the oval should be facing DOWN in the valve.
Insure that the replacement valve seat is inserted fully into the valve body, with the tab on the seat
going into the slot in the valve, then screw the seat retainer back into the valve body.
As the valve heats up to operating temperature, rotate the valves using the VALVE BREAK IN func-
tion to ensure free and smooth motion.
NOTE: A new valve seat may make more noise than an older, conditioned one. This noise should
dissipate after the valve is heated to operating temperature and rotated to condition the seat mate-
rial.
NOTE:
The rotors used in the valves of the 5250 Autosampler are designed to operate at elevated tem-
peratures. Best performance and rotor lifetime are achieved by keeping the valves hot, even
when the 5250 is temporarily not in use. Frequent heating and cooling of the valve oven may
cause the rotors to stick or shorten their lifetime.
Inlet valve with seat retainer and seat Valve rotor for inlet and outlet valves.
removed. Oval indicator, must face DOWN.
Seat
Seat retainer
FIGURE 10.14
Page 10.22
CDS ANALYTICAL 5250 PYROLYSIS AUTOSAMPLER

IMPORTANT VALVE CONDITIONING START-UP PROCEDURE
When first heating the autosampler, when resuming use after an idle period, or when increasing the
valve oven temperature, the input and discharge valves should be rotated several times. Especially
when connecting the autosampler and heating the valve oven from cold or room tempera-
ture, it is important to ensure free valve rotation until the oven reaches operating tempera-
ture. This is done automatically using the valve break-in mode. To activate this, with the autosampler
power off, hold the green START button on the front panel and turn power on. Continue to hold the
button in until the valve rotates and the bottom two LEDs (Dry and Clean) begin to blink. This will
continue to exercise the valves during the temperature change and prevent valve sticking. While
operating in this mode, the DCI will display “Break in mode”. Allow the unit to function in this mode
until the valve oven operating temperature has been reached. This function continues until intention-
ally exited, and the autosampler will perform no other function in this mode. To exit this mode, press
the RESET key on the front panel.
O-RING REPLACEMENT
The quartz pyrolysis zone is sealed between to the two valves using high-temperature o-rings. To
access these o-rings, the top (tube inlet) valve may be raised and lowered using the valve locK-down
nuts on top of the valve mount, as shown in Figure 10.15. Unscrewing these nuts permits raising the
top valve so that the pyrolysis chamber and/or o-rings may be replaced. The lock-down nuts must be
retightened after the chamber and o-rings have been positioned properly.
Valve lock-down nuts
Top o-ring
Pyrolysis chamber
Bottom o-ring
FIGURE 10.15.
Page 10.23
CHANGING FROM FRONT-DISCHARGE TO REAR-DISCHARGE TUBE COLLECTION
After pyrolysis, the quartz tubes are discharged from the 5250 via the tube discharge chute on the
front of the unit (see Figure 10.16). When the 5250 is installed on top of the GC, or if front-discharge
is not desired, the tubes may be discharged to the rear of the 5250 into a collection tray behind the
valve oven (see Figure 10.1). When using the front-discharge chute, the tubes pass through a hole
in the rear-discharge chute (Figure 10.17). To use the rear discharge tray, the hole must be plugged
with the metal stopper shown in Figure 10.17. This plug is inserted from the top with the legs down
so that the tubes now strike the top of the plug and roll back to the collection tray.
The rear-discharge tray has a handle on one end and slides out from the side of the 5250 for empty-
ing the spent tubes.
Valve oven
Chute
Collection tray
FIGURE 10.16. Tube discharge chute on front of 5250.

Page 10.24
Hole in Front discharge chute

Tray
Rear tray
located b
behind
valve oven
at the
bottom.
Plug used for rear-discharge.

Inserted into the hole with legs
down.
Figure 10.17. Front discharge tray and plug for rear-discharge.

Page 10.25
AUTOSAMPLER WITH TRAPPING

PYROPROBE AS 5250-T
The Pyroprobe Autosampler may be equipped with trapping capability, reactant gas function and
cryogenic trapping, which make it the Pyroprobe 5250-T. This version is installed the same way
ad the standard 5250, but includes additional valves and operational functions. A toggle switch on
thefront of the unit converts the autosampler from standard to trapping mode. Samples are
loaded into the carousel and drop into the pyrolysis coil in the same way as the standard 5250.
Selection and operation of most additional functions is done through the DCI software.
Trap
Valve oven
Direct/Trapping
Toggle switch
Figure 10.18. The Pyroprobe 525 -T Autosampler.

Page 10.26
INSTALLATION
Bulkheads for connecting flows IN to the 5250-T are located on the right rear of the pneumatics
module as shown in Figure 10.19. The flow controller for sample carrier is also located on the
rear, above the bulkheads. When reactant gas is being used, both the inert and reactant gas
carriers enter the base of the Pyroprobe control module and the exit from the base (fitting marked
TO PURGE) is connected to the Carrier IN bulkhead on the Autosampler as shown in Figure
10.20. The GC transfer line is connected in the same way as that used for all Pyroprobes, con-
necting inside the 5250-T valve oven at the T fitting shown in Figure 10.21.
In addition to the 37 pin D connector cable that goes from the side of the Pyroprobe controller to
the rear of the 5250-T, there is a round connector from the Remote I/O of the Pyroprobe to the
5250-T just above the 37 pin D connector. The heavy black Probe wire is connected to the front of
the 5250-T at the small terminal strip with the green/white wires on the left, red in the center and
black on the right.
The trap insert may be changed by loosening the thumbwheels that hold it in place and sliding it
out of the trap heater. Inlet of the new trap must face down.
Round Remote I/O

Connector
Flow controller Toggles
Flow in from Inlet

TO PURGE Outlet
bulkhead On-line
on Pyrorpobe Carousel
GC carrier
37 pin conector from

Pyroprobe controller
Figure 10.19 Rear of 5250-T.

