GC Introduction and Review
GC Introduction and Review
Overview GC
Supported configurations
— Empower in General
o 5890, 6890, 7890, 6850
o SSL, PTV, MMI, PPIP, COC
o 7683, 7683B, G1888, 7694
o FID, uECD, NPD, FPD, TCD
6890
7890
To remove the side panels, remove the torx screws and then
slide/push the panel back. (7890 pictured)
To remove the top panel covering the oven, open the lid so it’s
vertical, to allow the clip on the right side to slide out of the
retaining slot. Once this is done slide the left side out from the
retaining slot.
To remove the pneumatics cover, press the black clips on each
side of the cover and lift.
Removing inlet cover, remove the 4 torx screws and lift of the
cover. If there is an autosampler installed this will need removing
first.
To remove the detector cover, unscrew the torx screw, unclip and
lift up. Removing the detector cover exposes the electrometers
which use high voltages. Do not remove any of the electrometers
covers unless the power is disconnected from the rear of the GC.
•Split/Splitless
•Flip top (Easier maintenance)
•Headspace adapter
•Standard injection port
Standard
Septum retainer
Flip Top nut
Septum Assembly
Glass Liner
(with glass wool)
Pieces of septum
O-Ring
(for Liner)
Display panel
Status indicators
Melinda Foland
Thread an inlet nut and ferrule onto the column. Always use the
appropriate nut and ferrule according to the id of the column.
Insert the column into the inlet, holding septa, so that the depth of
the column remains correct. Tighten the nut with a spanner (do not
over-tighten the nut as this will cause the ferrule to crack and cause
leaks).
Once the column has heat cycle, installed the end of the column
to the detector.
When the TCD is exposed to air whilst hot, damage will occur to
the filament, therefore turn the filament off.
When the TCD is exposed to air whilst hot, damage will occur
to the filament, therefore turn the filament off.
Changing a Septum
Caution : The inlet parts are hot, be sure to cool in the inlet
down or wear heat proof gloves to avoid burns to the hands.
When handling the internal inlet parts make sure gloves are
used to prevent contamination.
Inspect and remove any old septa from the inlet by following the
‘cleaning the septum seat’, see further on in the document.
Changing a Septum
Place a new septum into the inlet, and press it firmly down to
seat it correctly.
Carefully wiggle the o ring to loosen it from the inlet body, grip
the liner with a pair of tweezers and gently lift it out of the inlet
taking care not to chip or break the liner.
Also inspect the inside of the inlet to check for any signs of
visual contamination. These can be removed out with a cotton
swab wetted with methanol.
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Use Only reserved.
Split/Splitless Inlet - Maintenance
Take a new liner and slide a new o ring onto the liner. Do not
use the old o ring as these become deformed after use.
Carefully lower the new liner into the inlet using tweezers. Then
gently push the top of the liner using the tweezers until the liner
hits the gold seal.
Close the flip top mechanism, be sure to line up the tab on the
bottom of the mechanism with the slot on the inlet assy. Then push
down and slide the tab to lock down the inlet.
Purge the inlet and column with carrier gas for 15mins before
heating up the inlet and oven.
Its advisable to bake out the inlet after this maintenance – see
bake out procedure.
At the end of this procedure its advisable to check for leaks –
see leak check method.
Remove the GC column and plug the end of the column with a
clean septa to prevent oxygen damage.
Tip out the gold seal and washer from the reducing nut.
Take a new gold seal and a new washer and place them into the
reducing nut, the orientation of the parts is important. The washer
needs to be placed into the reducing nut first, followed by the gold
seal.
The gold seal needs to be installed with the smooth, flat facing
upwards.
G3451A PP Inlet
¼ inch spanner
Metric ruler
Tweezers
Sonic bath
Description Part #
Methanol
Beaker
Column
½ inch spanner
Unscrew the column from the male fitting and the brass
ferrule should fixed in place on the column end.
Wipe the column with lint free tissue soaked with a little
methanol to remove any contamination.
Once the column has heat cycle, installed the end of the
column to the detector.
Changing a Septum
Caution : The inlet parts are hot, be sure to cool in the inlet down or
wear heat proof gloves to avoid burns to the hands.
When handling the internal inlet parts make sure gloves are used to
prevent contamination.
Changing a Septum
With all the insulating material fitted into the cup, and
the slide the spring lever to uncover the hole, slide the
cup slot over the inlet fitting, so that the insulating cup
touches the top of the oven. The release the spring into
the groove so that it is held in place.
