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

— SystemQT- for qualification

o 6850, 6890, 7890
o SSL, PPIP
o 7683, 7683B, G1888, 7694
o FID, TCD, uECD

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 7890 – Gas Connections (differences 6890
and 7890)
To make gas connections, making sure they have
the correct gas filters.

6890

7890

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 7890 – Removing Panels

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.

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 7890 – Removing Panels

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.

To remove the back cover to allow access to EPC/PCM modules:

1. Remove the 2 torx screws

highlighted in red
2. Loosen the 2 torx screw
highlighted in blue.
3. Lift the metal cover plate cover
up and off.

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 Intel parts

6890 Injection port

7890A Injection port

•Split/Splitless
•Flip top (Easier maintenance)
•Headspace adapter
•Standard injection port

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 Injection ports

Standard

Septum retainer
Flip Top nut

Injection port assembly

Aka Septum assembly

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 Liner

Do Not handle glass liner, o-ring, or septum with hands.

Always use Tweezers!

Septum Assembly

Glass Liner
(with glass wool)

Pieces of septum

O-Ring
(for Liner)

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 Front Panel

Display panel

Display of oven ramp

during runs

Status indicators

Stop and Start GC runs

Settings for oven,

inlets, detectors, etc.

Status- system status

Number pad for

settings input. Up and
down arrows for setting
navigation.

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 Front panel

Setting Temp Zones

1. Push the button
labeled for the temp
zone you want to set
2. Use the up and down
arrows to find the
exact temp you want
to change
3. Use number pad to
enter new
temperature settings.
Remembering to hit
Enter after each
entry.
 Example
— Oven
— Initial temp: Type
35 Enter
— Use down key to
ramp 1: 15 Enter

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 GC methods

 GC methods for injections should be used

from instrument method of the project.

 Autosampler settings should also be in the

instrument methods within the projects.

 Consult the document for any suspected

issues.

 For Manual OQ tests and troubleshooting

follow the following instructions.

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 Communication Basics

 6890 requires either serial cable or Avocent

box to convert serial to ethernet

 7890 and 6850 are both controlled by

ethernet.

 7890 requires ICS 1.2.2 (download from

Waters website)
 6850 requires ICS 1.2 (download from
Waters website)
 G1888 required Headspace Control Option
2.0 (must be purchased)
 7694 requires Headspace Control Option
2.0 (must be purchased)
 Agilent firmware versions must also be
verified

 If you have full control and

communications, the Run Samples page
should have all read backs active

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Maintenance

Melinda Foland

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 Inlet Maintenance

 Common Procedures: Customer also

performs often
— Installing column
o Details vary depending on inlet
— Change septum
o Must be changed every 100-200 injections
o Septum material makes difference on
longevity
o Sometimes septum nut replaced with Merlin
Microseal- no septum option

— Change inlet liner

o Replacement time varies with samples matrix
and throughput
• Bad matirx- clean more often
• High throughput- clean more often
o Type of liner differs with sample, sample
matrix, and application, so check with
customer before replacing
o Every time the liner is replaced the o-ring
should also be replaced

— Replace Gold Seal

o Not as routine as septum and liners
o Only as needed

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 Split/Splitless Inlet –
Installing a GC Column

 Load the general GC maintenance method.

Take the GC column out of the box. Familiarize with the

suggested operating conditions. Store the QC check sheet safely.
The column will come flame sealed at each end, be sure to
remove at least 1-2cms from each end of the column. Use a
ceramic wafer to cut the column.

To facilitate the installation of the column, thread a clean septa

onto the column.

Thread an inlet nut and ferrule onto the column. Always use the
appropriate nut and ferrule according to the id of the column.

Cut the end of the column using a ceramic wafer to ensure a

clean square cut is achieved. The ceramic wafer has a serrated
and sharp side, use the sharp side to cut the column. Inspect the
quality of the cut using an eye glass. The column should always be
cut after the nut and ferrule have been thread on.

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 Split/Splitless Inlet –
Installing a GC Column
Wipe the column with lint free tissue soaked with a little methanol
to remove any contamination.

The correct depth of column to be installed into the inlet is

between 4-6mm, from the tip of the ferrule. The septa helps to fix
the insertion depth as the column will not move freely on the septa.

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).

Tip: It is better to slightly under-tighten the nut, apply some inlet

heat and then re-tighten the nut if necessary.

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 Split/Splitless Inlet –
Installing a GC Column

Turn on the carrier gas flow, 1ml/min should be ok for a capillary

column. Ensure flow is coming through the column by placing the
end of the column into a vial of solvent, a fast steady stream of
bubbles should be seen. If no bubbles are seen, check the gas
supply and column insertion into the inlet.

Allow the carrier gas to purge through the column for

approximately 15 mins to expel any oxygen. It is vital this is done
without any heat applied from the oven or the inlet.

Program the inlet temperature to 250°C and allow the inlet to

reach temperature.

Program a slow temperature ramp into the GC, an initial

temperature of 40°C with a 5°C/min ramp and a final temperature
of approx 300°C with a short hold time of 5 mins. Always ensure
you consult the column manufacturers guidelines when
conditioning columns.

This initial column conditioning must NEVER be done with the

column installed into the detector, as this may cause un-necessary
detector fouling.

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 Split/Splitless Inlet –
Installing a GC Column

Once the column has heat cycle, installed the end of the column
to the detector.

It is advisable to leak check all column fitting using a helium

checker, if available.

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 S/SL Inlet - GC Methods for Maintenance

 General GC Maintenance Method

Oven Temperature set to 35°C

Inlet Temperature set to 35°C
Inlet Gas Pressure set to 0.0
Detector Temperature set to 35°C
Detector Flows set to Off

When performing column maintenance, allow time for both the

oven/column to cool before turning off the carrier gas flow. If no
column maintenance is being performed, leave the carrier gas
flowing through the GC column.

If the GC column is removed from the inlet, detector or both

then cap the ends of the column with a clean septa to prevent
oxygen damage.

If FPD maintenance is being performed, power off the GC and

remove the power cable at the rear.

Both FID and NPD detectors use high voltages, therefore be

sure to turn of the electrometer to disable the high voltages.

When the TCD is exposed to air whilst hot, damage will occur to
the filament, therefore turn the filament off.

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 S/SL Inlet - GC Methods for Maintenance

 Inlet Maintenance Method

Oven Temperature set to 35°C

Inlet Temperature set to Off
Inlet Gas Pressure set to 0.0

When performing column maintenance, allow time for both the

oven/column to cool before turning off the carrier gas flow. If
no column maintenance is being performed, leave the carrier
gas flowing through the GC column.

If the GC column is removed from the inlet, detector or both

then cap the ends of the column with a clean septa to prevent
oxygen damage.

Keep the all installed detectors at their temperature set points,

they do not need to be cooled.

When the TCD is exposed to air whilst hot, damage will occur
to the filament, therefore turn the filament off.

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 Split/Splitless Inlet - Maintenance

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.

Load the inlet maintenance method

 Remove the inlet septum nut

Carefully remove the septa by teasing with tweezers, taking care

not to scratch the sealing surface in and around the inlet port.

Inspect and remove any old septa from the inlet by following the
‘cleaning the septum seat’, see further on in the document.

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 Split/Splitless Inlet - Maintenance

Changing a Septum

Place a new septum into the inlet, and press it firmly down to
seat it correctly.

Replace the septum nut, and tightened it so that the ‘c clip’ is

about 1mm above the nut.
(Loose- no gap) (tight- gap)

Restore the GC operating temperatures

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 Split/Splitless Inlet - Maintenance

Changing a Liner and O-ring

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.

Load the inlet maintenance method.

 Undo the flip top cap by rotating the yellow clip anticlockwise to
release the flip top cap.

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.

Check the gold seal for any particulates or septa fragments, by

looking down into the inlet. Use as pocket torch if necessary. If the
gold seal is dirty this will also need replacing at the same time as
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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 Split/Splitless Inlet - Maintenance

Changing a Liner and O-ring

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.

Before installing the new liner ensure there are no o ring

fragments left behind from the previous o ring.

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.

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 Split/Splitless Inlet - Maintenance

Changing a Liner and O-ring

 Purge the inlet and column with carrier gas for 15mins before
heating up the inlet and oven.

Instructions on keypad stokes.

 Its advisable to bake out the inlet after this maintenance – see
bake out procedure.

Reload the analytical method.

If using the inlet counters, reset the liner counter.

At the end of this procedure its advisable to check for leaks –
see leak check method.

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 Split/Splitless Inlet - Maintenance

Changing the Gold Seal

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.

Load the inlet maintenance method

Remove the liner if there is one fitted.

Remove the GC column and plug the end of the column with a
clean septa to prevent oxygen damage.

Remove the insulation cup to exposed the reducing nut.

Remove the reducing nut, take care as this may be screwed

firmly into place, loosen using a spanner.

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 Split/Splitless Inlet - Maintenance

Changing the Gold Seal

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.

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 Split/Splitless Inlet - Maintenance

Changing the Gold Seal

Refit the reducing nut with the gold seal and washer to
the underside of the inlet. Taking care not to let any of the
insulating material enter the reducing the nut. Tighten the
reducing firmly with a spanner.

Refit the liner and the GC column.

Refit the insulation cup.

Its advisable to bake out the inlet after this maintenance

– see about procedure.

Reload the analytical method.

If using the inlet counters, reset the EMF counter.

At the end of this procedure its advisable to check for

leaks – see leak check method.

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 PPI Maintenance

G3451A PP Inlet

 The purged packed inlet (PP), uses packed columns or

0.530mm capillary columns.

 It can do direct injections into packed or wide bore

columns.