Page 10.27
Reactant gas carrier IN
Inert carrier IN
Carrier OUT connects to

the Carrier IN bulkhead
on the right rear of the
5250-T Head.
Figure 10.20. Reactant gas connections for Pyroprobe on rear of controller module.
Thumbwheel
Trap Inlet valve

Heater
Thumbwheel Pyrolysis coil
Transfer line Outlet valve

Connection
Figure 10.21. Valve oven of the 5250-T.

Page 10.28
OPERATION
When operating the 5250-T Autosampler, under Configuration, Accessory type, “Autosampler with
Trap” must be selected. The autosampler may now be used with or without trapping by using the
mode toggle on the front of the unit as shown in Figure 10.18. It is not necessary to reconfigure
the system using the DCI when changing between Direct and Trapping modes. This will happen
automatically, and the operating mode will be displayed at the bottom of the DCI screen as shown
in Figure 10.22.
Figure 10.22. Configuration of the 5250-T.

Page 10.29
Pyroprobe filament methods are programmed the same way used for all Pyroprobes. The deci-
sion of whether or not to use the reactant gas is part of the method and is saved. Methods are
sequenced for the samples using the Autosampler page of the DCI, just as for the standard 5250.
The valve oven of the 5250-T is set isothermally using the REST setpoint of the Accessory con-
trol.
Figure 10.23. Accessory REST setpoint is used to set the valve oven temperature.
Page 10.30
On the Isothermal zone control page of the DCI software, only the Transfer Line setpoint is used
since the valve oven is controlled using the Accessory page.
Figure 10.24. Transfer line.

Page 10.31
TRAP FUNCTIONS
On the Trap page of the DCI the Reactant gas may be selected for use. When Enabled, the
reactant gas is turned on for both the equilibration time and the pyrolysis run time. After this time,
the autosampler switches to the inert carrier to purge reactant gas out of the trap during the post
pyrolysis time. The post pyrolysis time is set at a minumum of 1 minute to protect the sorbents in
the trap from oxidation if air is being used as the reactant gas.
NOTE: Reactant gas function, either enabled or disabled, is saved as part of the Pyroprobe
method and so will be activated automatically in the autosampler sequence when a method using
this function is recalled.
If the 5250-T is equipped with cryogenic trapping, setpoints may be entered for the trap with
negative values. When running, the 5250-T will take the trap to the Initial (negative) setpoint
before placing the sample into the coil.
Figure 10.25. Reactant gas selected on the Trap page.

Page 10.32
Cryogenic Trapping
The trapping zone of the Pyroprobe 5250-T may be used with cryogenics to lower the collection
temperature below ambient. Only one cryogenic zone may be used at a time, so when using
cryogenic trapping, microswitch #2 must be in the ON position and #3 (for the cryogenic focuser)
in the OFF position.
To use cryogenic trapping, the standard trap heater must be replaced with the cyrogenic version,
which includes the heater and the well for liquid nitrogen, plus the fittings for entry and exit of the
liquid nitrogen. The solenoid for the liquid nitrogen has a plug which goes into the top socket on
the rear of the Pyroprobe control module. The existing trap heater (for ambient traps) is removed
from the 5250-T and the cryogenic trap is then plugged into the heater socket to the right of the
trap.
Because of the volume for the liquid nitrogen, and the added insulation, the cryogenic trap heater
assembly is considerably wider than the standard trap heater, so care must be taken when install-
ing it into the trapping zone of the Pyroprobe. Once installed, the system requires that the liquid
nitrogen supply be attached to the inlet of the solenoid box. The outlet of the solenoid box must be
connected to the IN tubing of the cryogenic trap itself, and the flow OUT tube for the liquid nitrogen
should be vented to prevent displacement of oxygen from the room.
LN2 IN
LN2 OUT
Cryogenic well and heater
To trap Cable From Tank

Liquid Nitrogen solenoid
Figure 10.26. Cryogenic trapping on the 5250-T.

Page 10.33
MODEL 5250T
READY
TIC TAH TAHH
TALL
SWAGEL RTD
TO GC
SWAGEL
SWAGEL
PRE-PRESS
NC
GC CARRIERIN
MPV-2
C 3 4
1 2 2 5
NO MPV-I
5 6
8 7 1 6
8 7
4 3
TAHH
REACTANTGAS OPTION
CARRIERIN
( F R O N TP A N E L ) 4 5 TALL
TAH
AS MPV-1
REACTANTGAS SV-1 SAMPLECARRIER 1 TIC
RTD
3
3 4
2 5
AS MPV-3 PYROLYSIS
CHAMBER
1 6
8 7
2
PURGE VENT
BACK OF UNIT
AS MPV-2
2
4 3
5
Figure 10.27. Flow Diagram for the 5250-T. Corresponding valves are indicated in photograph.
Page 11.1
SECTION 11. SPECIALIZED SYSTEMS

