PYROJECTOR II
Installation andOperation Manual

The Projector Mk 2 was tested in accordance with the EN55011 Group 1,
Class B emission requirements and EN50082-1 immunity requirements,
and EN61010-1. The test sample complied with both the EMI and EMC
test requirements as required by the Eurpoean EMC Directive 89/336/EEC,
and Low Voltage Directive as required by 72/23 EEC.

PYROJECTOR II
Index

1.0

WARRANTY

2.0

INTRODUCTION

3.0

INSTALLATION
3.1 FURNACE ASSEMBLY
3.2 INSTALLATION ON THE GC INJECTOR
3.3 MAIN CONTROL MODULE
3.3.1
3.3.2

Main Voltage Selection
Gas Connections
3.3.2.1
3.3.2.2

3.3.3

4.0

Septum Injection Head and Pelletizer Injection Head
Septumless Injection Head

Furnace Power Cable

OPERATION
4.1
4.2
4.3
4.4
4.5

FRONT PANEL CONTROLSREAR PANEL CONNECTIONSGAS FLOWSTEMPERATURE SETTINGSAMPLE INJECTION
4.5.1

Conventional Septum Injection
4.5.1.1
4.5.1.2
4.5.1.3
4.5.1.4

Low Viscosity Liquid Samples
High Viscosity Liquid Samples
Solid Samples
Pelletizer P-1

4.5.2

Septumless Sample Injection

4.5.3

Pelletizer Injection

4.5.2.1
4.5.3.1

Operation of Septumless Injector
Operation of Pellitizer Injector

4.6 FURNACE REMOVAL AND CLEANING
4.6.1
4.6.2
4.6.3

Quartz Furnace Liner Removal
Quartz Furnace Liner Cleaning
Quartz Furnace Liner Replacement

4.7 SYRINGE MAINTENANCE
4.7.1
4.7.2

PTFE Seal Replacement
Plunger Replacement

4.8 DIGITAL PRESSURE METER

5.0

OPERATING HINTS
5.1 TEMPERATURE PROFILES
5.2 CRYOGENIC OPERATION

6.0

SERVICE
6.1 PACKING & REORDER LIST
6.2 FAULT FINDING
6.2.1

Electrical Faults

6.3 FURNACE REPLACEMENT
6.4 THERMOCOUPLE REPLACEMENT

7.0

PYROJECTOR II – GC INJECTOR ADAPTORS

8.0

ELECTRICAL WIRING DIAGRAM

9.0

PNEUMATIC CONNECTIONS DIAGRAM

1.0 WARRANTYThe Pyrojector II control module is guaranteed against faults in materials andworkmanship for a period of twelve months from the date of invoice.
The Pyrojector II furnace assembly and components are subject to three months
warranty from the date of invoice.
This warranty implies free repair and/or
replacement of defective goods, only upon
proper written proof and (where
authorized) return of the defective product.

Note: SGE does not advocate the use ofhydrogen with this accessory due topotential problems associated with its
inflammable nature.

This unit has been designed to fulfill
the purpose of pyrolysis of small
samples for gas chromatography.
This warranty is void if the
instrument is used for any unrelated
purposes. SGE reserves the right torefuse free service under warranty
on any unit that has been abused or
tampered with in any way.
No other warranty or representation isexpressed or implied by SGE for its
products with respect to merchantability,
fitness for any particular use or purpose or
any other matter. SGE shall not, under any
circumstances, be liable for any incidental,
consequential, or compensatory damages
arising from use of, or in conjunction with,
its products. The maximum liability forbreach of warranty shall be the invoice
price of said products. SGE acknowledges
that there are many service engineers in
the field who have expertise to service the
Pyrojector II and to assist them, we haveenclosed the necessary data in thismanual. To protect your interest however,
we respectfully suggest that any failures beattended to by SGE service personnel or by
SGE authorized service people.

Pg 1

2.0 INTRODUCTION

Pyrolysis Gas Chromatography is a
specialized sample introduction techniquein which a high molecular weight sample
is heated rapidly to pyrolysing
temperatures up to 900˚C in a nonoxidizing atmosphere.
Under these conditions the high molecularweight sample will fragment or "unzip"
into lower molecular weight fragments,
which can be chromatographed in theconventional manner.
The result is normally a complex GC
chromatogram (or pyrogram), whose
profile is characteristic of the particularparent sample under the particularpyrolysis conditions. This technique isespecially valuable for the rapid
identification of samples, which are notchromatographable by conventional GC
techniques.
Examples of some of the areas ofapplication are:Identification of synthetic polymers
Bacteriological identification
Characterization of natural polymers
Forensic applications such as fiber or paintcross-matching
There are two major types of pyrolysis
units:
1. Continuous–mode pyrolyser –Essentially an on-line inlet furnace whichis continuously heated to the desired
pyrolysis temperature. SGE’s Pyrojector II isan example of this type of system. The
sample is injected directly into the furnace
using special types of syringes. The
advantages of this system are that thepyrolysis conditions can be controlled very
accurately and reproducible sample sizes
are more easily achieved.
2. Pulse-mode pyrolyser – The sample isplaced directly onto the cooled element at