Spring
lever
Put a beaker under the inlet inside the oven to catch any
drips of solvent and using a cleaning brush soaked in
solvent rub the interior of the inlet body.
If the column is not installed into the detector cap the
detector using a no hole ferrule and nut or using a
blanking nut.
>6 inches
Check column cut. It must be straight across- no
jagged edges or diagonal cuts. If the cut is bad, re-
trim the column; it is not necessary to take off as
much length.
Good Bad
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Use Only reserved.
Autosamplers
Common practices
— Change the needle
o If alignment is incorrect the needle can bend
and must be replaced
o Plungers can become stuck and the whole
syringe will need to be replaced
o If washes are not set up correctly, the needle
can become contaminated and need to be
replaced
G2913A 7683A
The 7683B ALS for the 7890
is the same as the 7683B for
the 6890.
The ALS main function is to
introduce liquid samples from
the vial rack into the inlet.
The tray can hold 100, 2mlv
vials.
The turret can either hold 1
sample or 8 samples along
with a number of pre and post
wash and waste bottles.
Removing a Syringe
1. Open the injector door
2. Open Syringe guide
(turn up)
3. Loosen Plunger screw
4. Remove syringe from
flange guide
5. Make sure needle
clears the needle
support foot
Syringe clip
Door
Vials
Installing a Syringe
1. Open the injector door
2. Move carriage up (or
down)
3. Insert the needle into the
Needle support foot.
4. Align syringe barrel with
flange guide and syringe
clip. Press syringe into
place
5. Close syringe latch (move
down)
6. Loosen plunger screw
7. Move the plunger carrier
loop down to top of
plunger and tighten
plunger screw.
8. Move the plunger carrier
loop up and down.
Observe if the syringe
plunger moves with the
plunger carrier loop.
9. Check that the needle is
still aligned with the
needle guide.
Plunger screw
Plunger
Flange
Flange Guide
Align Procedure
Usually the align procedure is only necessary when the align
light illuminates orange.
If the align mode is on, the ALS will not inject until the align
mode has been successfully performed.
Wait until the ALS is ‘stationary’, then remove all the bottles and
vials from the turret.
Open the tower door, slide the syringe carriage up until it stops
and remove the syringe.
Remove the ALS mounting post, then remove the calibration
probe from the bottom of the ALS by removing the screw and the
washer
Align Procedure
Usually the align procedure is only necessary when the align
light illuminates orange.
Take out the needle support assy from the ALS and press the
alignment button.
Align Procedure
The GC will display various diagnostic messages during the align
procedure. If any of the steps 1-5 fail the ALS will halt at step 2. If
this happens press the alignment button again to repeat the
procedure. If the alignment procedure fails again, unplug the ALS
and reconnect and repeat the alignment procedure. If fails again
call Agilent.
Once the ALS has stopped, all 4 indicator lights will flash.
Press the alignment button the ALS will go through the following
steps:-
1.The syringe carriage moves down, the turret will rotate to
confirm the probe is fitted.
2.The turret rotates until the calibration hole is under the
calibration probe.
3.The probe moves down and calibrates the turret to the syringe
carriage.
Align Procedure
Note: If the align mode light was not lit before the
alignment button was depressed, and then the alignment
fails, unplug/plug the ALS and the ALWS will restore the
previous ‘ok’ alignment values.
SQT OQ/Manual OQ
Inlet Pressure Decay Inlet gas flow control Pressure change= loses
Chosen by the Compliance < 2.0 psi in 5 minutes
Specialist Pressure change = gains
< 0.5 psi in 5 minutes
Calibrated Thermometer
— GC oven/detector probe
— GC inlet probe
Thermometer:
- display capable of 1.0 OC
- calibrated
Temperature Probe:
- measure at 100 OC and
230 OC ± 2 OC
- calibrated
Inlet Temperature
Probe
— Special probe
design to measure
inside the inlet.