PYROBOT
HIGH PRESSURE 5200
CATALYTIC REACTOR
PYROBOT
FIGURE 11.1 PYROBOT connected to Pyroprobe 5200.
DESCRIPTION
The CDS Analytical Pyrobot is an accessory for the Pyroprobe 5200 which permits moving
the sample through the pyrolysis zone while it is being heated. The sample is placed into a
long quartz or Silcosteel tube which is purged with sample carrier gas to the trap of the
5200 while the tube moves through the pyrolysis coil. Speed and direction of the tube
movement are controlled from the Pyrobot while the heating time and temperature are
controlled through the Pyroprobe 5200. After the sample has been collected to the trap of
the 5200, the trap is placed on-line with the GC, heated and desorbed at the start of the GC
run, as usual for the 5200. Sample carrier may be inert or reactant gas, as controlled by the
5200.
Movement of the tube through the coil begins at the start of the Pyroprobe run. The lower
end of the tube is connected to tubing which passes through a heated interface zone to
take the sample volatiles to the valve oven of the 5200, then to the trap. The total distance
traveled by the tube is controlled by placement of the lower Stop switch.
Page 11.2
Quarts sample tube
Coil filament
Stop switch at top
Coil placement
adjust screw
Nut and ferrule at

bottom of tube
Moving platform
Interface zone
FIGURE 11.2. Pyrolysis zone of the Pyrobot.
In use, the fitting at the lower end of the sample tube is attached to a moving platform.
While the sample is heated, the platform may be made to move up, down or remain sta-
tionary. Analytes are carried from the bottom of the tube through heated tubing in the
interface zone, into the valve oven of the 5200.
A Stop switch is located at the top of the platform traveling path so that the platform will
stop automatically when it elevates the sample tube. The lower stopping point is selected
by adjusting the location of the Stop switch at the bottom of the tube run. Placing the
sample tube within the coil between the upper and lower limits set by the Stop switches is
controlled by using the UP and DOWN buttons on the front of the Pyrobot.
Page 11.3
On the front of the Pyrobot are four buttons, a toggle switch and a speed control knob. The
buttons are labeled UP, DOWN, STOP, and HOME. Pressing either UP or DOWN will
cause the moving platform at the bottom of the sample tube to move up or down until it
contacts one of the Stop switches or until the STOP button is pressed. The speed at which
the tube travels is controlled by selecting a value from 1 to 999 on the selection knob, with
999 representing the fastest rate of moving.
The sample may be made to travel either up or down during sampling by using the
SAMPLE DIRECTION toggle switch. If the sample is moving down through the pyrolysis
coil in sampling, the home position is all the way at the top. If the sample is moving up
while it is heated, the home position is all the way down, when the platform contacts the
lower Stop switch. Pressing the HOME button will cause the platform to move all the way
up or down, depending on the sampling direction selected.
Changing the Home position with the toggle switch must be done while the Pyrobot is
turned off to become active. When the Pyrobot is turned on, it will update the sampling
direction and home position.
FIGURE 11.3. Front of the Pyrobot.

Page 11.4
Tubing from purge gas bulkhead connects to top of

sample tube
Sample Tube
Pyrolysis coil
Moving platform
Interface zone
Interface zone cable
Adjustable bottom stop
Sorbent trap
Bulkhead for purge gas to sample tube
FIGURE 11.4. Pyrobot connected to 5200.
Flow through the sample tube to the trap is controlled by the carrier gas flow controller on
the Pyroprobe 5200. The reactant gas feature is also programmed and used in the same
way as for the 5200 by itself. Purge gas is connected to the top of the sample tube using
PEEK tubing connected to the purge gas bulkhead, the left one of the two on top of the
5200.
Page 11.5
INSTALLATION
Connecting the Pyrobot to a gas chromatograph is identical to connecting the standard

5200 to the GC, shown in section 6 of the Pyroprobe manual. The 5200 must be operated
in the Trap mode to be sure that desorption of collected analytes takes place at the start of
the GC run.
The Pyrobot must be positioned to the left of the Pyroprobe 5200. Attaching the Pyrobot to
the 5200 requires connecting flow from the lower tube fitting (on the moving platform, see
Figure 11.2) to the 1/16” tubing inside the interface zone. PEEK tubing from the left 1/16”
bulkhead of the Pyroprobe 5200 must be attached to the top of the sample tube (see Fig-
ure 11.4). The three wires inside the Pyroprobe filament rod handle must be attached to
the gray connectors on the left side of the Pyrobot tower, as shown in Figure 11.1. The
Pyrobot and 5200 must be directly adjacent so that the moving platform with the lower tube
fitting moves smootlhy within the interface zone.
OPERATION
Sample is loaded into the long Pyrobot sampling tube, which is then installed as shown in
Figure 11.4. The tube is sealed with a Swagelok fitting at the top and bottom to provide
flow to the trap during sampling.
The Pyrobot filament temperature is controlled by the Pyroprobe 5200 software in the usual
way. Sample heating by the filament and movement through the coil both start at
Pyroprobe initial in the 5200 program. The total distance traveled is set by moving the
lower Stop switch assembly (see Figure 11.4).
After the sample tube has been installed, the sample should be taken to the Home position
by pressing the Home button on the front of the Pyrobot. The motor speed and sample
heating parameters must be synchronized to be sure that the sample travels the required
distance and is heated to the desired temperature during the Pyroprobe run.
Manual Operation
The Pyrobot may be used to pyrolyze samples without moving them during heating. The
sample tube is placed into position, then moved manually to the desired location using the
buttons on front of the Pyrobot. For manual operation, the remote start cable from the
5200 to the Pyrobot should be disconnected. When the 5200 filament fires, sample will be
purged to the trap of the Pyroprobe, but the motor will not turn on to move the sample tube.
After pyrolysis, the sample tube may be moved to another location manually and heated
again.
Page 11.6
Automatic Operation
In automaitc operation, the Pyrobot motor moves the sample through the coil while it is
being heated. Sample direction, home position, sample speed and length of sample move-
ment must be determined before the 5200 run is started. Once the coil begins to heat, the
sample motor will start, and move the sample until it comes to the appriopriate Stop switch.
Automatic operation involves the following steps:
1. Select sample direction and home position using the toggle switch.
2. Move the platform with the lower Swagelok fitting to the top of the Pyrobot. Insert the
sample tube through the coil and attach it at the top and bottom fittings.
3. Adjust the bottom stop switch to set the total sample movement distance.
4. Set the motor speed so that it moves the sample the required distance during
Pyroprobe heating step of the 5200.
5. Take the sample tube to the Home position.
The entire system run is started from the 5200 Run Method button. The interface tempera-
ture initial and final should be set the same (isothermal operation) so the Pyrobot will begin
moving the sample at the beginning of the run. Sample is transferred from the tube to the
trap of the 5200, then to the GC, so the Pyroprobe must be in the Trap mode, and appropri-
ate settings entered to desorb the trap at the start of the GC run
Page 11.7
HIGH PRESSURE 5200
The High Pressure option for the CDS 5200 permits pyrolysis at elevated pressures. The
interface zone is pressurized using a back pressure regulator, and flow from the BPR goes
through the trap of the 5200 for collection of the pyrolysate before transfer to the GC.
The High Pressure 5200 has two flows and two vents. There is a low pressure purge flow
which removes air and purges residuals from the system, and a high presure sampling
flow that permits sampling at elevated pressure, transporting the pyrolysis products to the
trap of the 5200. The two vents are located beside each other on the front of the 5200. In
the idle state, shown above, the purge flow is directed through the pyrolysis interface and
exits through the PURGE vent on the right. The high pressure sampling flow exits through
the AUXILIARY vent on the left. At the same time, GC carrier is flowing through the trap
and back to the GC through the transfer line.
MODEL 5200/ HIGH PRESS