the pyrolysis probe tip. The probe is theninserted and sealed into the inlet and theelement is rapidly heated (at a uniformrate), to the pyrolysis temperature range.
Pulsed systems have the disadvantage thatthe exact temperature is not measurable
and pyrograms are more hardware
dependent. In addition, small sample sizes
are more difficult to control.
General Considerations
The pyrolysis profile obtained is a functionof the individual type and design of thepyrolyser and the gas chromatographconditions. There are several factors thatwill affect the pyrogram profile andreproducibility. Among these are:Temperature control: Dependent on
pyrolyser design and hardware
considerations. (Furnace ID, length ofheated zone, etc).
Pyrolysis furnace gas flow: The gas flowrate determines the residence time of thesample pyrolysis products in the furnaceand may affect secondary pyrolysis.
Sample size: Best results are achieved withvery small sample sizes, which minimize
the occurrence of secondary reactions.
Pyrolyser/GC Interface: Choice of the GC
inlet type is important, primarily due tofactors such as discrimination and thewidth and size of the sample band as it isintroduced into the column.
SGE’s Pyrojector II has been developed withall these considerations in mind to give
reproducible pyrolysis.

Pg 2

3.0 INSTALLATION

Before commencing installation, please check all items listed on the packing list (page 12)
have been supplied. Contact your local SGE office or supplier if any parts are missing.

3.1 FURNACE ASSEMBLY
For shipment, the furnace is packed in a
number of pieces and requires assembly.
Refer to Figure 1 for the diagram of thefurnace assembly.
Insert a plug of quartz wool (6) into one of
the quartz furnace liners (3) to form a bed
approximately 5mm thick. This plugshould be positioned to be in the centre of
the furnace once installed.

quartz furnace liner into position. (It isessential that the quartz furnace liner isfully located into the end of the transfer
tube end fitting to avoid creating a large

dead volume.) Tighten the adapter
finger-tight, then one half of a turnwith a spanner.

Figure 1

This plug of quartz wool is required toprevent the sample from passing throughthe furnace into the cooler, lower part of
the tube without undergoing satisfactory
pyrolysis. The quartz wool is also of use toprevent particulate matter falling down
into the transfer line, resulting in blockages.

The Pyrojector II is supplied withthree different sample injection
heads:• Septum injection head
• Septumless injection head
• Pelletizer injection headSee section 4.5 on page 7 for a guideto selecting the most suitableinjection head for your application.

Carrier Inlet'C'
1. Septum Cap
Septum Purge 'P'
Spacer

2. Injection Head
3. Quartz Furnace Liner
4. Heat Shield
5. Furnace Assembly
6. Quartz Wool
Thermocouple

Lay the furnace on its side and slide thequartz furnace liner packed with quartz
wool into the furnace. (The liners are
symmetrical and can be inserted eitherway).
Fit a 1/4" graphite ferrule with 6mm ID(11) onto the outlet end of the quartz
furnace liner (3). The tapered end of theferrule should face into the baseplateassembly (7). (See Figure 1)
Insert the transfer tube (10) into the GC
instrument specific adapter (8) and screw
the adapter onto the baseplate to lock thePower Cables

Spacer

Cable Clamp
7. Base Assembly
8. Adaptor Unit
9. Septum

11. OGF4-06.
Graphite Ferrule

10. Transfer Tube

Existing GC Injector PortPg 3

Slide a 1/4" graphite ferrule with 6mm ID(11), taper first over the quartz liner at the
top of the furnace and screw on theselected sample injection head. Finger
tighten at first and then a further half turnwith a spanner.
CAUTION: Do not overtighten thefittings as damage to the furnace
liner may result.
3.2 INSTALLATION ON THE GC
INJECTOR
There are a range of instrument specificadapters (8) available to suit the injector ofmost commercial gas chromatographs.

Before proceeding any further, ensurethat the gas chromatograph has been
turned off and that the injection port
has cooled to room temperature.
Turn off all gas flows and allow any
pressure in the system to equilibrate
to pressure.
(See section 7.0). The type of GC injector
that the Pyrojector II is to be used withshould have been specified at the time ofordering the Pyrojector II.
Remove the GC injector’s septum cap andseptum. (Store these items as they will be
required when the pyrolyser is not being
used.)
Fit a new triple layer septum (9) into theinjector and slide it over the transfer tube
(10) on the furnace. (The septum size
should be the same as normally used on
the injector). Slide the transfer tube into
the injector port of the gas
chromatograph. Fasten the furnace byscrewing down the instrument specificadapter (8).
Note: Be careful to allow theinjection head assembly on top of
the furnace to turn freely.
3.3 MAIN CONTROL MODULE
3.3.1 Main Voltage Selection
Before connecting the control module tomains power, ensure the correct voltage tosuit the supply in the laboratory has been
set. This is indicated on the voltage selector
on the rear panel of the instrument. Insert

the correct fuse:– 800mA for 240 volt systems– 1.25A for 110 volt systems
MAIN ELECTRICAL CABLE
The power cable must be fitted with thecorrect plug to suit your electrical power
outlet.