 It is used when high efficiency separations that

capillary columns offer is not required.

 If gas flows of >10ml/min are required then wide

bore capillary columns can also be used with the
purged packed inlet.

 The purged packed inlet is flow controlled when the

column is not defined, however if a capillary column
are used, the purged packed inlet will be pressure
controlled.

 Has a maximum operating temperature of 400°C.

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 Inlet Maintenance

 Common Procedures: Customer also

performs often
— Installing column
o Packed column or capillary column
— Change septum
o Must be changed every 100-200 injections
o Septum material makes difference on
longevity
o Sometimes septum nut replaced with Merlin
Microseal- no septum option

— Change inlet liner

o Replacement time varies with samples matrix
and throughput
• Bad matirx- clean more often
• High throughput- clean more often
o Type of liner differs with sample, sample
matrix, and application, so check with
customer before replacing
o Every time the liner is replaced the o-ring
should also be replaced

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Purged Packed Inlet – Tools and
Consumables
Description Part #
Preventative maintenance kit 5188-6498
Purged packed glass liners and column adapters Glass 5080-8732
liner (25/pack)
deactivated (5/pack) 5181-3382
0.53-mm column adapter 19244-
80540
1/8-inch column adapter 19243-
80530
1/4-inch column adapter 19243-
80540
Recommended septa and O-rings for the purged 5181-1263
packed inlet 11-mm solid septum, low-bleed, red
(50/pk)
11-mm septum with partial through-hole, low-bleed, 5181-3383
red (50/pk)
11-mm septum, low-bleed, gray (50/pk) 5080-8896
Merlin Microseal septum (30 psi) 5181-8815
11-mm high-temperature silicone septum (350 °C and 5182-0739
higher) (50/pk)
Viton O-ring (Top insert weldment) (12/pk) 5080-8898
Nuts and Ferrules
1/8-inch id Swagelok stainless steel nut, front ferrule, 5080-8751
back ferrule 1/8-inch column (20 each/pk)
1/8-inch id Swagelok brass nut, front ferrule, back 5080-8750
ferrule 1/8-inch column (20 each/pk)
1/8-inch id Vespel/ graphite ferrule 1/8-inch column 0100-1332
(10/pk)
1/8-inch id brass tubing nut 1/8-inch column(10/pk) 5180-4103
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 Purged Packed Inlet – Tools and
Consumables
Description Part #
1/4-inch id Swagelok stainless steel nut, front ferrule, back 5080-8753
ferrule 1/4-inch column (20 each/pk)

1/4-inch id Swagelok brass nut, front ferrule, back ferrule 5080-8752

1/4-inch column (20 each/pk)

1/4-inch id Vespel/graphite ferrule Inlet/detector liner/adapters 5080-8774

1/4-inch column(10/pk)

1/4-inch id brass tubing nut 1/4-inch column (10/pk) 5180-4105

.530 Ferrule, Vespel/graphite, 0.8-mm id 0.45-mm and 0.53-mm 5062-3512
capillary columns (10/pk)

Ferrule, graphite, 1.0-mm id 0.53-mm capillary columns (10/pk) 5080-8773

Column nut, finger-tight (for 0.53-mm columns) Connect column 5020-8293

to inlet or detector

.320 Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm capillary 5062-3514

columns (10/pk)

Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25-mm, and 5080-8853

0.32-mm capillary columns (10/pk)

Column nut, finger-tight (for .100- to .320-mm columns) 5020-8292

Connect column to inlet or detector

.250 Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2-mm, and 5181-3323

0.25-mm capillary columns (10/pk)

Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25-mm, and 5080-8853

0.32-mm capillary columns (10/pk)

Column nut, finger-tight (for .100- to .320-mm columns)Connect 5020-8292

column to inlet or detector

.100 and .200 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, and 0.25- 5181-3323

mm capillary columns (10/pk)

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 Purged Packed Inlet – Tools and
Consumables
Description Part #
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
All Ferrule, no-hole Testing (10/pk) 5181-3308
Capillary column blanking nut Testing–use with any 5020-8294
ferrule
(2/pk)
Column nut, universal Connect column to inlet or 5181-8830
detector
Column cutter, ceramic wafer Cutting capillary columns 5181-8836

¼ inch spanner

Lint free gloves

Metric ruler

0- or 00- grade steel wool

Tweezers

Septum nut wrench

Compressed dry air or N2

Sonic bath

7-16 inch spanner (quantity 2)

9/16 inch spanner

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 Purged Packed – Tools and Consumables

Description Part #

Methanol

Beaker

Cleaning brushes – FID Cleaning Kit 9301-0985

Column

½ inch spanner

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 Purged Packed - Maintenance

Installing a Column Adapter

Caution: Take care the oven and inlet parts may still be hot enough to
cause burns to the hands.

Load the inlet maintenance method.

Before installing the adapter, wearing lint free gloves,

clean the adapter with some methanol to remove any
contamination.

Put the tubing nut and graphite/vespel ferrule onto the

adapter and inset into the inlet base until it stops.

With the adapter held in this positions finger tighten the

nut, and then tighten the nut with an extra ¼ turn with a
spanner.

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 Purged Packed – Installing Columns

Installing a Packed Metal Column

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.

Load the GC maintenance method.

Both ¼ inch and 1/8 inch metal columns require an inlet
adapter to be fitted.

Attached the column to the adapter by finger tightening

the nut. Then tighten the nut an additional ¼ turn for a
1/8 inch column or an additional ¾ turn for a ¼ inch
column, using spanners.

Using 2 spanners will help keep the adapter nut in situ

and stop it rotating whilst the column nut is tightened.

Push the Config, Column 1 or Column 2 and enter 0.0 in

either Length or Diameter. Identify which inlet or detector
the column is installed into.

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 Purged Packed – Installing Columns

Installing a Packed Metal Column

Caution: Do not use hydrogen carrier gas to condition the column, as
the outlet of the column expels the hydrogen into the oven therefore
causing an explosive risk.

Condition the column are per the column manufacturer’s

guidelines. Typically for a packed column raise the oven
temperature slowly. The conditioning temperature is
never higher than <30°C than the maximum
temperature.
Let the oven, inlet and detector to come to temperature
and stabilize and then retighten the column fittings.

Ideally condition the column overnight at the final

temperature and then cool the oven to room temperature
with carrier gas on.
Column type Typical Flows
(ml/min)
2mm id glass 20-30
1/8 inch od metal 20-30
4mm id glass 50-60
¼ inch od metal 50-60

Let the oven, inlet come to temperature and then

retighten the column fittings.

Once the column has been conditioned install the

column into the detector using a adaptable fitting.
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 Purged Packed – Installing Columns

Installing Ferrules onto a Metal Column

Check the column end is cut square. Check there are no
burrs or irregular shapes to the end of the column.

Place a stainless steel Swagelok male fitting into a

bench vice, and secure it.

Place a brass Swagelok nut and 2 piece ferrule onto the

column and then insert into the s/s male fitting in the
vice.

Push the column until it bottoms out in the s/s fitting

and then withdraw 1-2 mm and then finger tighten the
nut.

Tighten an additional ¾ turn using a spanner for a 1/8

inch column and an additional 1-1/4 turn for a ¼ inch
column.

Unscrew the column from the male fitting and the brass
ferrule should fixed in place on the column end.

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 Purged Packed – Installing Columns

Installing a Capillary Column

Load the general GC maintenance method.

Take the GC column out of the box. Familiarize with the

suggested operating conditions. Store the QC check sheet
safely. The column will come flame sealed at each end, be
sure to remove at least 1-2cms from each end of the
column. Use a ceramic wafer to cut the column.

Install a 0.53mm column adapter onto the inlet.

To facilitate the installation of the column, thread a

clean septa onto the column.

Thread an inlet nut and ferrule onto the column. Always

use the appropriate nut and ferrule according to the id of
the column.

Cut the end of the column using a ceramic wafer to

ensure a clean square cut is achieved. The ceramic wafer
has a serrated and sharp side, use the sharp side to cut
the column. Inspect the quality of the cut using an eye
glass.

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 Purged Packed – Installing Columns

Installing a Capillary Column

The column should always be cut after the nut and ferrule
have been threaded on.

Wipe the column with lint free tissue soaked with a little
methanol to remove any contamination.

The correct depth of column to be installed into the inlet

is between 1-2mm, from the tip of the ferrule. The septa
helps to fix the insertion depth as the column will not
move freely on the septa.

Insert the column into the inlet, holding septa, so that

the depth of the column remains correct. Ensure the
bottom of the septum is flush with the bottom of the nut
then finger tighten the nut.

Tighten the column nut with an additional ¼ - ½ turn

with a spanner.

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 Purged Packed – Installing Columns

Installing a Capillary Column

Configure the column dimensions using the front keypad.

Turn on the carrier gas flow, 1ml/min should be ok for a

capillary column. Ensure flow is coming through the
column by placing the end of the column into a vial of
solvent, a fast steady stream of bubbles should be seen. If
no bubbles are seen, check the gas supply and column
insertion into the inlet.

Allow the carrier gas to purge through the column for

approximately 15 mins to expel any oxygen. It is vital this
is done without any heat applied from the oven or the inlet.

Program the inlet temperature to 250°C and allow the

inlet to reach temperature.

Program a slow temperature ramp into the GC, an initial

temperature of 40°C with a 5°C/min ramp and a final
temperature of approx 300°C with a short hold time of 5
mins. Always ensure you consult the column manufacturers
guidelines when conditioning columns.

This initial column conditioning must NEVER be done with

the column installed into the detector, as this may cause
un-necessary detector fouling.