S IDE OF 5 2 0 0
READY
HI GH P R E S SC O N T R O LM O D U L E
TIC TAH TAHH
GC CARRIER TALL
VENT
LOAD RUN
RTD
TO GC
3 4 3 4
2 5 2 5
HIGHPRESSURE MPV-2 MPV-1
HP HE 1 6 1 6
8 7 8 7
500 PSIG M A X . SYSTEM HIGHPRESSURE
HP HE
0 - 500 PSIG
TIC TAH TAHH
TALL
VALVEOVEN
RTD
LOWPRESSURE TAHH TAHH
I N T E R F A C EP U R G E F L O WC O N T R O L TALL SWAGEL SWAGEL

TALL
80 PSIGM A X
TAH TAH
L E G AWS L E G AWS
SAMPLE VENT PURGE VENT

TIC TIC
(FRONT PANEL)
RTD RTD
1 AT THE READY STATE THE PROBE IS
LOADED INTO THE INTERFACE. ONCE INTERFACE
TRAP
PROBE IS SEALED, PURGE GAS CLEARS PROBE
THE INTERFACE OF ANY AIR TO VENT.
2 AT THE SAME TIME THE HIGH PRESURE L EGAWS
SIDE OF MPV-2 IS AT SET PRESSURE

AND PURGING TO VENT.
3 GC CARRIER FLOW IS BACKFLUSHING

THE TRAP TO GC.
FIGURE 11.5. High pressure 5200.

Page 11.8
When MPV-2 is in the RUN position, the purge flow exits through the AUX vent on the left.
Sample flow goes through pyrolysis interface and then the back pressure regulator, and
exits at the PURGE vent on the right. Above, the trap is still on-line with the GC, as it
would be before collecting sample or in desorbing the sample to the GC for analysis.
M O D E L 5200/ H I G H P R E S S
MPV-2 ROTATED TO THE RUN POSITION
SIDE OF 5200
HIGH PRESS CONTROLM O D U L E

TIC TAH TAHH
GC CARRIER TALL
VENT
LOAD RUN
RTD
BPR
TO GC
3 4 3 4
2 5 2 5
HIGH PRESSURE MPV-2 MPV-1
HP HE 1 6 1 6
8 7 8 7
500 P S I G M A X . SYSTEM HIGH PRESSURE
HP HE
0 - 500 PSIG
TIC TAH TAHH
TALL
VALVEOVEN
RTD
LOW PRESSURE TAHH TAHH
INTERFACEP U R G E FLOW CONTROL TALL

SWAGEL SWAGEL
TALL
80 PSIG M A X
TAH TAH
L E G AWS L E G AWS
TIC
SAMPLE VENT PURGE VENT TIC
(FRONT PANEL)
RTD RTD
INTERFACE
TRAP
PROBE
L EGAWS
FIGURE 11.6. High pressure 5200, RUN position.

Page 11.9
When sampling at high pressure, MPV-2 is in the RUN position and MPV-1 is rotated so
that flow goes to the trap. In this configuration, high pressure sample flow goes through the
pyrolysis zone, out the back pressure regulator and then through the trap before exiting at
the PURGE vent on the right. The low pressure purge flow is exiting the AUX vent on the
left.

SIDE OF 5200
SAMPLING
GC CARRIER
HIGH PRESS CONTROL MODULE TIC TAH TAHH
TALL
( H E A T E DO V E NC H A M B E R )
LOAD RUN
HP VENT DOWN RELIEF VALVE RTD
TO GC
SYSTEM PRE-PRESSURE
METERING VALVE VENT 3 4 3 4
HIGH PRESSURE 2 5 2 5
HP HE MPV-2 MPV-1
OFF 1 6 1 6
8 7 8 7
PRE-PRESS
CONNECT HERE WHEN USING HIGH PRESSURE OPTION
SYSTEM
SYSTEM CARRIER
METERING VALVE
TIC TAH TAHH
LOW PRESSURE
TALL
SYSTEM INTERFACE PURGE
80 PSIG M A X VALVE OVEN
0 - 500 PSIG
RTD
TAHH TAHH
CONNECT HERE WHEN USING LOW PRESSURE (STANDARD) OPTION FLOW CONTROL TALL TALL
TAH TAH
TIC
S A M P L EV E N T P U R G EV E N T TIC
( F R O N TP A N E L )
RTD RTD
3 4
2 5
SAMPLE CARRIER IN INTERFACE
MPV-RG TRAP
1 6 PROBE
8 7
L EGAWS
REACTANTGAS IN
HIGH PRESSURE REACTANT GAS OPTION
FIGURE 11.7. High pressure 5200, SAMPLING position.