Note: Local electrical regulations for
power cabling must be compliedwith. It is the responsibility of theuser to ensure that the correct powerplug with an earth connection is
attached to the mains lead.
3.3.2 Gas Connections
Locate the Pyrojector II control module at aconvenient place on or near the gas
chromatograph.
Connect a 1/8" gas supply line from themain carrier line to the rear of the control
module. Use a 1/8" graphite front ferrule forsealing.
Two 1/16" lines should be connected to the
PYROLYSIS GAS OUT and SEPTUM PURGE IN
on the rear of the control module using
1/16" vespel sealing rings. These lines arethen connected to the injection head (2) on
the furnace.
(Ensure the pyrolysis zone of the injection
head is blocked off.
- in the septum injection head a
septum should be in place;- with the pellitizer injection head the
supplied plug should be in place;- with the septumless injection head theseal is closed.
When the gas connections are complete, andbefore heating of the furnace is commenced,
pressurize the system and check for leaks
around all connections.
(It is recommended that the outlet of the GC
injector be blocked and the system pressurized.
Then turn off the gas supply and monitor the
supply pressure – any leak will result in a dropin the pressure reading).
If hydrogen is to be used as the carrier gas it is
the responsibility of the user to take allnecessary safeguards with respect to safety.
SGE does not recommend the use off hydrogenin this system. Hydrogen leaks will result in afire and it should be noted that hydrogenburns with an invisible flame.

Gas Leaks must be eliminated before
proceeding with the operation of thesystem.

Pg 4

3.3.2.1 Septum Injection Head andPelletizer Injection Head
The connections are made as follows
using 1/16" vespel sealing rings
provided.

Figure 2

12. spring

Module Injection Head
Pyrolysis gas out to “C”
Septum purge in to “P”
3.3.2.2 Septumless Injection Head
The PYROLYSIS GAS OUT from the rearof the control module is connected tothe "carrier in", as shown in Figure 2.

13. poppet
14. 1/16 stainless steel nut
15. 1/16 vespel sealing ringMTV-3 connection
16. pnumatic head
17. seal

The SEPTUM PURGE IN on the module isconnected to the purge point on thepneumatic head.
To operate the pneumatic seal in the
septumless injection head a means ofswitching gas to the pneumatic headneeds to be installed.
Connect a 1/16" OD compressed gas line
to the pneumatic head (16) using a
1/16" stainless steel nut (14) and 1/16"
vespel sealing ring (15). The line is then Purge Inlet
connected using a 1/16" vespel sealing
ring to the MTV-3 toggle valve as
illustrated in Figure 3.
A 1/16" line is then connected to thebase port of the MTV-3 valve to acompressed gas source of not more than
100psi, but not less than 50 psi. Again
Carrier Gas Inlet
use a 1/16" vespel sealing ring. The
MTV-3 should be installed in aconvenient position.
3.3.3 Furnace Power Cable
The power cable from the furnace
incorporates the low voltage heater powerlines and the thermocouple wires. Plug thecable into the rear of the control unit.

Figure 3
Vent
ClosedPneumatic
Connection
Compressedgas supply
Gas InOpen

Pg 5

4.0 OPERATION

Figure 4

4.1 FRONT PANEL CONTROLSPURGE Used to set the septum purge flow to
0.5 - 1 mL/min. Flow may be measured at therear panel.

PYROLYSIS TEMPERATURE ºCPYROJECTORPRESSURE Regulator for setting the pressurein the pyrolysis furnace. Usually set to 5psi
above the column pressure.
FURNACE PRESSURE Indicates the pressure
at the inlet to the furnace. (psi)
TEMPERATURE SET
Pressing either the up or down TEMPERATURE
SET buttons displays the set point temperatureof the temperature control circuit (˚C).
4.2 REAR PANEL CONNECTIONSFURNACE PRESSURE

PURGE
PRESSURE

TEMPERATURE SET

Figure 5
COVER
WARNING:
ELECTRIC SHOCK HAZARDDISCONNECT INSTRUMENT POWER
CORD BEFORE REMOVINGCOVER

FURNACE240

SEPTUM PURGEPYROLYSIS GASPYROLYSIS GAS IN Inlet carrier gas line for
furnace pyrolysis gas.
PYROLYSIS GAS OUT Outlet carrier gas line
to be connected to the furnace purge head
connection "C".
SEPTUM PURGE IN Septum purge line
connector from the septum purge outlet on the
furnace purge head connection "P".
SEPTUM PURGE OUT Outlet port for checking
the purge flow and venting the septum purge gas
to a safe disposal area.
MAIN SWITCH/FUSE Main power inlet andfuse holder. Use the following fuse:– 220/240V 500mA– 110/120V 1.0amp
FOUR PIN SOCKET Power socket for furnace
supply and temperature sensor.
VOLTAGE SELECTOR Allows selection
between 120V and 240V.

IN

OUT

4.3 GAS FLOWS
Optimize the gas flows on the GC to thosesettings required for the particular analysis andallow the oven, detector and injector
temperatures to reach their set point.
Adjust the pressure control on the Pyrojector
II’s control unit to give a pressure reading on
the control unit pressure gauge of 5psi abovethat of the column head pressure. Refer to theoperating hints section to provide anindication of the effect of gas flow.
4.4 TEMPERATURE SETTING
The digital temperature controller used in the
Pyrojector II is a microprocessor developed
specifically for the SGE range of instruments.
The “temperature set” facility built into thiscontroller incorporates both a fast and slow
scroll modes to allow for easy temperature
setting over large temperature ranges.
To set the desired temperature, press either theup or down button labeled “TEMPERATURE
SET” on the lower left side of the front panel. It
will automatically display the set temperature.
Press the set button once and the temperature
controller will be activated in the fast scroll
mode. Press the set button a second time andthe temperature controller changes into theslow scroll mode. With the set buttons released,
the temperature controller will display the set
temperature for a few seconds and thenautomatically change back to displaying theactual temperature.
4.5 SAMPLE INJECTION
Three different sample injection heads are

Pg 6

supplied with the Pyrojector II. Each is intended
for a particular type and size of sample.
4.5.1 Conventional Septum Injection
The sample is injected through a septum.
The pyrolysis zone is always sealed fromexternal air. A conventional syringe, with aneedle diameter 0.75mm or less, may be
used for injecting liquid samples or samples
in solution.
4.5.1.1 Low Viscosity Liquid Samples

Figure 6
Seal

Spiraldart ejected. Loose darts can be recoveredat a convenient time from the furnace
when cleaning or replacing the liner.