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 Purged Packed – Installing Columns

Installing a Capillary Column

Once the column has heat cycle, installed the end of the
column to the detector.

It is advisable to leak check all column fitting using a

helium checker, if available.

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 Purged Packed - Maintenance

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.

Load the inlet maintenance method

 Remove the inlet septum nut

Carefully remove the septa by teasing with tweezers,

taking care not to scratch the sealing surface in and
around the inlet port.

Inspect and remove any old septa from the inlet by

following the ‘cleaning the septum seat’, see further on in
the document.

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 Purged Packed - Maintenance

Changing a Septum

Place a new septum into the inlet, and press it firmly

down to seat it correctly (must be wearing gloves).

Replace the septum nut, and tightened it so that the ‘c

clip’ is about 1mm above the nut.

Restore the GC operating temperatures

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 Purged Packed - Maintenance

Cleaning the Septum Seat

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.

Load the inlet maintenance method.

Remove the septum nut and septa to expose the

septum seat.

Remove the insert weldment.

Remove any dirt/contamination or septa stuck to the

septum nut or septum seat. It can be removed with a
small piece of 0-/00- grade steel wool. In hard to reach
places hold the wool with tweezers. Blow the septum nut
and septum seat with some clean compressed air or N2 to
remove any residual particles. DO NOT allow any particles
enter the inlet.
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 Purged Packed - Maintenance

Cleaning the Septum Seat (only if necessary)

Check the o ring for signs of ware, replace if necessary.

Replace the weldment and firmly hand tighten.

Install a new septa and replace the septum nut.

Hand tighten the septum nut so that there is approx

1mm between the nut and the c ring.

Reload the analytical method and reset the septum

counter.

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 Purged Packed - Maintenance

Changing the o-ring

Caution: Take care the oven and inlet parts may still be hot enough to
cause burns to the hands.

Load the inlet maintenance method.

Remove the top weldment from the inlet and remove

the old o-ring use tweezers if required.

Install a new o ring and replace the insert weldment,

and hand tighten firmly/

Reload the analytical method.

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 Purged Packed - Maintenance

Changing the Glass Liner

Caution: Take care the oven and inlet parts may still be hot enough to
cause burns to the hands.

Load the inlet maintenance method.

Remove the top inlet weldment.

Using a pair of fine tip tweezers carefully remove the old

inlet liner. Note the liner has a ‘fluted’ end, this must be
placed at the top of the inlet.

Inspect the liner for septa particles and contamination,

replace if necessary. Hold the new liner with the fluted
end using tweezers and carefully lower into the inlet.

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 Purged Packed - Maintenance

Changing the Glass Liner

Due to the narrow ID of the liner you may experience

problems installing the new liner when a capillary column
is installed. In this case remove the column, install the
new liner and replace the column.

Replace the insert weldment and hand tighten firmly.

Reload the analytical method.

Reset the liner counter.

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 Purged Packed - Maintenance

Installing the Insulation Cup

Caution: Take care the oven and inlet parts may still be hot enough to
cause burns to the hands.

 To install the insulation cup first cap the inlet with a no

hole ferrule and nut or a blanking nut to ensure no
insulation material enters the inlet.

 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

Remove the no hole ferrule and nut or the blanking nut.

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 Purged Packed - Maintenance

Cleaning the PP Inlet (if necessary)

Caution: Take care the oven and inlet parts may still be hot enough to
cause burns to the hands.

Load the inlet maintenance method.

Remove the column, septum nut, and septum.

Remove the insert weldment, o-ring and liner.

If the column adapter is used, remove.

Sonicate the septum nut, top insert weldment and

adapter in methanol or a suitable solvent that will remove
the contamination.

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.

Use compressed air/N2 to dry the inside of the inlet

body.

Re install the column adapter, liner and o- ring.

Re install the insert weldment, septa and septum nut.

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 Purged Packed - Maintenance

Cleaning the PP Inlet

Re install the column and check for leaks.

Reload the analytical method.

Reset the septum and liner counters.

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 Purged Packed - Checks

Bake out Procedure

Program the column flow to the typical operating value
or program the capillary column to a gas velocity of
approximately 30cm/s.

Allow the column to purge with carrier gas for

approximately 10 minutes before any heat is applied.

If the column is not installed into the detector cap the
detector using a no hole ferrule and nut or using a
blanking nut.

Program the inlet temperature to 300°C or

approximately 25°C above the typical operating
temperature of the column if installed.

Program the column temperature approximately 25°C

above the final GC oven temperature ramp of the
analytical method used. However be sure not to exceed
the column manufactures maximum temperature
guidelines.

Bake out the for approximately 30 minutes or until the

detector baseline is free from contamination peaks.

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 Column

 Common Column Procedures

— Install new column
o Length of column inserted into injection port
depends on the injection port and injection
technique.
o Length of column inserted into detector
depends on the detector
o Best practice is to flow carrier gas through the
column for 15-20 minutes before any heat is
applied to the injection port or oven. This gets
rid of any air or oxygen in the column.
o Once purged of gases bake the column out at
300oC for 30 minutes.

— Clip front end of the column

o Front end of column often gets contaminated
and must be trimmed.
o Trim a minimum of 6 inches
o Trimming several feet off the column is
common

— Getting a good cut on the column is very

important to good chromatography so make
sure to get a good cut on the column (see
next slide)

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 Column maintenance

When trimming the column, it is important to trim off

At least 6 inches.

Hold the ceramic wafer perpendicular to the column and

across column with light, but firm pressure.

>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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 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

— Replace Wash Solvent/ Empty Waste

o Wash and Waste vials must be monitored for
solvent levels

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 7683 Autosampler - Overview

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.

Highlighted in blue is the tray.

Highlighted in orange is the injector (or the tower).
Highlighted in green is the turret.
Highlighted in red is the syringe carriage.
Highlighted in yellow is the vial gripper.

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 7683 ALS

 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

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 ALS

See next page

Syringe latch (closed)

Syringe clip

Door

Needle support foot

Vials

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 7683 ALS

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.

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 ALS syringe

Plunger carrier loop

Plunger screw

Plunger

Flange

Flange Guide

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 7683 Autosampler – Checks

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

Pici of the calibration probe

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 7683 Autosampler – Checks

Align Procedure
Usually the align procedure is only necessary when the align
light illuminates orange.

If the GC is a 6890N then on the front panel press Options,

scroll to Diagnostics and then scroll to Front or Back
Injector.

Take out the needle support assy from the ALS and press the
alignment button.

The ALS will then go through a number of steps namely:-

1.The ALS clears the syringe carriage for turret rotation.

2.The turret rotates to confirm the needle support was removed
and determines which turret is fitted.
3.The syringe carriage, moves down, homes, then moves up.
4.The syringe carriage moves down in steps until it hits the turret
in order to set the position of the turret.
5.The plunger moves to calibrate and stops.

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 7683 Autosampler – Checks

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.

Refit the calibration probe into

the syringe carrier exactly as you
would when installing a syringe.

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.

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 7683 Autosampler – Checks

Align Procedure

Once the alignment procedure is finished, the align

mode light will extinguish. Remove the calibration probe
and replace it into its storage position underneath the
ALS.

Refit the needle support assy and syringe.

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.

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 ALS cables

 Ensure the cable is secure on the

instrument’s rear panel.

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SystemsQT

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 SQT

 SQT documentation starts assuming that all

communications are already setup and
working properly
 Make sure you have sufficient gas supplies
— Carrier gas
— Detector gas
— Makeup gas
 Test running a sample before you start the
wizard to double check communications
 System IQ- still in node properties
 Instrument methods may have to be
remade
— If the configuration does not match the
project configuration
— All injectors programmed as front injector-
so you will need to edit for back injectors
— Detectors are programmed as front detector-
need to edit detector section
— Known error for 6850- if method created and
saved without temperature ramp and then
re-edited with ramp, ramp will not function.
Need to completely rewrite method.

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 Agilent GC Qualification

SQT OQ/Manual OQ

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 Manual OQ Tests

Temperature Integrity Tests

GC Oven Temperature Accuracy Test

GC Oven Temperature Stability Test

GC Heated Zones Temperature Accuracy Test (excluding µECD)

Due to the possible risk of radio active contamination, electron
capture detectors are excluded from this service

Headspace Accuracy Tests

Headspace valve operation and heated zones temperature

accuracy Test (Headspace Sampler only)

Pressure Integrity Tests

Inlet Pressure Accuracy Test

Inlet Pressure Decay Test

Flow Accuracy Test

Detector Flow Accuracy Test

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 Objectives of OQ Tests

 Temperature Integrity Tests

— Oven/Inlet/Detector temperature accuracy is
important:
o comparability between systems
o transferring methods
— Oven/Inlet/Detector temperature stability is
critical:
o qualitative
o quantitative analysis
 GC Heated Zones Temperature Accuracy
Test
— The inlet zones are to be hot enough to
vaporize but not so hot as to thermally
decompose sample.
— The detector zones are to be hot enough to
evaporate sample and prevent condensation.
 Pressure Integrity Tests
— Pressure integrity of the inlet is critical for
o repeatable injection
o retention times.
— The pressure decay and pressure accuracy
tests combine to demonstrate pressure
integrity.

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 Objectives of OQ Tests

 Headspace Accuracy Test

— Temperature accuracy of the heated zones is
important for comparability between systems
and transferring methods.
— Oven accuracy is critical to quantitative
headspace methods.
— Correct valve functioning is critical to
operation.

 Detector Flow Rate Accuracy Test

— An unstable carrier gas flow rate may
produce a drifting baseline and false broad
peaks.