Page 11.10
MPV-2 selects which of the flows goes through the Pyroprobe interface. In the LOAD
position, the low pressure carrier goes through the pyrolysis interface and continues
through MPV-1 and exits the vent on the right. In this configuration, the high pressure
carrier is directed out the vent on the left.
When MPV-2 is in the RUN position, the high pressure flow goes through the Pyroprobe
interface and proceeds out the vent on the right while the low pressure carrier is vented on
the left.
MPV-1 selects whether the trap is on-line with the Pyroprobe or with the GC. MPV-1 is
operated automatically via the software of the 5200, placing the trap on-line with the
Pyroprobe for sampling, and then with the GC for desorption at the start of the GC run.
MPV-2 is operated manually, and must be in the RUN position when using the high pres-
sure carrier for pyrolysis.
Lock
Pressure adjust
Back Pressure Adjust

Regulator housing
MPV-2
Probe inlet
(Interface)
Purge vent
Auxiliary vent
Low pressure
flow adjust
FIGURE 11.8. High pressure 5200, front view.

Page 11.11
Setting pressure and flow
Flow of the low pressure carrier is used for purging air from the system when loading a
sample, or for operating the 5200 in the standard (not high pressure) mode. Flow is set
using the black knob located on the front of the 5200.
Flow of the high pressure carrier is set using the metal knob located on the high pressure
module, and is measured at the left-hand vent on the front of the 5200 (Auxiliary vent in
Figure 11.8) with the Pre-pressure diverter in the System direction.
Pressure in the high pressure carrier is set by rotating the nut on top of the back pressure
regulator. The nut has a smaller locking nut in the center (see Figure 11.8). The nut is
turned clockwise to increase pressure and the pressure is indicated on the digital readout
located on the high pressure module. There is a Pre-pressure flow to permit increasing the
system pressure faster. To use the Pre-pressure, turn the Pre-pressure diverter briefly to
the left (Pre-pressure) direction, then back to System. Pre-pressure flow is also measured
at the auxiliary vent on the 5200, with the Pre-pressure diverter in the Pre-pressure direc-
tion.
HIGH PRESS CONTROL MODULE
S
W
HP VENT DOWN
A
G
E
L
W
SE
G
L
A
RELIEFV A L V EV E N T
S
WA
G
E
L
W
SE
G
L
A
PLUG
3 4 SYSTEM PRE-PRESSURE
2 5
METERING VALVE VENT
SAMPLE CARRIER IN MPV-RG
4 2
HIGHPRESSURE
1 6
S
WA
G
E
L
W
SE
G
L
A
8 7
S
WA
G
E
OFF
L
W
SE
G
L
A
PRE-PRESS
SYSTEM
REACTANT GAS IN SYSTEM CARRIER

METERING VALVE
5 1
S
WA
G
E
L
W
SE
G
L
A
3 SYSTEM XDUCER
0 - 5 0 0 P S I G
PI
1 Pressure readout Reactor

Temperature
2 Vent valve
3 High pressure flow

Adjust
4 Pre-Pressure
Adjust
5 Pre-Pressure
Diverter
FIGURE 11.9. High Pressure Module

Page 11.12
Sample loading
CAUTION
When MPV-2 is in the RUN position, the probe interface is at elevated pressure. The high
pressure valve (MPV-2) must always be in the LOAD position before inserting or
removing the Pyroprobe from the interface zone.
Samples are loaded into the quartz tubes in the same way as for standard pyrolysis. The
tube is inserted into the coil of the probe rod and then the Pyroprobe is inserted into the
interface.
Once the probe rod is inserted into the interface, the retaining nut must be secured with
wrenches before applying high pressure.
When the high pressure valve is rotated to the RUN position, the interface zone goes to
elevated pressure immediately. Because of the increased volume of the interface zone, the
pressure on the gauge will drop when the valve is turned to the RUN position. Pressure on
the gauge will then increase to the setpoint pressure, at which time the carrier gas will
begin to flow from the vent on the right. Be sure that flow has been established before
initiating the Pyroprobe run.
After making a high pressure run, the valve must be turned to the LOAD position before the
probe can be removed.
Page 11.13
Reactant gas option
The reactant gas option permits automatic switching from a reactant gas (such as air or
hydrogen) to an inert gas (helium) to purge the reactant gas from the system before trans-
ferring the sample to the GC. In the High Pressure 5200, the inert purge gas goes through
the pyrolysis zone, and is also operated at high pressure. This requires the addition of a
third 8-port valve, located in the cabinet of the 5200.
When using the reactant gas option, time is programmed for this function in the same was
as for the standard 5200. Time is entered under the trap section, in the box called Reac-
tant Gas. The time entered is the time desired for the reactant gas to be on during pyroly-
sis. After the spedified time, the valve will ratate and switch the carrier to the inert gas for
the ballance of the program. The 5200 automatically switches to inert carrier one minute
before the end of the interface program, so the reactant gas time may be set to any value
up to one minute less than the total interface time.
M O D E L 5200/ HIGH PRESS