Figure 7

SampleDart

4.5.1.4 Pelletizer P-1
Withdraw the long plunger from thePelletizer barrel and ensure the shortplunger is inserted into the narrow end of
the barrel. Insert (or pour) sample into thewider bore of the glass barrel forming apellet by compacting the sample between
the ends of both plungers.

For low viscosity liquids, or samples
dissolved in volatile solvents, aconventional syringe is recommended.
(SGE does not recommend using plungerin-needle syringes due to the hightemperatures in the furnace, which could
cause the plunger to bind in the needle.)
When using the septum injection head, aneedle of 7.5cm length is recommended.

At this stage, for certain samples e.g.
Thermoplastics, a denser pellet may be
moulded by gently heating the barrel while
the sample is under compression between
the two plungers.

4.5.1.2 High Viscosity Liquid Samples
For liquids that have a high viscosity, or
contain a high level of suspended
material, we recommend the use of the
SGE Solids Injector (7.5cm) with a spiralplunger (p/n 009982).

Transfer the pellet to the solids injector byinserting the longer plunger into the smallbore of the Pelletizer and forcing the pellet
into the needle.

Samples in a solution are applied to thespiral section of the plunger. The solvent is
evaporated depositing the solid on the
spiral section of the plunger, which is thenretracted into the needle. The injection port
is then penetrated and on depressing theplunger fully the sample is carried into theheated injection port.

Withdraw both plungers and insert theneedle of the solids injector, with its
plunger retracted, as far as possible into thelarge bore of the Pelletizer barrel.

Insert a dart into the end of the needle,
after withdrawing it from the Pelletizer,
and inject the sample into the furnace.

Figure 8

4.5.1.3 Solid Samples
Solid samples in the form of granules,
fibers and powders can be packed into thebore of the solids injector needle with theplunger retracted. Alternatively, samples
can be cut out with the sharp tip of theneedle or pressed into pellets using thePelletizer.
When solid samples are being introduced,
the supplied solids injector (7.5cm) withthe flat tipped plunger may be used. It is
recommended that a dart is used in theend of a solids injector syringe when
injections through a septum are being
performed. This guides the needle throughthe septum, preventing septum material
being deposited in the pyrolysis zone.
After penetrating the septum, the plunger
is depressed, and both the sample and thePg 7

4.5.2 Septumless Injection
Solid samples may be introduced using
the solids injector (Needle &Plunger_11cm) kit (supplied), by changing
over the needle and plunger. (This is toensure the sample is ejected into thecentre of the furnace).
Because the seal is opened pneumaticallyas the syringe needle is inserted into theinjector, there can be no damage to theseal by the needle. This has the advantagethat it is not necessary to cool thepyrolysis zone regularly to remove
accumulated darts.
The septumless injection head may be
used with needles up to 0.7mm diameter.
For preparation of the sample for injection
the instructions as for the septum injection
head should be followed in sections 4.5.1.3
and 4.5.1.4. The exception is that darts
are not required when the solids injector isbeing used to introduce solid samples.
(See Figure 2)
4.5.2.1 Operation of Septumless
Injector
1. Set the required conditions for thechromatograph and the Pyrojector II.
2. After the pyrolysis temperature hasstabilized, take the sample into thesolids injector as described in section
4.5.1.3 or if a liquid sample, into a
conventional syringe with a needle
diameter less than 0.7mm.
3. Gently introduce the syringe needle
into the poppet (13) until it meets theresistance of the seal.
4. Actuate the toggle valve to introduce
the compressed gas into the pneumatichead. The poppet will lift against the
spring (12) allowing
the seal (17) to open which allows theneedle to be passed through into theinjection area.
5. Immediately close the toggle Figure
3, make the injection swiftly andwithdraw the needle.

Figure 9
18. Precision bore glass tube
19. Long plunger
20. Short plunger
21. Black injector cap
18

22. o-ring seal

19

23. Pellitzer body
24. Septum Purge In
25. Nut
26. Ferrule “C”
27. Pyrolysis Gas Out
28. Plug
28
20

21

22
27

25
26
26
25

23

24

NOTE: It is not necessary to reopen theseal to withdraw the needle.
4.5.3 Pelletizer Injection
The sample size of solids introduced by theabove methods is limited to a few milligrams.
In some instances it is necessary to introduce
larger sample sizes than this. This is most
likely when the sample under investigation
has a low level of organic matter present e.g.
when geochemical samples such as coals,
petroleum source rocks and recent sediments
are being examined.
SGE has designed the Pelletizer Injector(P-3), for the introduction of this type ofsample, with an inside diameter of 1.6mm. It
is ideal for sample sizes up to 10 milligrams.
The P-3 Pelletizer consists of a precision bore
glass tube (18), a short plunger (20) to help
compress the sample and a long plunger (19)for expelling the solid sample into the
Pyrojector II furnace. (See Figure 7)
The Pelletizer Injection Head is installed as
detailed in Section 3.1.
Pg 8