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 OQ Test Specifications

Test Name Setpoint and Limits

Parameters

Oven Temperature Temp 1= 230 OC Accuracy = ± 1% from

Accuracy and Temp 2= 100 OC setpoint
Stability (stability measured at Stability <=0.5 OC
Temp 2)

Headspace Vent and N/A Valve functions properly

Pressurization Valve
Integrity

Headspace Heated Inlet: 250 OC Inlet = ± 10 OC of setpoint

Zones Temperature Detector: 300 OC Detector = ± 15 OC of
Accuracy setpoint

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

Inlet Pressure Inlet pressure = 25 psi Accuracy = ± 1.2 psi

Accuracy

Detector Flow Flow rate varies by Accuracy = ± 10% of

Accuracy detector type normal flow rate
(not performed for NPD) (or 0.5 mL/min, which ever
is larger)

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 Tools for Manual OQ

 The Manual OQ tests require specialized

tools.
— Tools must be calibrated

 Calibrated Thermometer
— GC oven/detector probe
— GC inlet probe

 Calibrated Flow meter

— With adapter for FID (19301-60660)
— With Rubber Adapter Tube

 Calibrated Manometer (pressure meter)

— Special probe for inlet

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 Tools for Manual OQ

 Both the GC Oven/Det probe and the Inlet

Probe use the same thermometer
— Equivalent probes and thermometers may be
used if calibrated and meet specifications

Thermometer and Probe

Specifications:

Thermometer:
- display capable of 1.0 OC
- calibrated

Temperature Probe:
- measure at 100 OC and
230 OC ± 2 OC
- calibrated

Also necessary: A device to hold

probe in place, such as
- high temperature tape
- paper clip
- clamp

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 Probes for Thermometer

 Inlet Temperature
Probe
— Special probe
design to measure
inside the inlet.

Inserted into
Injection port

 GC Oven Probe
— Special flexible
stainless steel
probe

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 Tool for Manual OQ

 Digital Manometer (pressure meter)

— Capable of 100 psi
o +/- 0.2 % accuracy FS
— Probe is very fragile!
— Beware of the ferrules- they need to be
replaced periodically

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 Tools Manual OQ

 Digital flow meter

— At least 1.0 – 100 mL/min
o +/- 3% (calibrated)

FID Adapter TCD Rubber

(19301-60660) Adapter Tube

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 Before OQ begins

 Before any Manual OQ procedures may

begin, the GC temperature zones must be
turned down to safe temperatures, and gas
flows turned down or OFF.

— Uninstall the column. Cap both ends with a

piece of septum to keep air out.

— After column and oven have cooled, reduce

all inlet flows to 0.0 ml/min

— Turn inlet temperatures OFF.

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 Manual OQ settings

Parameter Setting Front Panel

Operations
Oven set point 230 oC Oven button
Initial temperature – use number
keys
Hit Enter
Ramp OFF

Oven set point 100 oC Oven button

Initial temperature – use number
keys
Hit Enter
Ramp OFF

Front/Back Inlet set 250 oC Front Inlet button (Back inlet button)
Down arrow

point Temperature – use number keys

Hit enter

Front/Back Inlet 25 psi Front Inlet button (Back inlet button)

Down arrow twice to Pressure

Pressure test Use number keys

Hit enter

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 Manual OQ settings

Front/Back 300 oC Front Detector button (Back detector

button)

Detector set point Temperature- use number keys

Hit enter

Front/Back H2: 30 mL/min Front Detector button (Back detector

Air: 400 mL/min button)

Detector Flow FID Makeup: 25

mL/Min
Down arrow once to H2- use number
keys-hit Enter
Down arrow once to Air- use number
keys-hit Enter
Down arrow once to Makeup-use
number keys-hit Enter

Front/Back Makeup: 5 mL/min Front Detector button (Back detector

Reference: 30 button)

Detector Flow TCD mL/min Down arrow once to reference- use

number keys-hit Enter
Down arrow once to makeup-
constant makeup

Front/Back Makeup: 25 Front Detector button (back detector

mL/min button)

Detector Flow uECD Down arrow to makeup – use number

keys – hit Enter

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GC Oven Temperature Accuracy
and Stability Test

 GC Oven Temperature Accuracy

— Measured at 2 different temperature set
points
— Accuracy is determined as the difference
between the set point and the observed
temperature
— Probe placement important

 GC Oven Temperature Stability Test

— Measured at one set point
— Five readings taken 4 minutes apart
— Stability is determined by temperature being
within 0.5oC of set point at each reading
— Probe stays in same place as the Accuracy
test

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 GC Oven temp tests

 Place Probe in back of GC by fan- next to GC

oven temperature sensor
— Not touching metal
— Door must close for test (feed through corner)

Feed
probe
through
HERE

GC
Probe temp
sensor

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 Oven Temperature

 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

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 Inlet OQ tests

 GC Heated Zone Accuracy Test

— Both Inlet and Detector
— Temperature measured using calibrated
thermometer with special design
— Two measurements are taken
— Accuracy is determined by difference
between setpoint and observed temperature

Inlet

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 GC Heated Zones

 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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 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.

The FID takes the longest to come to temperature. The

TCD is pretty quick.

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 Inlet Pressure Test

 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

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 Inlet Pressure Tests

 Inlet Pressure Accuracy and Decay Tests have

the same setup.
— Probe installed in Inlet like the column

(Probe in column nut)

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 Detector Flow Accuracy Test

 Detector Flow Accuracy Test

— Flows measured with external calibrated
mass flow meter
— Accuracy is determined by the difference
between observed flow rate and flow rate set
point (set on GC front panel)
— Accuracy must be determined for each
detector gas used

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 Detector Flow Accuracy Test

 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

— For FID Detector

o Hydrogen 30 mL/min
o Air 400 mL/min
o Make-up 25 mL/min

— For TCD Detector

o Reference 30 mL/min
o Make-up 5 mL/min

— μECD Detector
o Make-up 25 mL/min

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Headspace OQ Tests

 Headspace Heated Zones Temperature

Accuracy Test
— Temperature is measured with external
calibrated thermometer
— Special probe design for thermometer
— Accuracy is determined as the difference
between found value and set point values.

 Headspace Valve Operational Test

— Valves are physically checked
o Switching
o Leakage

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 Headspace Temperature Accuracy

 Headspace Oven Temperature Accuracy

— Open the headspace oven door
— Position the calibrated thermometer probe in
the slot located under the small metal plate
of the oven’s door

— Carefully close the oven door

— Set the headspace oven temperature to
100OC
— Wait until the headspace oven is ready,
allowing sufficient time for it to reach and
stabilize at set temperature
— Record temperature on Form 6

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 Headspace

G1888 Probe Placement 7694 Probe Placement:

Place probe direct in
sampling opening

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 Test Injections

 Run test injection to confirm that your

system is functioning properly before
beginning the maintenance procedures.

 Open Run Samples with the appropriate

project for your instrument configuration.

 Run Test Injections (not necessary to use

SQT wizard)
— Use Load samples function
— Chose previously made sample set method
— Chose Test injections
— Select/highlight injections line
— Click the green run samples icon
— Select run only selected lines

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Use Only reserved.
 Maintenance Procedures

 Most of the maintenance procedures are

the same as the general GC we discussed
previously

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 Repair: Inlets

 Split Splitless: By far the most common

inlet used. Followed by PTV and MMI. PPIP
is most highly used if packed columns are
required.

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Use Only reserved.
 Split/Splitless

 Split/Splitless

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Use Only reserved.
Split/Splitless Inlet – Tools and
Consumables
Description Part #

Liners

Split Low-pressure drop, glass wool, single taper, 870 5183-4647

µL
Split Glass wool, 990 µL 19251-
60540
Split—Manual only Empty pin and cup, 800 µL 18740-
80190
Splitless Single taper, glass wool, 900 µL 5062-3587

Splitless Single taper, no glass wool, 900 µL 5181-3316

Splitless Dual taper, no glass wool, 800 µL 5181-3315

Splitless—Direct inject 2-mm id, quartz, 250 µL 18740-

80220
Splitless—Direct inject 2-mm id, 250 µL 5181-8818

Direct inject —Headspace or purge and trap 1.5-mm 18740-

id, 140 µL 80200
Direct column connect Single taper, splitless 4-mm id G1544-
80730
Direct column connect Dual taper, splitless 4-mm id G1544-
80700
Nuts and Ferrules

.530 Ferrule, Vespel/graphite, 0.8-mm id 0.45-mm 5062-3512

and 0.53-mm capillary columns (10/pk)
Ferrule, graphite, 1.0-mm id 0.53-mm capillary 5080-8773
columns 5080-8773 (10/pk)
Column nut, finger-tight (for 0.53-mm columns) 5020-8293
Connect column to inlet or detector
COMPANY CONFIENTIAL – For Internal © 2010 Waters Corporation. All rights
.320
Use Only Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm 5062-3514 reserved.
 Split/Splitless Inlet – Tools and
Consumables
Description Part #

Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25- 5080-

mm, and 0.32-mm capillary columns (10/pk) 8853
Column nut, finger-tight (for 0.53-mm columns) 5020-
Connect column to inlet or detector 8293
.320 Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm 5062-
capillary columns 3514
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25- 5080-
mm, and 0.32-mm capillary columns (10/pk) 8853
Column nut, finger-tight (for .100- to .320-mm 5020-
columns) Connect column to inlet or detector 8292
.250 Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2- 5181-
mm, and 0.25-mm capillary columns (10/pk) 3323
.100 and .200 Ferrule, Vespel/graphite, 0.37-mm id 0.1- 5062-
mm and 0.2-mm capillary columns 3516
Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2-mm, 5181-
and 0.25-mm capillary columns (10/pk) 3323
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25- 5080-
mm, and 0.32-mm capillary columns (10/pk) 8853
Column nut, finger-tight (for .100- to .320-mm 5020-
columns) Connect column to inlet or detector 8292
All Ferrule, no-hole Testing (10/pk) 5181-
3308
Capillary column blanking nut Testing–use with any 5020-
ferrule 8294
Column nut, universal Connect column to inlet or 5181-
detector (2/pk) 8830
Column cutter, ceramic wafer Cutting capillary columns 5181-
(4/pk) 8836
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 0.25- 5080-
mm, and 0.32-mm capillary columns (10/pk)
COMPANY CONFIENTIAL – For Internal
8853
© 2010 Waters Corporation. All rights
Use Only reserved.
 Split/Splitless Inlet – Tools and
Consumables
Description Part #
General

Septum retainer nut for headspace 18740-

60830
Septum retainer nut 18740-
60835
11-mm septum, high-temperature, low-bleed, 50/pk 5183-
4757
11-mm septum, prepierced, long life, 50/pk 5183-
4761
Merlin Microseal septum (high-pressure) 5182-
3444
Merlin Microseal septum (30 psi) 5181-
8815
Nonstick fluorocarbon liner O-ring (for temperatures up 5188-
to 350 °C), 10/pk 5365
Graphite O-ring for split liner (for temperatures above 5180-
350 °C), 10/pk 4168
Graphite O-ring for splitless liner (for temperatures 5180-
above 350 °C), 10/pk 4173
Split vent trap PM kit, single cartridge 5188-
6495
Retaining nut G1544-
20590
Gold-plated seal (standard application) 5188-
5367
Gold-plated seal with cross (high split flows) (includes SS 5182-
washer) 9652
Stainless steel washer (0.375-inch od), 12/pk 5061-
5869
Reducing
COMPANY nut – For Internal
CONFIENTIAL 18740-All rights
© 2010 Waters Corporation.
Use Only reserved.
 Split/Splitless Inlet – Tools and
Consumables
Description Part #

Capillary Inlet PM Kit, split 5188-

6496
Capillary Inlet PM Kit, splitless 5188-
6497
¼ inch open end spanner

Lint free gloves

Column

Isopropanol

Lab Tissue

Metric Ruler

Tweezers

0- or 00- grade steel wool

Compressed (dry and filtered) air or N2

½ inch spanner

T20 torx driver

Cleaning brushes (from the FID kit) 9301-

0985

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Use Only reserved.
 Split/Splitless Inlet – Installation

 Power off the GC using the front on/off button.

 Unplug the rear power cable.

 Remove the inlet panel by removing the 4 screws.

Lift off the inlet panel to expose the inlet

components.

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 Split/Splitless Inlet - Installation

 Remove the headspace transfer line support (if there is

one installed).

 Open the GC oven door, by pushing the opener firmly.

Swing the door wide open to allow for easy access to
oven/column/detector components.

Detach the GC column that is installed in the inlet using a

1/4inch spanner.

Plug the end of the GC column to prevent oxygen

damage using a clean inlet septum.

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 Split/Splitless Inlet - Installation

 With the oven door open, loosen the 2 screws so that

the insulating cup can be removed.

The insulating material inside the insulating cup is in 3

pieces, each has a different size hole. This is because the
diameter of the reducing nut, and inlet nut is different. Be
sure to fit these correctly to ensure the insulating material
fits snugly against the metal parts. The piece of insulating
material with the smallest hole goes into the cup first
followed by the next size and so on.

Close the oven door.

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 Split/Splitless Inlet - Installation

 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.

Remove the 3 screws holding the inlet in place.

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 Split/Splitless Inlet - Installation

 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.

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 Split/Splitless Inlet - Installation

 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.

Refit the septum nut using the flip top mechanism.

Refit the insulating cup and column.

Refit the transfer line support.

Refit the inlet panel and restore power to the GC.

At the end of this procedure its advisable to check for

leaks – see leak check method.

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Use Only reserved.
 Purged Packed Inlet

 Purged Packed Inlet

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Use Only reserved.
 Purged Packed Inlet – Tools and
Consumables
Description Part #
Preventative maintenance kit 5188-6498
Purged packed glass liners and column adapters Glass 5080-8732
liner (25/pack)
deactivated (5/pack) 5181-3382
0.53-mm column adapter 19244-
80540
1/8-inch column adapter 19243-
80530
1/4-inch column adapter 19243-
80540
Recommended septa and O-rings for the purged packed 5181-1263
inlet 11-mm solid septum, low-bleed, red (50/pk)
11-mm septum with partial through-hole, low-bleed, red 5181-3383
(50/pk)
11-mm septum, low-bleed, gray (50/pk) 5080-8896
Merlin Microseal septum (30 psi) 5181-8815
11-mm high-temperature silicone septum (350 °C and 5182-0739
higher) (50/pk)
Viton O-ring (Top insert weldment) (12/pk) 5080-8898
Nuts and Ferrules
1/8-inch id Swagelok stainless steel nut, front ferrule, 5080-8751
back ferrule 1/8-inch column (20 each/pk)
1/8-inch id Swagelok brass nut, front ferrule, back ferrule 5080-8750
1/8-inch column (20 each/pk)
1/8-inch id Vespel/ graphite ferrule 1/8-inch column 0100-1332
(10/pk)
1/8-inch id brass tubing nut 1/8-inch column(10/pk) 5180-4103
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Use Only reserved.
 Purged Packed Inlet – Tools and
Consumables
Description Part #

1/4-inch id Swagelok stainless steel nut, front ferrule, 5080-8753

back ferrule 1/4-inch column (20 each/pk)
1/4-inch id Swagelok brass nut, front ferrule, back 5080-8752
ferrule
1/4-inch column (20 each/pk)
1/4-inch id Vespel/graphite ferrule Inlet/detector 5080-8774
liner/adapters
1/4-inch column(10/pk)
1/4-inch id brass tubing nut 1/4-inch column (10/pk) 5180-4105

.530 Ferrule, Vespel/graphite, 0.8-mm id 0.45-mm and 5062-3512

0.53-mm capillary columns (10/pk)
Ferrule, graphite, 1.0-mm id 0.53-mm capillary 5080-8773
columns (10/pk)
Column nut, finger-tight (for 0.53-mm columns) 5020-8293
Connect column to inlet or detector
.320 Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm 5062-3514
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
.250 Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2- 5181-3323
mm, 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
.100 and .200 Ferrule, Vespel/graphite, 0.37-mm id 5062-3516
0.1-mm and 0.2-mm capillary columns (10/pk)
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Use Only reserved.
 Purged Packed Inlet – Tools and
Consumables
Description Part #

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
All Ferrule, no-hole Testing (10/pk) 5181-3308

Capillary column blanking nut Testing–use with any 5020-8294

ferrule
(2/pk)
Column nut, universal Connect column to inlet or 5181-8830
detector
Column cutter, ceramic wafer Cutting capillary columns 5181-8836

¼ inch spanner

Lint free gloves

Metric ruler

0- or 00- grade steel wool

Tweezers

Septum nut wrench

Compressed dry air or N2

Sonic bath

7-16 inch spanner (quantity 2)

9/16 inch spanner

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Use Only reserved.
 Purged Packed – Tools and Consumables

Description Part #

Methanol

Beaker

Cleaning brushes – FID Cleaning Kit 9301-0985

Column

½ inch spanner

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Use Only reserved.
 Purged Packed – Installation

Agilent G3451A 0-100psi Packed Purged EPC Inlet

(PP)

Parts required

Purged packed inlet (pici shows it installed)

EPC module

Pici needed

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 Purged Packed – Installation

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.

Remove the detector, pneumatics and ALS tray if one is

installed.

Remove the inlet cover and the EPC module bracket

next to the inlet EPC.

 If no inlet has been installed in this position before, the

round metal cutout will need to be removed using
diagonal cutters, ensuring the metal nibs are retained on
the cutout and not left behind on the GC chassis.

The insulation material (plug) underneath the metal

cutout also needs removing.

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 Purged Packed – Installation

The make an opening in the inner oven insulation use a

razor/knife to cut a circle or use a screwdriver to carefully
punch a hole and gradually remove the excess insulation.
Wipe away any insulation from the inside of the oven.

With the oven door open, install the bottom cover plate
using heat resistant screws.

Fit the bottom inlet insulation into the inlet cavity.

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.

Secure the inlet in place by tightening the 3 screws

taking care to ensure the screws are threaded correctly.
The screws should then be tightened firmly in turn until
the inlet is securely fixed in place.

Looking on the left of the inlet on the GC chassis there is

heater cable connector, plug in the heater cable and then
use the tab on the GC chassis to tuck away the cable so
that it will not pinch when the inlet cover is replaced.

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 Purged Packed – Installation

heater cable

heater connection

inlet screws

Heater cable tucked away so

that it will not be pinched

For the EPC module, plug in the communications cable

(can be found in the inlet module EPC slot area on the
GC) into the inlet module PCB.

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.

EPC tubing tidied into the

pneumatics area

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 Purged Packed – Installation

Secure the EPC using the module bracket.

Install the insulation cup to the underside of the inlet as

detailed on page xxx

Replace the GC covers/panels, taking care to ensure no

cable/tubing are pinched.

Plug in the power cable at the rear of the GC and power

on .

Using the GC front keypad, press the Configure, Front

Inlet or Back Inlet, then press Mode/Type and
Enter.

Reboot the GC by pressing Options, then scroll to

Reboot the GC? and press On/Yes twice to reboot the GC
and have the changes take affect.

The EPC installed needs to be calibrated see page xxx.