Inserted into
Injection port
GC Oven Probe
— Special flexible
stainless steel
probe
Front/Back Inlet set 250 oC Front Inlet button (Back inlet button)
Down arrow
Feed
probe
through
HERE
GC
Probe temp
sensor
Accuracy:
— Set oven temp to 230OC using front panel
o Wait 5 minutes to stabilize
o Record the temperature on Form 6
— Set oven Temperature to 100OC using front
panel
o Wait 5 minutes to stabilize
o Record temperature on Form 6
— Leave probe in the oven for Stability Test
Stability
— Set oven temperature to 100OC
o Wait 5 minutes to stabilize
o Record temperature at 5 intervals of 4 minutes
on Form 6
• 4th minute
• 8th minute
• 12th minute
• 16th minute
• 20th minute
Inlet
Inlet
— Make sure the inlet adapter is capped
— Set Inlet pressure to 25psi via front panel
— Position the calibrated thermometer on the
inlet such that the tip of the probe is inserted
through the inlet septum (see previous slide)
— Set inlet temperature to 250 OC on front
panel
o Wait 5 minutes to stabilize
o Record the temperature on Form 6
Detector
— Make sure the detector inlet is capped
— Insert the thermometer probe (same as for
inlets) into the FID body. Insert until it
cannot go in any further. (see next slide)
— Ensure the insulator cap is covering the FID
inlet.
— Set detector temperature to 300 OC on Front
Panel
o Wait 5 minutes to stabilize (could take 30 30
min)
o Record the temperature on Form 6
— This test is excluded for the ECD and μECD
detector because of the radioactive isotope
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Use Only reserved.
Heated Zones
Detector
This test often requires patience. Let the detector come
to temperature. Measure after 5 minutes, but often it
takes closer to 30 min. Remove the thermometer and
try again after 10 or 15 minutes.
Accuracy
— Remove the column Inlet and install the
manometer in GC Inlet (see next slide)
— Cap the inlet septum purge with a 1/8 inch
Swagelok cap
— Configure the column dimension from the
front panel of GC (30m x 320um)
— Pressurize the GC with inlet pressure as 25
psi (set value from front panel of GC –
constant pressure mode - splitless)
— Allow sufficient time to stabilize
— Record the value on Form 6
— Accuracy must be ± 1.2 psi of set point
pressure
Decay Test
— Follow procedure for Accuracy test
o Once pressure has stabilized for 5 minutes
Turn OFF the inlet pressure for GC front panel
o Wait 5 more minutes and record the pressure
on Form 6
— Decay must be <2 psi
Flow Accuracy
— Cap the detector inlet (see below)
— Turn OFF all the detector flows except the
one being tested (all must be tested
separately)
— For the type of detector being used, connect
the appropriate flow meter adapter to the
detector’s exhaust
— Wait for the flow meter reading to stabilize
— Record flow in Form 6
— μECD Detector
o Make-up 25 mL/min
Split/Splitless
Liners
Column
Isopropanol
Lab Tissue
Metric Ruler
Tweezers
½ inch spanner
Undo the flip top cap by rotating the yellow clip anticlockwise.
This allows for the septum head to be removed and pushed to one
side to allow the inlet body to be removed.
Unplug the heater cable and carefully un-route the cable from
the cable mounting so that when the inlet is removed it does not
snag.
Detach the helium carrier gas line from the inlet at the split line
filter, taking care not to damage the Swagelok fitting.
Carefully lift the inlet from the chassis and place the inlet onto a
clean piece of paper. Check the insulating material in the bottom of
the chassis, is intact and not broken or damaged.
Whilst the inlet is on the bench, check the carrier gas weldment on
the inlet for any visible cracks.
To refit the inlet, simply reverse the instructions. Lower the inlet
into the hole in the chassis and carefully lower it into position. To
make this easier open the oven door and gently pull on the reducing
nut to encourage the inlet to sit into the correct position.
Once the inlet is seated into the chassis, fasten the three screws.
Re-attach the carrier gas inlet line at the split line filter
and plug in the heater cable. Ensure the cable is re-
routed back into the cable mounting to avoid damage
when the covers are replaced.
¼ inch spanner
Metric ruler
Tweezers
Sonic bath
Description Part #
Methanol
Beaker
Column
½ inch spanner
Parts required
EPC module
Pici needed
With the GC off and the power cable removed from the
rear of the instrument.
Note : if this inlet is replacing another inlet that has been installed in the
same position on the GC the other inlet must be un-configured using the front
GC keypad before this inlet is installed.
During the installation of the inlet ensure an antistatic wrist band is worn and
connect to metal chassis.
With the oven door open, install the bottom cover plate
using heat resistant screws.