4.5.3.1 Operation of Pelletizer
Injector
1. The solid sample to be analyzed
needs to be in a cut up or ground state,
so that it can be introduced into the P-3
glass pelletizer tube (18). Do not
attempt to deposit too much sample in
the tube so that the plug cannot be
moved easily when pushed with theplunger.
2. When the sample has been placed in
the tube it should be gently compressedusing the two plungers. The shorter of
the two plungers should be inserted in
the end of the glass that is grooved. Do
not overcompress the sample, as thiswill make it difficult to expel thesample from the pelletizer into thefurnace. (Overcompression will also
affect the dispersion and rapid heatingof the sample in the furnace.) Remove
the short plunger from the glass tube.3.
With the furnace carrier gas turned off,loosen the black injector cap (21) andslide the grooved section of thepelletizer tube into the o-ring seal (22)in the injector head. Firmly tighten theblack cap and set the correct pyrolysis
gas pressure at the control module.
Check that the septum purge isapproximately 1-2mL/min.
4. When the conditions in the gas
chromatograph are ready for injection,quickly depress the P-3 plunger so thatthe sample is rapidly expelled from thetube into the hot quartz furnace liner. It
is important that the sample is sent all
the way into the middle of the hot
furnace zone and caught in the quartz
wool.
5. Leave the glass pelletizer with theplunger depressed in the injector head
until the GC run is finished and the GC
column is cooling down. Then thepyrolysis gas can be turned off and theblack septum cap can be loosened andthe pelletizer removed.
6. A plug (28) is provided to block theopen end of the quartz lined pyrolysis
zone while the P-3 pelletizer has been
removed for cleaning or sample
loading.
7. Before the next sample is prepared
ensure that the pelletizer tube is clean
and free of particulate material.
Because the plunger is a very accurate
fit in the glass barrel any remaining
material may jam the plunger andpossibly crack the glass.

4.6 FURNACE REMOVAL AND CLEANING
Periodic cleaning of the quartz furnace liners is
required to prevent the build-up of excesscarbon residues in the liner and for theremoval of accumulated darts from the solids
injector. (A deterioration of peak shape will
begin to become evident when approximately
10 darts have accumulated in the quartz
furnace liner).
4.6.1 Quartz Furnace Liner Removal
Caution: Before removing the furnace
turn off the electrical power to thecontrol module and allow thetemperature of the furnace to cool.
When the furnace is sufficiently cool,turn off the gas flow to the furnace fromthe control module.
Turn off the gas flow to the injector of thegas chromatograph. Use the heat resistant
gloves supplied, to prevent burns. Loosen
the instrument specific adapter (8) byunscrewing it half of a turn from thebaseplate assembly (7). Undo the injection
head (2). Carefully lift the injection headup from the quartz liner and lean it to theside. Gently pull the furnace liner out of
the furnace.
Note: Even with the protective gloves,
make sure the furnace liner has cooled
before attempting to hold onto it.
4.6.2 Quartz Furnace Liner Cleaning
Push the quartz wool out of the furnace anddiscard it in a safe receptacle. Reclaim thedarts and clean by washing with detergent
and water. (Or a proprietary cleaning agent
and an ultrasonic bath.) Clean the quartz
tube by rinsing with detergent and scrubbing
with a pipe cleaner or thin brush. (It may benecessary to clean it with a proprietarylaboratory cleaning agent and an
ultrasonic bath.)
Replace the quartz wool plug (using fresh
quartz wool every time), ensuring that it islocated approximately half way down
the liner.
4.6.3 Quartz Furnace Liner
Replacement
Re-insert the clean quartz furnace liner bypushing it through the furnace and locating
it in the instrument specific adapter (8). It is
most important that the furnace liner islocated correctly at the top of the transfer
tube (10). Tighten the instrument specificadapter (8) half a turn into the baseplateassembly (7) to secure the liner and make agas tight seal. Reposition the injection head(2) and tighten the nut with a spanner ahalf turn to seal the assembly to the liner.
Pg 9

4.7 SYRINGE MAINTENANCE
4.7.1 PTFE Seal Replacement
Each Syringe and Repair Kit is supplied witha spare PTFE Seal Tube and Insertion Tubeassembly – see Figure 8.
As illustrated, a small PTFE tube seal (6) islocated inside the glass barrel, around theplunger, and located at the back end of theneedle. Generally, this seal should not
require replacement, but if it becomes
dislodged or damaged it can be replaced.
Is The Seal In Position?
To check, simply remove nut (33) and spring(31) leaving the needle (30) and plunger
assembly still inside the glass barrel (35).
Gently push needle into the barrel (35). If
the 1.5mm long PTFE Tube Seal (34) is
missing, the needle stop (32) will rest flush
against the face of the glass barrel. If theseal is in position the needle stop (32) will
protrude about 1.5mm from the face of theglass barrel as illustrated in the schematic
drawing.
Seal replacement can be made as follows:1. Loosen syringe nut (33) and withdraw
plunger assembly.
2. Remove nut (33), needle (30) and spring(31) as illustrated.
3. The seal insertion tool is supplied
assembled as illustrated, and consists of astainless steel tube (40) wire (41) and PTFE
seal (34).
4. Hold Insertion Tool assembly in one
hand and syringe barrel in the other andinsert the seal (34) and tube (40) into thesmall hole in the glass barrel where theneedle normally fits. Then withdraw wire(41) about 5mm, which will leave the seal
in position. Remove the insertion tool
5. Replace needle (30) and nut assembly
ensuring spring (31) is located against
stop (32).6. Refit plunger and then tighten
nut.
4.7.2 Plunger Replacement
1. Loosen nut (33) and withdraw plunger
assembly from syringe.
2. Firmly hold threaded section (38) on
guide tube (37) and unscrew button (39).
Pliers may be required.
3. Push out plunger wire (29) andstrengthening sheath (36) throughthreaded section of guide tube (37).
4. Fit new plunger and lock into position
with button (39).
5. Insert the plunger assembly down levelwith the zero mark on the scale.
6. Tighten nut.
7. Thoroughly clean needle before use