SIDEO F 5200
READY
GC CARRIER
H I G H P R E S S C O N T R O LM O D U L E
TIC TAH TAHH
TALL
VENT
LOAD RUN
RTD
TO GC
C O N N E C TH E R E W H E N U S I N G H I G H P R E S S U R EO P T I O N
3 4 3 4
HIGHPRESSURE 2 5 2 5
HP HE MPV-2 MPV-1
1 6 1 6
8 7 8 7
SYSTEM
TIC TAH TAHH

LOW PRESSURE
TALL
I N T E R F A C EP U R G E
80 PSIG M A X VALVEOVEN
0 - 5 0 0 PSIG
RTD
TAHH TAHH
C O N N E C TH E R E W H E N U S I N G L O W P R E S S U R E( S T A N D A R D O
) PTION FLOWCONTROL TALL SWAGEL SWAGEL
TALL
TAH TAH
L E G AWS L E G AWS

TIC TIC
(FRONT PANEL)
RTD RTD
3 4
2 5
MPV-RG TRAP
1 6 PROBE
8 7
1 AT THE READY STATE THE PROBE IS
LOADED INTO THE INTERFACE. ONCE
PROBE IS SEALED, PURGE GAS CLEARS L EGAWS
REACTANT GAS IN THE INTERFACE OF ANY AIR TO VENT.
2 AT THE SAME TIME THE HIGH PRESURE

SIDE OF MPV-2 IS AT SET PRESSURE
HIGH PRESSURE REACTANT GAS OPTION AND PURGING TO VENT.
3 GC CARRIER FLOW IS BACKFLUSHING

THE TRAP TO GC.
FIGURE 11.10. High Pressure reactant gas option.

Page 11.14
M O D E L 5200/ HIGH P R E S S
MPV-2 ROTATED TO THE RUN POSITION
SIDE OF 5200
GC CARRIER
TI C TAH TAHH
TALL
VENT
LOAD RUN
RTD
BPR
TO GC
C O N N E C T H E R E W H E N U S I N G H I G H P R E S S U R E OPTION
3 4 3 4
HP HE MPV-2 MPV-1
1 6 1 6
8 7 8 7
SYSTEM
TI C TAH TAHH
LOW PRESSURE
TALL
INTERFACEPURGE
80 PSIG M A X VALVEOVEN
0 - 500 PSIG
RTD
TAHH TAHH
C O N N E C T H E R E W H E N U S I N G L O W P R E S S U R E ( S T A N D A R D )O P T I O N FLOW CONTROL TALL SWAGEL SWAGEL

TALL
TAH TAH
L E G AWS L E G AWS

TI C TI C
(FRONT PANEL)
RTD RTD
3 4
2 5
INTERFACE
SAMPLECARRIERIN MPV-RG TRAP
1 6 PROBE
8 7
L EGAWS
REACTANTGAS IN
HIGH PRESSUREREACTANTGAS OPTION

SIDE OF 5200
SAMPLING
GC CARRIER
HIGH PRESS CONTROL MODULE TIC TAH TAHH
TALL
(HEATEDOVENCHAMBER)
LOAD RUN
HP VENT DOWN RELIEF VALVE RTD
TO GC
SYSTEM PRE-PRESSURE
HP HE MPV-2 MPV-1
OFF 1 6 1 6
8 7 8 7
PRE-PRESS
SYSTEM
SYSTEM CARRIER
METERING VALVE
TIC TAH TAHH
LOW PRESSURE
TALL
0 - 500 PSIG
RTD
TAHH TAHH
CONNECT HERE WHEN USING LOW PRESSURE (STANDARD) OPTION FLOW CONTROL TALL TALL
TAH TAH
TIC
SAMPLEVENT PURGEVENT TIC
( F R O N TPANEL)
RTD RTD
3 4
2 5
MPV-RG TRAP
1 6 PROBE
8 7
L EGAWS
REACTANT GAS IN
HIGH PRESSURE REACTANT GAS OPTION
FIGURE 11.11. High Pressure reactant gas option, sampling.

Page 11.15
Pneumatic Connections
SIDE OF 5200
SAMPLING

GC CARRIER
6 (HEATEDOVENCHAMBER)
TIC TAH TAHH
TALL
5 LOAD RUN
4 HP VENT DOWN RELIEF VALVE RTD
TO GC
SYSTEM PRE-PRESSURE
HP HE MPV-2 MPV-1
OFF 1 6 1 6
8 7 8 7
PRE-PRESS
3 8
SYSTEM
SYSTEM CARRIER
METERING VALVE
TIC TAH TAHH
LOW PRESSURE
TALL
0 - 500 PSIG
RTD
CONNECT HERE WHEN USING LOW PRESSURE (STANDARD) OPTION 7 FLOW CONTROL
TAHH
TALL
TAHH
TALL
TAH TAH
TIC
SAMPLEVENT PURGEVENT TIC
(FRONTPANEL)
RTD RTD
3 4
2 5
MPV-RG TRAP
1 6
2 8 7 PROBE
L EGAWS
REACTANT GAS IN
1 HIGH PRESSURE REACTANT GAS OPTION
Bulkheads
1 Reactant gas IN
2 Purge gas (high pressure) IN
3 Carrier gas OUT to 5200 8
4 Reactor vent 6
5 Pressure relief vent 7
6 GC flow IN
7 Purge gas (low pressure) IN
8 High Pressure IN from
HP Module
5 4 1 2 3
FIGURE 11.12. High Pressure reactant gas 5200, pneumatic connections.