If the inlet assy tubing has been wrapped around the
inlet or epc for transportation/packaging, uncoil the tubing
and then offer the inlet into the cavity. Its easier to tease
the inlet into place by gently pulling on the bottom of the
inlet from inside the oven whilst pushing the inlet from
the top.
heater cable
heater connection
inlet screws
Slide the EPC module into place, taking care not to pinch
the cables/tubing. Tidy the tubing from the EPC to the
inlet using the spec at the side of the EPC, ensure the
tubing will not be pinched when the covers/panels are
replaced.
Gas Flows
Air 0 - 800 ml/min
H2 0 - 100ml/min
Makeup gas N2 or 0 - 100ml/min
He
Description Part #
Description Part #
Description Part #
Gasket 5180-4165
Ignitor 19231-60680
Parts required
FID assy
Pici needed
EPC assy
Pici needed
Power off the GC and unplug the power cable from the
rear of the GC.
EPC
mounting
brackets
Now place the FID into the detector cavity, and with the
oven door open gently pull on the bottom of the detector
assy to tease the detector into position.
Take the FID PCB from the antistatic bag and position
the PCB into the LHS of the detector positions on the right
side of the GC.
The FID pcb has notches cut out of the board, and this
allows for it to be aligned with the retaining hooks on the GC
chassis. To fit the FID pcb slide on the board up to ensure the
slots on the pcb fit into the retaining hooks on the chassis. If
the pcb is fitted correctly it will lay flat. Then secure the pcb in
place by tightening the captive thumbscrew.
captive thumbscrew
retaining slots on
the PCB
ignition cable
The new EPC installed for the FID will need calibrating. This must
be done with no gas line connected to the rear of the GC.
Adaptable FID
With all the insulating material fitted into the cup, and the
GC column installed, slide the spring lever to uncover the
hole, slide the cup slot over the detector fitting, so that the
insulating cup touches the top of the oven. The release the
spring into the groove so that it is held in place
adaptable fitting
Place a ¼ inch ferrule and nut onto the adapter nut and
then insert into the detector until it bottoms out.
Thread an inlet nut and ferrule onto the column. Always use the
appropriate nut and ferrule according to the id of the column.
The column should always be cut after the nut and ferrule have
been threaded on.
After heating up the detector leak check the fitting using a leak
checker.
First cool down the heated zones of the oven and the fid
and turn off the gas supplies. pici or instructions keypad
how to. Wear lint free gloves to prevent contamination of
any internal detector parts
3. Remove the 3 T10 screw from the top of the collector
assy
14. Take the upper insulator and place it with the lip
facing upwards
18. Place the collector assy back into the GC taking care
not to damage the inter connect spring and insert the 3
T10 screws and tighten then to 18inch-pounds.
exposed jet
interconnect spring
Place the jet onto a clean piece of paper and either clean
the jet or replace with a new one.
Using a lint free q tip clean the inside of the jet cavity
with some methanol
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Use Only reserved.
FID Detector – Maintenance
Install a new jet, making sure to only handle the new jet
with tweezers. Screw the jet into place using the custom
torx driver. The jet must NOT be over tightened as this
will cause irreversible damage the jet or even the base of
the detector. The jet needs tightening to 10 inch-pounds,
which is 1/6th past finger tight.
1/6th turn
Turn off the FID flame and verify the FID electrometer
is on
Baseline Check
TCD
Description Part #
Capillary columns
Description Part #
.530 column id
Description Part #
.100 and .200 column id
Ferrule, Vespel/graphite, 0.37-mm id 0.1-mm and 5062-3516
0.2-mm capillary columns (10/pk)
Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2-mm, 5181-3323
and 0.25-mm capillary columns (10/pk)
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25- 5080-8853
mm, and
0.32-mm capillary columns (10/pk)
Column nut, finger-tight (for .100- to .320-mm 5020-8292
columns) Connect column to inlet or detector
For all column id
Lab tissue
¼ inch spanner
Parts required
TCD frame
Power off the GC and unplug the power cable from the
rear of the GC.
Route the MSD heated zone cable along the top of the
GC to the RHS of the GC. The cable will need to be route
underneath the detector gas lines and through the
channels, use the main communication grommet to keep
the all the cables together.
Pici
Build the TCD frame by first attaching the manual flow
bezel using the 3 screws provided.
Ensure the metal nibs are retained on the cutout and not
on the oven chassis.
Remove the insulation plug and then using a flat
screwdriver carefully punch a hole into the oven insulation
approximately 1/4inch diameter is ok.