Figure 1029Type B Syringe30

31 32 33

29

36

34

35

34

37

38 39

40

41

PFTE Seal Insertion Tool
4.8 DIGITAL PRESSURE METER.
Optimum performance in pyrolysis capillarychromatography requires accurate and precise
measurement of furnace gas pressure. The
Pyrojector II ’s Digital Pressure Meter
implements a solid state pressure transducer
capable of measuring gas pressure from 0 to
100psi(0 to 690kPa) with a resolution of 0.1psi(1kPa).
To change the pressure units from psi to kPa,
remove the covers to gain access to Digital
Meter Circuit Board. Find the jumper blocklabeled J1 & J2 (see wiring diagram). Removalof jumper J1 allows measurement in kPa.
CAUTION: Ensure no power is supplied tothe unit when removing the covers.

Figure 11
Pressure Meter Circuit Board

J1
J2

Pg 10

5.0 OPERATING HINTS
The pyrolysis products obtained primarily
depend on two things:- The temperature in the pyrolysis
furnace.
- The residence time of the sample in the
furnace.
With the Pyrojector II, both of these parameters
may be adjusted to obtain the required
pyrolysis profile.
As an example:
The chromatograms on page 18 show the effectof changing the pyrolysis temperature on the
breakdown of n-Butyl Benzene dissolved inpentane.
For reproducible pyrolysis, the flow of gas
through the furnace must be well controlled. In
the Pyrojector II, this is achieved with arestrictor in the transfer tube between the
furnace and the GC’s injector. The pressure in
the furnace is controlled separately from thepressure in the gas chromatograph’s injector.
The pressure in the furnace should be set above
the pressure in the GC injector.
A differential of approximately 5psi (35 kPa) is
a good starting point but it can be altered tochange the pyrolysis products.
Increasing the pressure differential decreases
the sample residence time in the furnace
because the flow rate through the furnaceincreases. In this situation the degree ofpyrolysis is decreased. The degree of pyrolysis
can be increased by reducing the pressure
differential to increase the sample residence
time in the furnace.
Where non-reconcentrating gas
chromatography injection techniques are being
used such as split or direct injection, thepressure differential must not be too low. For
non-reconcentrating injection techniques it is arequirement that the sample is introduced onto
the chromatography column in a narrow bandso that there is a minimal contribution to peakbroadening from the sampling technique. If
the flow in the pyrolysis furnace is too low thesample takes an excessive time to transfer onto
the column and is spread along the column,
resulting in broad peaks and loss of resolution.
(When reducing the pressure differential, watch
for signs of peak broadening).
5.1 TEMPERATURE PROFILES
If any changes are made to the column headpressure, the pressure in the pyrolysis furnacemust also be adjusted to maintain the same
pyrolysis conditions.
Where a split type injector is used, the split
flow may be changed within a range without
affecting the pyrolysis conditions. Dependingon the design of the injector, if the split flow isincreased excessively, the pressure in theinjector may drop slightly, increasing thepressure differential and thus increasing theflow in the pyrolysis furnace, which may
slightly change the pyrolysis conditions.
If identification of pyrolysis products is required,
standards can be injected into the Pyrojector II
using the following technique. The furnace
temperature should be dropped to a level atwhich breakdown of the standard will notoccur. The standard may be injected as a liquid
or in solution and can be injected using a
conventional microliter capacity syringe. The
retention time of the resulting peak can becompared with the pyrogram.
5.2 CRYOGENIC OPERATION
For some injection modes, and where theresidence time of the sample in the pyrolysis
furnace is likely to be excessive, it will benecessary to focus the pyrolysis products at thestart of the column. If the products of interest
are non-volatile, it may be possible to do thissimply by using a reduced initial temperaturein the GC column oven. It will then benecessary to do a temperature programmed GC
run.
If it is necessary to focus more volatilecomponents on the column, then cryofocussing
will be necessary using liquid carbon dioxide
or nitrogen.
SGE has available the following cryogenic
accessories to allow cryofocussing to be carriedout.
1. The cold trap kit-CO2(p/n 093346) is for use with liquid CO2 and issuitable for the majority of applications where
cryofocussing isrequired with the Pyrojector II.
The coolant flow is controlled by a special
valve, which is pneumatically actuated. The
actuation of the valve is controlled through apneumatic switch (supplied with the cold trapkit) or a solenoid valve which can be operated
through the external events of an integrator
or gas chromatograph.
2. The cold trap kit-N2(p/n 093345) is used where lower temperatures
are required and uses liquid nitrogen forcooling. This option would be required where
cryofocussing of volatile components in ovens
having a relatively high temperature isrequired. Operation of this system is similar to
the CO2 cold trap system.
3. Indirect Cryogenic Cold Trap(p/n 0933451), the indirect system allows the
choice of coolant to suit the application.
Anything from liquid nitrogen to alcohol/dry
ice or even ice/brine mixture may be used.
For further information, request PD-0044-A.
"Cryogenic Cold Trap – Easily installed kits for
Cryofocusing in Gas Chromatography."Pg 11

6.0 SERVICE
6.1 PACKING & REORDER LIST
This packing list is to be used as a reference when checking the contents of your kit. Any
items missed during shipment can be requested from this list.
DESCRIPTIONQUANTITY

REORDER PART NO.