When both pressure and gas type has been configured,

connect the gas supplies to the rear of the GC, and leak
check all the new fitting/connections.

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 Repairs: Detectors

 FID: The most common detector. ECD and

TCD are close behind. NPD and FPD are not
overly common due to their very specific
selectiveness.

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Use Only reserved.
 FID

G3462A Flame Ionization Detector

 Can purchase 2 versions of the FID, the capillary

column optimized or the adaptable for either packed
or capillary columns.

 Able to detect a wide range of organic compounds

with a minimum detectable level of (for tridecane
<1.8pg C/s.

 The FID has linear dynamic range >107 (+/- 10%).

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Use Only reserved.
 FID Detector – Overview

G3462A Flame Ionisation Detector

Gas Flows
Air 0 - 800 ml/min
H2 0 - 100ml/min
Makeup gas N2 or 0 - 100ml/min
He

Maximum operating temperature of 450°C.

The FID signal is displayed in picoamperes, (pA).

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Use Only reserved.
 FID Detector – Tools and Consumables

Description Part #

.530 Ferrule, Vespel/graphite, 0.8-mm id 0.45-mm 5062-3512

and 0.53-mm capillary columns 5062-3512 (10/pk)
Ferrule, graphite, 1.0-mm id 0.53-mm capillary 5080-8773
columns (10/pk)
Column nut, finger-tight (for 0.53-mm columns) 5020-8293
Connect column to inlet or detector
Column nut, finger-tight (for .100- to .320-mm 5020-8292
columns) Connect column to inlet or detector
.250 Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 5181-3323
0.2-mm, and 0.25-mm capillary columns (10/pk)
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 5080-8853
0.25-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
.100 and .200 Ferrule, Vespel/graphite, 0.37-mm id 5062-3516
0.1-mm and 0.2-mm capillary columns (10/pk)
Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2- 5181-3323
mm, and 0.25-mm capillary columns (10/pk)
Ferrule, graphite, 0.5-mm id 0.1-mm, 0.2-mm, 5080-8853
0.25-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
All Ferrule, no-hole Testing (10/pk) 5181-3308

Capillary column blanking nut Testing–use with any 5020-8294

ferrule
Column nut, universal Connect column to inlet or 5181-8830
detector, (2/pk)
Column cutter, ceramic wafer Cutting capillary 5181-8836
columns, (4/pk)
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Use Only reserved.
 FID Detector – Tools and Consumables

Description Part #

Screw, M4 × 25 mm, Torx, T20 0515-2712

PTFE chimney (optional) 19231-21050

Collector assembly G1531-60690

FID/NPD capillary column adapter 19244-80610

FID/NPD 1/8-inch packed column adapter 19231-80520

FID/NPD 1/4-inch packed column adapter 19231-80530

Insulation (3/pk) 19234-60715

Insulation cup assembly 19234-60700

Nut, 1/4-inch, brass, for packed column adapters 5180-4105

(10/pk)
Ferrule, Vespel, 1/4-inch, for packed column 5080-8774
adapters (10/pk)
Capillary 0.29 mm (0.011 inch) 61.5 mm 19244-80560

Capillary, high-temperature (use with simulated 19244-80620

distillation) 0.47 mm (0.018 inch) 61.5 mm
Packed 0.46 mm (0.018 inch) 63.6 mm 18710-20119

Packed, wide-bore (use with high-bleed applications) 18789-80070

0.76 mm (0.030 inch) 63.6 mm
Capillary 0.29 mm (0.011 inch) 48 mm G1531-80560

High-temperature (use with simulated distillation) G1531-80620

0.47 mm (0.018 inch) 48-mm
Column

Collector nut 19231-20940

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Use Only reserved.
 FID Detector – Tools and Consumables

Description Part #

Spring washer 3050-1246

Ignitor castle 19231-20910

Ignitor castle, Hastelloy 19231-21060

Upper/lower collector insulator G1531-20700

Collector body G1531-20690

Collector body, Hastelloy G1531-21090

Spanner nut (collector) 19231-20980

Collector mount G1531-20550

Collector housing G1531-20740

Gasket 5180-4165

Ignitor 19231-60680

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 FID Detector – Installation

Parts required

FID assy
Pici needed

EPC assy
Pici needed

Insulation and Insulation cup

Note : Do not detach the tubing between the EPC module

and the inlet assy, as this prevent leaks.

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Use Only reserved.
 FID Detector – Installation

Power off the GC and unplug the power cable from the
rear of the GC.

Remove the pneumatics, top detector and RHS panel

With an ESD wrist strap on, and attached to gnd,

remove the EPC modules brackets by loosening the
captive screws.

EPC
mounting
brackets

Remove the round metal cutout for the detector using

diagonal cutters. Ensure the nibs are on the cutout to be
thrown away.

Remove the circular insulation plug and discard.

With a flat screwdriver, make a hole in the oven

insulation approximately ¼ inch ID.

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 FID Detector – Installation

Open the oven door and clean away any insulation

material that has fallen through, then fit the FID bottom
insulation into the cavity.

With the detector assy rested on the top of the GC close

to the detector cavity, take the EPC and locate the correct
mounting position for the EPC.

Detector EPC Slot

Position
Front Detector Front
Back Detector Back
Connect the communication cable to the EPC module

Slide the EPC module in to the vertical slot tracks and

ensure the cables are not being pinched.

Position the tubing into the channel between the EPC

slots to reach the detector, ensure the tubing is free form
the EPC module brackets.

Refit the EPC module brackets by tightening the captive

screws, ensure no cables/tubing are pinched.

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 FID Detector – Installation

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.

Secure the detector into place by tightening the 4

screws.

If there is excess tubing, bend it carefully so that it is

neatly stored on top of the oven, ensure none of the
tubing will be pinched by the cover/panels.

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.

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 FID Detector – Installation

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

Connect the front detector cable and the ignition cable.

ignition cable

communication cable (this cable

will be either F-DET or B-DET
depending on where the detector
assy is physically fitted)

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 FID Detector – Installation

Connect the electrometer signal ribbon cable.

electrometer signal ribbon cable

 Refit the covers/panels in reverse order, plug the rear power

cable and switch the on the GC.

Using the front GC keypad, press the Configure, Front Det or

Back Det (depending on where the hardware has been installed),
then press Mode/Type and Enter.

On pressing enter a caution message will appear asking for a

reboot of the GC. To reboot the GC press Options,
Communications, Enter, and scroll down the Reboot the GC?.
Press On/Yes twice to reboot the GC and ensure the changes take
effect.

Once the detector has been configured it will be recognised as

the FID on the GC display, and all the parameters related to the
FID will appear in the scroll down menus for control of the FID.

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.

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 FID Detector – Installation

When the EPC had been calibrated, configure both

pressure and gas type, then connect up the gas lines, and
leak check.

Fit the insulation cup

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 FID Detector – Installation

Installing the Insulation Cup

 The insulation cup is only required for the adaptable FID.

Adaptable FID

Spring lever from

insulator cup fits in grove

Take the metal cup body and place 3 pieces of insulating

material, be sure to match up the slots in the insulating
material with the slot in the metal cup.

 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

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 FID Detector – Installation

Installing an Adaptable Fitting

Caution: Take care the oven and detector parts may still
be hot enough to cause burns to the hands.

adaptable fitting

 Load the general GC maintenance method.

Place a ¼ inch ferrule and nut onto the adapter nut and
then insert into the detector until it bottoms out.

Whilst holding the adapter in place finger tighten the

nut, then tighten an extra ¼ turn using a spanner to
secure the adapter in place.

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 FID Detector – Installing a GC column

Installing a Capillary Column

Caution: Take care the oven and detector parts may still be hot enough to
cause burns to the hands. The column will have been conditioned when
installed into the inlet, therefore it can installed into the detector.

Load the general GC maintenance method.

To facilitate the installation of the column, thread a clean septa

onto the column.

Thread an inlet nut and ferrule onto the column. Always use the
appropriate nut and ferrule according to the id of the column.

Cut the end of the column using a ceramic wafer to ensure a

clean square cut is achieved. The ceramic wafer has a serrated
and sharp side, use the sharp side to cut the column. Inspect the
quality of the cut using an eye glass.

The column should always be cut after the nut and ferrule have
been threaded on.

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 FID Detector – Installing a GC column

Installing a Capillary Column

Wipe the column with lint free tissue soaked with a little methanol
to remove any contamination.

Install the column into the detector, if the column ID is >0.1mm

push the column into the detector gently until it bottoms out, then
finger tighten the nut and then withdraw the nut approximately
1mm. The tighten the nut an extra ¼ turn with a spanner. If the
column is 0.1mm or less install the column into the detector 68mm
from the tip of the ferrule for an adaptable fitting FID or 48mm for a
capillary optimised fitting FID. Use the septum to fixed the
length/depth of the column into the detector and then holding the
septum under the nut finger tighten the nut and then tighten the nut
an extra ¼ turn with a spanner.

Fit the insulation cup.

 After heating up the detector leak check the fitting using a leak
checker.

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 FID Detector – Installing a GC column

Installing a Capillary Column

 Reload the analytical method.

After heating up the detector leak check the fitting using

a leak checker.

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 FID Detector - Maintenance

Replacing the FID collector assy

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

Unplug the Ignitor cable

Unscrew the 3 T10 screws

Carefully remove the assy, be sure not to damage the

interconnect spring which is exposed once the collector assy
is removed.

Caution: Do not touch or bend the interconnect spring as

this can adversely effect the sensitivity of the FID

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 FID Detector – Maintenance

Replacing the FID collector assy

 Install the new collector assy. If the new collector assy
has an Ignitor cable or protective packaging, remove
these before fitting.