Pici needed
screws
EPC module
supporting slots
Fit the detector module (and EPC) into the TCD frame,
lay the frame on the bench and push the EPC module into
the slots. Ensure the switching valve wire in not pinched,
especially when the frame is place against the instrument.
short piec
tubing
connected
to the
reference
short piece
gas fitting
of tubing
connected
to
longthe
makeup
piece gas
fitting
of
tubin
T manifold assy g
conn
ected
Attach the other short piece of tubing using a 1/8 inch nut to
and ferrule to the makeup gas fitting on the epc module. the
bulkh
ead
fittin
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© 2010 Waters Corporation.
Use Only reserved.
TCD Detector – Installation
Attach the long piece of tubing using a 1/8 inch nut and
ferrule to the bulkhead fitting.
Take the TCD PCB from the antistatic bag and place
onto the pcb frame, match up the notches on the board to
the retaining slots on the pcb frame. Once the board is
laid flat, slide the board right and secure in place with the
thumb screw.
retaining slots
thumbscrew
Fit the TCD pcb cover and secure in place using the torx
screw.
Wipe the column with lint free tissue soaked with a little
methanol to remove any contamination.
Caution : If hydrogen is being used as the carrier gas, switch off the
supply and cap the end of the column to prevent an oven explosion.
If there is a column installed into the inlet but not the
detector, maintain carrier gas flow to prevent column
damage, but only if the carrier gas is helium. If the carrier
gas is hydrogen, turn of the carrier gas supply and plug
the end of the end of the column.
uECD
G3497 uECD
The micro Electron Capture
Detector (uECD) releases ß particles
That collide with the carrier gas
molecules which produce low
energy electrons.
Each ß particle will produce about
100 electrons.
These electrons produce a small current, known as the
reference or the standing current. It is measured in a
pulsed circuit.
When samples molecules are hit by electrons, the
electrons are captured by the sample molecule, creating
negatively charged ions.
When a compound that captures electrons goes through
the detector, the pulse rate rises and is converted into a
voltage and recorded.
The radioactive isotope in the cell is 63Ni.
Description Part #
Description Part #
9/16 spanner
Methanol
¼ inch spanner
Parts required
uECD PCB
uECD EPC
uECD nameplate
Now place the uECD assy into the detector cavity, with
the oven door open gently pull on the bottom of the
detector assy to tease the detector into position.
Attach the vent tube so that waste gas from the uECD
can be vented away via an exhaust system. The tubing
should be placed between the slots in the pneumatics
area and out through the rear of the GC.
Take the uECD pcb from the antistatic bag and position
the pcb into RHS of the detector positions on the right
side of the GC.
fit the uECD pcb here (on the rear detector position)
The uECD pcb has notches cut out of the board, and
this allows for it to be aligned with the retaining hooks on
the GC chassis. To fit the uECD pcb slide on the board up
to ensure the slots on the pcb fit into the retaining hooks
on the chassis. If the pcb is fitted correctly it will lay flat.
Then secure the pcb in place by tightening the captive
thumbscrew.
captive thumbscrew
communication connection
Connect the electrometer cable to the eECD pcb.
The new EPC installed for the uECD will need calibrating.
This must be done with no gas line connected to the rear
of the GC.
Finger tighten the nut and then tighten using the 9/16
spanner until its snug
With all the insulating material fitted into the cup, and
the slide the spring lever to uncover the hole, slide the
cup slot over the detector fitting, so that the insulating
cup touches the top of the oven. The release the spring
into the groove so that it is held in place.
Wipe test kits are available for purchase from Agilent p/n
18713-60050. Items required for the wipe test are
included in the kit.
Once all the filter papers are bagged remove gloves and
wash hands thoroughly with mild soap and water.
Incidents
If an incident whereby the occurrence involving the uECD
(radioactive material) may have caused or threatens to
cause
a.Exposure to dangerous levels of radiation
b.Release of dangerous amounts of radioactive materials
Refer the NRC regulations or follow your local regulations
for advice.
1.Inlet Modules
2.Detector Modules
3.Pressure Control Modules, (PCM)
4.Auxiliary Pressure Controllers, (Aux EPC)
BACK OF GC
Inlet Modules
back
front
Detectors Modules
Slot in Name
Pneumatics
SLOT 1 PCM A
SLOT 2 PCM B
SLOT 5 PCM A (if no PCM in slot 1 and 2)
SLOT 6 PCM C
BACK OF GC
BACK OF GC
Tower Tower
installe installed
d on on the
the front inlet
back
inlet
1 2