Control Module1

0950301

Furnace

10950220

Power Lead (no plug)

1

Installation and Operation Manual1

Kevlar Gloves1

MN-0280-E

Pyrojector Accessories Kit:
- 1/8" Graphite Ferrules (Pkt 5)- Spanner, (1/4" x 5/16"AF)- Spanner, (1/2" x 9/16"AF)- 1.25A Slo Blo Fuse
- 800mA Slo Blo Fuse
- 10mL Syringe- Pellitizer Injector (P1)
- Pellitizer Injector (P3)- Solids Injector (SI-1)- Pre-Drilled 10mm Triple Layer Septa (Pkt 10)- 1/16" Graphite Vespel Ferrules/0.8mm ID (Pkt 5)- 1/16" Vespel Sealing Rings (Pkt 10)- O-Ring, Silicone (Pkt 2)- O-Ring, Nitrile (11mm)- O-Ring, Nitrile (3mm)- Transfer Tube
- Needle Seal (Pkt 5)- Quartz Tube for Furnace- Pellitizer Injection Adaptor- Septum Injection Adaptor- Septumless Injection Adaptor- MTV-3 Toggle Valve- Deactivated Quartz Wool
- Seat Removal Tool
- Solids Injector (Needle & Plunger Kit_11cm)- 1/4" Graphite Ferrules with 6mm ID (Pkt 10)- Steel Darts (Pkt 5)

1
1
2
1
1
1
1
1
1
1
2
2
1
1
1
1
1
2
1
1
1
1
1
1
1
1
1

Installation Accessories Kit:
- Stainless Steel Tubing (1/16" x 0.8mm ID x 5m)- Copper Tubing (1/8" x 1/16" ID x 5m)- 1/16" Graphite Ferrules (Pkt 10)- 1/8" Graphite Ferrules (Pkt 5)- 1/8" Graphite Vespel Ferrules/1/16" ID (Pkt 2)- 1/8" Extended Stainless Steel Nut (Pkt 2)- 1/16" x 1/16" x 1/16" Stainless Steel Union Tee- 1/8" x 1/8" x 1/8" Stainless Steel Union Tee- 1/8" x 1/16" Reducing Union-1/16" x 1/16" Stainless Steel Union

18030003
18030001
0020600099860099880099820418550726550726530401100401080401030950205
09321640
095012018060001
1236101
03162891
0726212031765096030

1
1
1
1
1
1
1
3
1
1

Solid Sampling Kit:
- Sample Injector Adaptor- Quartz Tube Adaptor- Punch/Probe Adaptor- Injector Head
- Injector Head Cap- Quartz Tubes (Pkt 50)- 1/16" Extended Stainless Steel Nuts (Pkt 2)- 1/16"/1.0mm ID, PTFE Ferrules (Pkt 2)- O-Ring, Nitrile (Pkt 2)- 1/16" Graphite Vespel Ferrules (Pkt 2)0726020726030726020950204
1
1
1
1
1
2
1
1
1
1

0950095

072661The Pyrojector II is supplied with one adapter for interfacing the pyrolysis furnace to the GC injection system.

Pg 12

6.2 FAULT FINDING
6.2.1 Electrical Faults
Failure of the thermocouple or the furnace element are the most likely areas where faults candevelop. The following table should assist in the location of a problem.

Fault

Possible Cause

Action Required

No readout

No power to control
moduleCheck power is available to unit
Check main cable
Check fuse for rating and continuity
Check voltage selector

Transformer failure

Test continuity of transformer wingdings

Thermocouple failure

Replace thermocouple

Thermocouple not locatedcorrectly in furnace

Refer to thermocouple
replacement instructions

Temperature Controller
readout shows excessivein temperature display

6.3 FURNACE REPLACEMENT
Failure of the furnace element requires complete
replacement of the furnace. The normal DC
resistance of the furnace element isapproximately 7-9 ohms, but this will increase
with time due to erosion of the filament.
It is recommended that the resistance bemeasured before purchasing a replacement
furnace to ensure that the furnace has in fact
failed.

4. Remove the instrument specific adapter unit
(8) from the baseplate assembly (7).
The replacement furnace assembly (partnumber 0950220) includes the heatshield (4),the baseplate assembly (7) and thethermocouple/power cable and plug.
The furnace assembly can be reinstalled byfitting the quartz furnace liner, adapter unit
and injector head as detailed in the
installation instructions in section 3.1.

1. Caution: before attempting to replace
the furnace make sure that the gases
are turned off.
2. Unplug the connector from the rear of thecontrol module.
3. Disconnect the carrier gas and purge lines
to the injection head. Loosen the adapter by
unscrewing the nut half of a turn. Then undo
the injection head. Carefully lift the injection
head up from the quartz liner and place it to
the side. Gently pull the furnace liner out of
the furnace.
NOTE: Make sure the furnace has cooled
sufficiently before handling it.