 Insert the 3 T10 screws and tighten to 18inch-pounds,

and reconnect the Ignitor cable.

To complete the replacement of the collector assy,

perform the FID leakage current and FID baseline checks.

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 FID Detector – Maintenance

Maintenance on the FID collector assy

 First cool down the heated zones of the oven and the
FID and turn off the gas supplies. Also wear lint free
gloves to prevent contamination of any internal detector
parts

1. Disconnect the Ignitor plug

2. Remove the Ignitor assy from the collector assy

3. Remove the 3 T10 screw from the top of the collector
assy

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 FID Detector – Maintenance

Maintenance on the FID collector assy

4. Carefully remove the collector assy tasking care not

to damage the interconnect spring

5. Place the collector assy onto a clean piece surface

6. Loosen and remove the collector nut

7. Remove the collector nut washer

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 FID Detector – Maintenance

Maintenance on the FID collector assy

 8. Remove the castle (note the upper insulator has stuck
on the bottom of the castle this may be removed and may
need to be replaced for reassembly)

9. Remove the collector

10. Remove the lower insulator (note the lower insulator

may need to be replaced for reassembly)

11. The collector assy is now dismantled

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 FID Detector – Maintenance

Maintenance on the FID collector assy

 12. To reassemble the collector assy, take a the lower
insulator and place it with the lip facing downwards

13. Replace the collector

14. Take the upper insulator and place it with the lip
facing upwards

15. Replace the castle making sure the orientation of

the threaded hole for the Ignitor is correct

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 FID Detector – Maintenance

Maintenance on the FID collector assy

 16. Replace the collector washer

17. Replace the collector nut, ensure when tightening

the collector nut that the orientation of the castle remains
correct

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.

19. Reconnect the ignitor assy, ensure the threads are

free from dirt, tighten the ignitor with a spanner to ensure
good electrical contact

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 FID Detector – Maintenance

Maintenance on the FID collector assy

19. Insert the 3 T10 screws and tighten then to 18inch-

pounds, and reconnect the ignitor cable.

To complete the maintenance on the collector assy,

perform the FID leakage current and FID baseline checks.

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 FID Detector – Maintenance

Replacing or Cleaning the Jet

Caution: Take care the oven and detector parts may still be hot enough to
cause burns to the hands.

Load the general GC maintenance method.

If a column is installed, remove it from the detector.

Remove the FID collector assy

exposed jet

interconnect spring

Taking care not to damage the interconnect spring,

loosen the jet using a custom torx driver. Then carefully
remove the jet using a pair of tweezers.

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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 FID Detector – Maintenance

Replacing or Cleaning the Jet

Using a lint free q tip soaked in some methanol clean

the inside of the jet cavity, blow dry with some clean
compressed air or N2.

clean this area

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

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 FID Detector – Maintenance

Replacing or Cleaning the Jet

Refit the collector assy, and column. It is available to

check there is carrier gas flow through the column.

 If using the GC counters reset the jet count.

Check the FID leakage current

Bake out the detector.

Reload the analytical method and allow the heated

zones to stabilise before performing analyses.

If needed check the FID baseline

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 FID Detector - Checks

Leakage Current Check

Load an analytical method

Ensure gas flows are suitable for ignition

Ensure the FID is heated to operating temperature,
(300°C)

 Turn off the FID flame and verify the FID electrometer
is on

 Using the front keypad, press Front Detector or Back

Detector, depending on the position of the FID hardware,
and then scroll to Output.

Check the output is stable and <1.0pA

Note : If the output is unstable or >1.0pA, power off the

GC and inspect the serviced parts for correct assembly.
Pay particular attention to the upper parts of the FID.
Check for contamination, and if is the problem follow the
bake out procedure

 If the leakage current passes turn the flame back on.

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 FID Detector - Checks

Baseline Check

To perform the baseline check the GC column needs to

be installed, load a typical checkout method.

 Program the GC oven temperature to 35°C.

 Using the front keypad, press Front Detector or Back

Detector, depending on the position of the FID hardware,
and then scroll to Output.

 With GC showing ready and the flame lit, check the

output is stable and is <20pA.

Note : If the output is unstable or is >20pA, it could

indicate that either the FID or the gas supply is
contaminated. Investigate further to isolate where the
contamination is coming from, if it is confirmed as the
FID, perform the bake out procedure.

Ensure the detector temperature is 350 - 375°C.

Ensure typical operating flows are used.

Light the FID flame.

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 FID Detector - Checks

Bake out Procedure

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.

Caution : The detector and components can be hot. Wear heat

resistant gloves to prevent burns to your hands.

 Bake out of the FID can be performed with or without

the column installed.

 Load a typical maintenance method, wait until the GC is

showing ready.

 If no column is installed into the FID, use a capillary

adapter, column nut with blanking ferrule to plug the
detector.

If a column in installed ensure the carrier gas is flowing

through the column. If there is no flow, remove the
column and plug the inlet/outlet ends of the column with
a clean septa.

Program the GC oven temperature to 250°C or approx.

25°C above the operating temperature of the GC column.
Take care not to exceed the column manufacturers
temperature operating guidelines, otherwise the column
phase may be damage

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 FID Detector – Checks

Bake out continued…..

Keep the temperature of the oven at nominal value for

30 mines or when the baseline begins to stabilise at the
lower value. Typically the baseline will rise and then fall
giving a lower value than before.

Diagram needed here

 Reload the analytical method to allow the FID to

equilibrate.

 Note the FID output value, typically is should be lower

than the initial reading – contact Agilent

Ideally with a GC column installed the FID, a system

baseline should be <20pA.

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 TCD

 TCD

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 TCD Detector – Overview

G3432A Thermal Conductive Detector

The TCD is a universal detector

and can be used to analyse all
compounds.
(left side of GC)

The TCD has minimum detectable

Level of 400pg tridecane/ml when using helium as a
carrier gas.

The TCD has a linear dynamic range of >105 (+/- 5%).

The TCD has a maximum temperature of 400°C

The TCD pictures here is installed on the 7890 as a third

detector so it fits on the left side of the GC.

The TCD does not destroy the sample therefore this

detector can be used in series to another detector for
example a FID.

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 TCD Detector – Tools and Consumables

Description Part #

Capillary columns

Capillary Nut, 1/8-inch id, brass Swagelok 10/pk 5180-4103

Back ferrule, for 0.1-mm to 0.53-mm capillary 5182-3477

columns 10/pk
Front ferrule, 0.53-mm capillary columns 10/pk 5182-9673

Front ferrule, 0.32-mm capillary columns 10/pk 5182-9676

Front ferrule, 0.1-mm, 0.2-mm, and 0.25-mm 5182-9677

capillary columns 10/pk
1/8-inch Swagelok plug 5180-4124

¼ inch packed columns

1/4-inch packed column adapter G1532-

20710
1/8-inch id Vespel/graphite ferrule 10/pk 0100-1332

Nut, 1/8-inch id, brass 10/pk 5180-4103

Ferrule, Vespel, 1/4-inch 10/pk 5080-8774

1/4-inch id tubing nut, brass 10/pk 5180-4105

1/8-inch Swagelok plug 5180-4124

1/8 inch packed columns

Ferrule, 1/8-inch Vespel/graphite 10/pk 0100-1332

Nut, 1/8-inch id, brass 10/pk 5180-4103

1/8-inch Swagelok plug 5180-4124

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 TCD Detector – Tools and Consumables

Description Part #

Optional TCD capillary hardware

Capillary adapter G1532-

80540
Ferrule, Vespel, 1/8-inch 10/pk 0100-1332

Nut, brass, 1/8-inch 10/pk 5180-4103

.530 column id

Vespel/graphite, 0.8-mm id 0.45-mm and 0.53-mm 5062-3512

capillary columns (10/pk)
Ferrule, graphite, 1.0-mm id 0.53-mm capillary 5080-8773
columns (10/pk)
Column nut, finger-tight (for 0.53-mm columns) 5020-8293
Connect column to inlet or detector
.320 column id

Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm capillary 5062-3514

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
.250 column id
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
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 TCD Detector – Tools and Consumables

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

Ferrule, no-hole Testing (10/pk) 5181-3308

Capillary column blanking nut Testing–use with any 5020-8294

ferrule
Column nut, universal Connect column to inlet or 5181-8830
detector (2/pk)
Column cutter, ceramic wafer Cutting capillary 5181-8836
columns (4/pk)
Other supplies

7/16 inch spanner

Lab tissue

Lint free gloves

¼ inch spanner

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 TCD Detector – Installation

Parts required

TCD frame

TCD detector and EPC module

TCD pcb assy

Solenoid valve bracket

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 TCD Detector – Installation

Power off the GC and unplug the power cable from the
rear of the GC.

Remove the pneumatics, detector, LHS and back (top)

panels

With an ESD wrist strap on, and attached to gnd.

Install the solenoid valve bracket by fitting the 4 small

valve plugs and 2 large aux heater plugs into the bracket.
Pici needed

Plug in the aux zone/valve box cable connector to the

A&P PCB (A&P PCB is the analog and power board).

Position the bracket so that the screws on the top over

the screw holes in the chassis and ensure the cables are
routed from the bottom of the bracket. Tighten the screws
to fasten the bracket to the chassis.

Plug in the MSD heated zone cable into position A1 or

A2 on the bracket, ensure you note the position as it will
be needed once the installation is complete for the
configuration of the hardware using the GC front keypad.

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 TCD Detector – Installation

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.

Next attach the frame support using the screws

provided and then attach the corner bracket, again using
the bolts and screws provided.