Page 11.16
CATALYTIC REACTOR
The Pyroprobe 5200 - either with or without the high pressure option - may be equipped
with a temperature controlled catalytic reactor down-stream from the pyrolysis zone. This
permits creating volatiles from a sample using pyrolysis, then chemically treating them with
a catalyst. Figure 11.13 shows the placement of the reactor zone in the 5200 equipped
with the back pressure regulator for high pressure work. As shown in Figure 11.12, the
reactor is placed between the Pyroprobe and the back pressure regulator, so that the
pyrolysis and the catalyst are both at the elevated pressure. Flow into and out from the
reactor tube are both below the reactor in the valve oven, as shown in Figure 11.14. The
catalyst tube is inserted into the reactor heater from the bottom and secured with Swagelok
fittings. Temperature for the reactor heater is set using the digital controller as shown for
the high pressure version in Figure 11.9.
Back pressure regulator
Reactor heater
Catalyst tube
Figure 11.13. Pyroprobe 5200 with catalytic reactor.

Page 11.17
When using the reactor with a standard (low pressure) Pyroprobe, the analytical flow is set
using the black knob on front of the Pyroprobe, and the interface purge is set using the
metering valve which is the silver knob on the side of the Pyroprobe (see Figure 11.15).
There are three 1/16” bulkheads on the left side of the 5200, as shown in Figure 11.15. GC
flow is connected to the one marked GC, and sample carrier PURGE gas is connected
from the fitting on the rear of the 5200 marked TO PURGE. An additional interface purge is
connected from a tank of inert gas (60 - 80 psi) to the fitting at the top marked INTERFACE
PURGE.
Flows for the high pressure version are set as shown in Figure 11.9.
Flow out of reactor

Catalyst tube
Flow into the reactor tube
Figure 11.14. Reactor catalyst tube and fittings.

Page 11.18
Interface purge gas

From tank
Flow in from GC
Sample Purge from

rear of 5200
Metering valve for

Interface purge
MODEL 5200/WITH REACTOR

SAMPLING WITH REACTOR ONLINE
GC CARRIER
SIDE OF 5200
TIC TAH TAHH
TAH TALL
( H E A T E DO V E NC H A M B E R )
OFF LINE ON LINE

REACTOR
TIC RTD
Sample purge gas RTD

TO GC
Black knob on 2
MPV-2
3 4
5 2
MPV-1
3 4
5
LOW PRESSURE
Pyroprobe
1 6 1 6
SAMPLE PURGE 8 7 8 7
FLOW CONTROL
TIC TAH TAHH
Interface purge
TALL
VALVE OVEN
LOW PRESSURE RTD
Silver knob. INTERFACEPURGE
TAHH TAHH
METERINGVALVE TALL SWAGEL SWAGEL

TALL
TAH TAH
L E G A W S L E G A W S
TIC
S A M P L EV E N T P U R G EV E N T TIC
( F R O N TP A N E L )
RTD RTD
INTERFACE
TRAP
PROBE
L EGAWS
Figure 11.15. Pneumatics of the 5200 low pressure system with reactor.
Page 12.1
SECTION 12. INDEX
ITEM DESCRIPTION PAGE NUMBER
1500 Interface 6.01

1500 Interface, operation 6.10
8000, use with 6.12
Accessory type 4.05

Adapting GC septum 6.09
Assembling modules 6.17
Autosampler 10.1
Ballast resistor 7.05

Brill Cell 8.01
Brill Cell, installation 8.02
Calibration 3.05
Calibration 5200 4.06
Calibration number 4.05
Care of filaments 3.07
Catalytic reactor 11.16
Cell, Brill 8.01
Changing mode 5.07
Collection trap 4.11
Communication 4.07
CONFIGURATION menu 4.05
CONFIGURATION menu, 5200 4.06
Connect 4.07
Connections, electrical 6.20
Consumables 2.06
Cover, FT-IR 8.04
Cryogenic trap 6.30
Page 12.2
Description 5000 3.01

Description, 5150 3.03
Description, 5200 3.04
Desorption 5.04
Desorber, test tube 5.18
Desorber, VOST tube 5.20
Desorption tube, Pyrex 5.10
Diagram, interface 6.02
DIP, connection 7.02
Direct insertion probes 7.01
Direct to GC 5.07
Discharge trays, Autosampler 10.23
Disconnect 4.07
Diverter valve 6.11
EDIT menu 4.03

Electrical connections 6.20
Filament replacement 5.09

Filament, programming 4.08
Filaments, care of 3.07
Filaments, ribbon 3.08
FILE menu 4.02
Front Panel 3.02
FT-IR instrument cover 8.04
FT-IR interfacing 8.01
FT-IR probe 7.03
Fuse 6.20
Fuse, filament 6.20
GC Handshake 4.05
GC interface installation 6.03
GC Interfacing 6.01
GC transfer line 6.13
Page 12.3
Gradient, thermal 5.08
Half-Inch Probe 7.9

Handshake, GC 4.05
High Pressure 5200 11.7
I
Initial Set-up 4.7, 5.14
Installation, Autosampler 10.13

Installation, Cryogenic focuser 6.24
Installation, interface 6.03
Interface installation 6.03
Interface programming 4.09
Interface, programmable 4.10
Interfacing, FT-IR 8.01
Interfacing, GC 6.01
Isothermal zones 4.13
Kit, sampling 9.01
Mass spec probe 7.01