Pg 13

6.4 THERMOCOUPLE REPLACEMENT
Thermocouple failure is indicated by 0 or 1
displayed on the temperature controller
display. The thermocouple can be replaced andis available upon request.
Caution: before attempting to replace
the thermocouple, make sure that thewhole system including the gas
chromatograph is turned off and allelectrical power and gases are turnedoff.
1. Unplug the connector from the rear of thecontrol module.
2. Disconnect the carrier gas and purge lines
to the injection head. Loosen the adapter by
unscrewing the nut half of a turn. Then
undo the injection head. Carefully lift the
injection head up from the quartz liner andplace it to the side. Gently pull the furnace
liner out of the furnace.

13. Push the thermocouple up into thefurnace until it is located approximately inthe middle of the furnace.
14. Replace the baseplate making sure thethree spacers are correctly located on thespacer rods between the furnace and thebaseplate and that the cable clamp is
located directly below the cables. Screw thespacer rods into the baseplate and lock into
position with the locknuts.
15. Replace the cable clamp ensuring thatthe thermocouple wire is located next to thescrew and held in place by the power cable.
16. Replace the furnace as detailed in the
installation instructions in section 3.1.

NOTE: MAKE SURE IT HAS COOLEDSUFFICIENTLY BEFORE ATTEMPTINGTO HANDLE IT.
3. Place the furnace assembly on the bench
and undo the cable clamp and the otherscrews on the base assembly.
4. Remove the faulty thermocouple from thefurnace being careful to ensure that all thewire is removed from the surface.
5. Push the rubber sheath back from thebody of the cannon plug and unscrew thecable clamp screw.
6. Loosen the screw from the body of theplug by turning clockwise into the plug.
Push the cable assembly through the body
until the rear of the pins are exposed.
7. Unsolder the thermocouple from pins 2
and 3.
8. Pull the faulty thermocouple wires out of
the cable sheath and discard them.
9. Push the welded end of the newthermocouple wires through the plug, rubber
sheath, and then through the cable sheath.
10. Solder the loose ends of thethermocouple wires to pins 2 and 3 of thecannon plug.
Note the following polarities:
PIN 2:RED BRAIDPIN 3:YELLOW BRAID
Check resistance is 3.5 – 5 ohms
11. Push the pin assembly into the plug
body and secure with the screw. Screw in thecable clamp screw to hold the cables andrelieve the strain on the pin connections.
12. Replace the rubber sheath on the end of
the plug.

Pg 14

7.0 PYROJECTOR II- GC INJECTOR ADAPTORS

Instrument Description

Part No.

Antek 3000
PE 8300, 8500
PE F30, 900/10/90
Sigma
Konik
Pack Beck 437-439
Pack Beck 436
Varian 3700 - Packed
Vista 6000 - Packed
Varian 3700 - Capillary
Vista 6000 - Capillary
Tracor 560/65/70
Varian 33/34/3500
Varian 3700-1075 opt
Vista 6000-1075 opt
Unijector Mk II
HP–5830-90, 5700-Capillary
HP–5830/40, 5700-Packed
HP–5880/90-Packed
Girdel 3000
Delsi DI700, DI200
Shimadzu 8A-17A
Hitachi 163
Finnigan Tremetrics
Phillips 4400 GC
Shimadzu SPL-14
Carlo Erba
Dani 3000,6500,84/8500
Carlo Erba 4160

0950021095002109500210950021095002109500210950021095004209500420950043
0950043
0950043
0950043
095004509500450950051
09500130950021095001109500520950053095007109500710950080
09500820950085
09500900950091
0950091

Pg 15

Pyrolysis Temperature 600oC

Pyrolysis Temperature 700oC

Components:
1. Pentane
2. Benzene
3. Toluene
4. Ethylbenzene
5. Styrene
6. n-Propylbenzene
7. n-Butybenzene

Pyrolysis Temperature 800oC

Pyrolysis Temperature 900oC

Pg 16

Pg 17

Figure 12

Pneumatic Connections
Pressure Gauge

IN

Pyrolysis
Pressure
Regulator

Pyrolysis Gas

OUTIN
Septum Purge

Septum Purge Valve

OUT

www.sge.com

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Toll Free: 1800 800 167
Tel:+61 (0) 3 9837 4200
Fax:
+61 (0) 3 9874 5672
email:
support@sge.com
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Tel:(800) 945 6154
Fax:(512) 836 9159
email:
usa@sge.com
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+44 (0) 1908 568844
Fax:+44 (0) 1908 566790
email:
uk@sge.com

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Tel:
+33 (0) 1 69 29 80 90
Fax:+33 (0) 1 69 29 09 25
email:
france@sge.com
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Tel:
06 4429 0206
Fax:
06 4429 0724
email:
sge.italia@tin.it
SGE (Deutschland) GmbHTel:
+49 (0) 6151 860486
Fax:+49 (0) 6151 860489
email:
germany@sge.com

SGE China
Tel:+86 (10) 6588 8666
Fax:
+86 (10) 6588 6577
SGE Japan Inc.
Tel:
+81 45 222 2885
Fax:
+81 45 222 2887
email:
japan@sge.com
SGE India
Tel:+91 (022) 471 5896
Fax:
+91 (022) 471 6592
email:
sgeindia@vsnl.com

Publication No. MN-0280-E

Rev:08 10/01