Menu, configuration 4.05
Menu, configuration 5200 4.06
Menu, edit 4.03
Menu, file 4.02
Menu, tools 4.04
Method editor 4.04
Method editor 4.14
Method save 4.02
Method, new 4.02
Methods, sequence 4.12
Page 12.4
Microswitches 3.11
Model 1500 Interface 6.01
Model 8000, use with 6.12
Modules, 5150, 5200 6.17
Mounting tray, GC 6.03
Mounting tray, GC 6.07
Multiple steps 5.06
New method 4.02
Operating mode 4.06

Operation 5.01
O-ring replacement, Autosampler 10.22
Panel, front 3.02

PIDs 4.04
Placement of sample 5.08
Pneumatics module 6.17
Power supply 6.21
Print method 4.02
Printer setup 4.02
Probe calibration number 4.05
Probe, FT-IR 7.03
Probe, 1/2” 7.9
Probe, protected coil 7.07
Probe, thermocouple 7.04
Programmable interface 4.10
Programming 4.01
Programming filament 4.08
Programming interface 4.09
Protected coil probe 7.07
Py Mode 4.06
Pyrex desorption tube 5.10
Pyrobot 11.1
Page 12.5
Reactant gas 5.05

Reactant gas, High Pressure 11.13
REactor, catalytic 11.16
Replacement, filament 5.09
Resistor, ballast 7.05
Ribbon filaments 3.08
Rod replacement 5.09
Rotor, valve 10.20
Sample capacity 3.06

Sample handling kit 9.01
Sample placement 5.08
Sample loading, Autosampler 10.10
Sample loading, High Pressure 11.12
Save method 4.02
Semivolatiles 5.03
Sensors, Autosampler 10.4
Septum retainer, adapting 6.09
Sequence 4.12
Set-up, Initial 4.7
Setting High Pressure and Flow 11.11
Single step pyrolysis 5.02
Specifications 2.01
Start-up 3.05
Steps, multiple 5.06
Switches, Micro 3.11
Temperatures, isothermal 4.13

Test tube desorber 5.18
Thermal desorption 5.04
Thermal desorption, 1/4” tube 5.10
Thermal gradient 5.08
Thermal PIDs 4.04
Page 12.6
Thermocouple probe 7.04

TOOLS menu 4.04
Transfer line 4.13
Transfer line, GC 6.13
Trap mode 4.06
Trap. Collection 4.11
Trap, cryogenic 6.30
Trapping mode 5.05
Tube discharge, Autosampler 10.23
Valves, Autosampler 10.19

Valve oven 4.13
Valve, diverter 6.11
Venting volatiles 5.02
Volatiles, transferring 5.04
VOST tube desorber 5.20
Warranty 2.04
Windows, FT-IR 8.03

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Page 1.

P0 BOX 277 465 Limestone Road, Oxford, PA 19363

SECTION 2. Specifications and warranty

SECTION 3. Product description and probe calibration

SECTION 6. Pyroprobe Installation and GC Interfacing

SECTION 7. Alternative Probes

SECTION 8. Pyroprobe FT-IR Interfacing

SECTION 9. Sample Handling Kit

SECTION 10. Pyroprobe 5250 Autosampler 10.1

SECTION 11. Specialized Systems

High Pressure 5200

Catalytic Reactor 11.16

SECTION 12. INDEX 12.1

SECTION 2. SPECIFICATIONS AND WARRANTY

Equipment Rating (Pollution Degree) 2

Installation Overvoltage Category II

The equipment does not contain batteries.

The equipment does not employ laser sources

The equipment does not contain flammable liquids.

Valve Oven 300 350 375 50

R11 R14 R17 R20 R23 R26

FILAMENT TEMPERATURE Settable in 1°C increments to 1400°C

TIMES Settable in units of 0.01 second to

HEATING RATES Settable in units of 0.01°C/millisecond

INTERFACE TEMPERATURE Settable in l°C increments to 350°C

TIMES Settable in units of 0.01 minute to

HEATING RATES Isothermal Model 1500

DRY MODE User selectable

CLEAN MODE User selectable

SEQUENCE Up to 8 methods, each with GC start

FILAMENT TEMPERATURE Settable in 1°C increments to 1400°C

TIMES Settable in units of 0.01 second to

HEATING RATES Settable in units of 0.01°C/millisecond

INTERFACE TEMPERATURE Settable in l°C increments to 350°C

TIMES Settable in units of 0.01 minute to

HEATING RATES Settable in units of 0.01°C/minute to

DRY MODE User selectable

CLEAN MODE User selectable

SEQUENCE Up to 8 methods, each with GC start

FILAMENT TEMPERATURE Settable in 1°C increments to 1400°C

TIMES Settable in units of 0.01 second to

HEATING RATES Settable in units of 0.01°C/millisecond

INTERFACE TEMPERATURE Settable in l°C increments to 350°C

TIMES Settable in units of 0.01 minute to

HEATING RATES Settable in units of 0.01°C/minute to

DRY MODE User selectable

CLEAN MODE User selectable

SEQUENCE Up to 8 methods, each with GC start

1. Term of Warranty: Covered Events. Products manufactured by CDS are warranted

a. Failure of mechanical parts due to normal wear and tear.

4. Limitation of Damages: CDS SHALL NOT BE LIABLE FOR CONSEQUENTIAL

7. Modification in Design or Discontinuance of Products: CDS reserves the right to

Item Part Number

1/4" Coil filament rod 10P25003

1/4" Ribbon filament rod 10P25002

Probe seals (25) 1002-0333

Graphite ferrules (10) 1006-0345

Economy quartz tubes (100) 10A1 3008

Fire-Polished quartz tubes (20) 10A1 3007

Quartz wool 1001-0345

Septum retainer for interface 1001-0162

Sample handling kit 0100-9014

Collar for 1/4" probe 2002-0642

6 mm Vespel ferrules PL50 4912