Cover the holes on the frame using the 2 labels provided

Pici
Route the third detector heated zone cable through the
sheet metal notch and grommet.

Fit the bulkhead fitting retainer to the rear side of the

TCD frame by securing the screw. The bulkhead fitting is
then placed so that the fixed nut is inside the retainer and
tighten the backing nut to secure the fitting in place.

Remove the metal cutout on the LHS of the GC where

the detector will be installed using diagonal cutters.

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 TCD Detector – Installation

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

Plug in the third detector heated zone cable from the

back of the third detector flow frame to the MSD heated
zone cable.

Position the TCD frame to align with the round cutouts,

then tighten the two 4mm captive screws located at the
top of the frame.

Tighten the other four screws which are positioned

through the round cutouts at the bottom of the frame.
Pici needed

Prepare the EPC, remove the 2 torx screws on the top of

the module and then attach the bracket using the screws
provided and ensure the switching valve wire is routed
thought the bracket cutouts.

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 TCD Detector – Installation

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.

Secure the EPC module to the frame using the screws

provided.

Position the detector over the cutout made in the side of

the GC and secure into place using the 3 screws provided.

detector heater cable

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 TCD Detector – Installation

Plug in the TCD heater cable to the third detector heated

zone cable plug. Ensure the cable is neatly stored between the
GC and the bezel.
Pici needed

Bend the pneumatics cabling between the detector and the

EPC so that there is room for the TCD PCB installation.

Install the T manifold assy, attach one short piece of tubing

using a 1/8 inch nut and ferrule to the reference gas fitting on
the epc module.

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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 TCD Detector – Installation

Attach the long piece of tubing using a 1/8 inch nut and
ferrule to the bulkhead fitting.

Install the TCD pcb frame using the 2 captive screws.

captive screws (one of which is shown the

other is to the RHS just clipped off the
picture).

 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

notches in the board

 thumbscrew

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 TCD Detector – Installation

Fit the TCD pcb cover and secure in place using the torx
screw.

 Plug in the filaments cables, (thick black wire sheath)

and the ΔPRT cables, (thin white sheath) coming from the
TCD into the TCD board. With a small flat blade
screwdriver push on the orange connector tabs and insert
the cable then release the connector tab to lock the cables
into position.

thin white wires ΔPRT

orange connector

thick black wires filament

Around the EPC module area at the rear of the GC,

connect the comm cable Aux Det2 to plug Aux Det2.
pici

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 TCD Detector – Installation

Around the EPC module area at the rear of the GC,

connect the comm cable EPC5 to plug EPC5.

Route these cables from the EPC area in between the

pneumatics area through to the TCD detector frame.

 route cables in this space

 Connect the TCD switching valve cable to the switching

valve lead on the EPC, and then plug the other end into
the TCD board.

TCD switching valve cable

TCD switching valve connections

TCD detector connection

 Plug in the TCD detector cable to the TCD board.

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 TCD Detector – Installation

 If there is a red TCD cap installed on the TCD exhaust

remove it.

Fit the TCD detector frame cover on right side of GC

using the 2 torx screws.
GC Back GC front

Replace the remaining GC panels/covers, and plug the

rear power cable in and turn on the GC.

Using the GC front keypad, press Configure, Aux Det#

and Enter.

Press Mode/Type and scroll to choose the Aux Heater and

press Enter. On the GC screen a prompt will appear asking
to select a heater to install. Press Aux 1 or Aux 2
depending on where the MSD heated zone cable was
plugged, (either A1 or A2). A message will appear on
screen requesting a reboot.

To reboot the GC, press Options, scroll to

Communications and press Enter.

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 TCD Detector – Installation

Scroll to Reboot the GC? And press On/Yes twice for

the GC to reboot and accept the changes made to
configuration.

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 TCD Detector – Installing a Column

Installing a Capillary Column

Caution: Take care the oven and detector
parts may still be hot enough to cause burns
to the hands.
The column will have been conditioned when installed into the inlet,
therefore it can installed into the detector.

Load the general GC maintenance method.

Fit a front ferrule, back ferrule and 1/8 brass swagelock

nut onto the column.

Cut the end of the column using a ceramic wafer to

ensure a clean square cut is achieved. The ceramic wafer
has a serrated and sharp side, use the sharp side to cut
the column. Inspect the quality of the cut using an eye
glass.

Wipe the column with lint free tissue soaked with a little
methanol to remove any contamination.

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 TCD Detector – Installing a Column

Installing a Capillary Column

Gently push the column into the detector until it

bottoms out and then finger tighten the nut.

Retract the column by 1mm and then tighten the nut by

an extra ¼ turn with a spanner.

Reload the analytical method.

 After heating up the detector, leak check the fittings

using a leak checker.

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 TCD Detector – Maintenance

Bake out Procedure

Caution: Take care the oven and detector parts may still be hot
enough to cause burns to the hands.

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 the column is not installed into the detector, cap the

detector using a no hole ferrule and nut or use a blanking
nut.

If no column is installed into the detector, turn of the

TCD filament to protect it from irreversible damage from
oxygen.

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.

Program the reference gas flow to approximately 20 –

30ml/min and program the detector temperature to
375°C.

Maintain the detector temperature at 375°C for 2-3

hours to bake out the detector from contaminants.

Once the bakeout is complete reinstall the column if

needed.

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 TCD Detector – Maintenance

Bake out Procedure

 Reload the analytical method, and let the oven, inlet

and detector temperatures stabilise before using for
analysis.

Once the column fittings have heat cycled, re-tighten if

necessary.

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 uECD

 uECD

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 uECD Detector – Overview

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.

Properties of 63Ni Amount

Half life 101.1 years
Emission max.65.87keV beta radiation
Melting Point 1453°C
Size of the active 6mm id, 4.2mm ht
part
Total activity of the 555MBq (15 millicuries) maximum
cell
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 uECD Detector – Tools and Consumables

Description Part #

Fused silica indented mixing liner G2397-

20540
Makeup gas adapter G2397-
80520
ECD wipe test kit 18713-
60050
Insulation (3/pk) 19234-
60715
Insulation cup assembly 19234-
60700
Nut, 1/4-inch Swagelok adapter (10/pk) 5180-4105

Ferrule, graphitized Vespel, 1/4-inch (10/pk) 5080-8774

Capillary column blanking nut 5020-8294

.530 Ferrule, Vespel/graphite, 0.8-mm id 0.45-mm 5062-3512

and 0.53-mm capillary columns (10/pk)
Ferrule, graphite, 1.0-mm id 0.53-mm capillary 5080-8773
columns (10/pk)
Column nut, finger-tight (for 0.53-mm columns) 5020-8293
Connect column to inlet or detector
.320 Ferrule, Vespel/graphite, 0.5-mm id 0.32-mm 5062-3514
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
.250 Ferrule, Vespel/graphite, 0.4-mm id 0.1-mm, 0.2- 5181-3323
mm, 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, CONFIENTIAL
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– For Internal
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 uECD Detector – Tools and Consumables

Description Part #

.100 and .200 Ferrule, Vespel/graphite, 0.37-mm id 5062-3516

0.1-mm and 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
All Ferrule, no-hole Testing (10/pk) 5181-3308

Capillary column blanking nut Testing–use with any 5020-8294

ferrule
Column nut, universal Connect column to inlet or 5181-8830
detector (2/pk)
Column cutter, ceramic wafer Cutting capillary columns 5181-8836
(4/pk)
Column

Column blanking nut 5020-8294

Column nut universal (inlet or detector) 5181-8830

Ceramic wafer 5181-8836

9/16 spanner

Methanol

Lint free gloves

¼ inch spanner

5/16 inch spanner

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 uECD Detector – Installation

Agilent G3497 MicroCell Electron Capture Detector

(uECD)

Parts required

ECD detector assy

uECD PCB

uECD EPC

uECD nameplate

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 uECD Detector – Installation

Power off the GC using the front on/off button and

remove the power cable from the rear of the GC.

Remove the pneumatics, detector and RHS panels

With an ESD wrist strap on, and attached to gnd,

remove the EPC module brackets by loosening the captive
screws.

EPC mounting brackets

Remove the round metal cutout for the detector using

diagonal cutters. Ensure the nibs are on the cutout to be
thrown away.

Remove the circular insulation plug and discard.

With a flat screwdriver, make a hole in the oven

insulation approximately ¼ inch ID.

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 uECD Detector – Installation

Open the oven door and clean away any

insulation material that has fallen through then fit
the uECD bottom insulation into the cavity.

With the detector assy rested on top of the GC

close the detector cavity, take the EPC and locate
the correct mounting position for the EPC.

Detector EPC slot

Position
Front detector Front
Back detector Back

Connect the communication cable to the EPC

module

Slide the EPC module into the vertical slot tracks

and ensure the cables are not being pinched.

Position the tubing into the channel between the

EPC slots to reach the detector, ensure the tubing
is free from the EPC module brackets.

Refit the EPC module brackets by tightening the

captive screws, ensure no cables or tubing is
pinched.

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 uECD Detector – Installation

Connect the uECD heater cable to the GC heater

connector, which is found on the right side of the GC
adjacent to the detector cutout.

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.

Secure the detector into place by tightening the 4

captive screws.

If there is excess tubing bend it carefully so that it is

neatly stored on top of the oven, ensure none of the
tubing will be pinched by the covers/panels.

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.

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 uECD Detector – Installation

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

retaining slots on the pcb

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 uECD Detector – Installation

electrometer signal ribbon cable connection

communication connection
Connect the electrometer cable to the eECD pcb.

Connect the comms cable to the uECD pcb. The comm

cable for the detector will be either labeled F-DET for the
front detector position or B-DET for the back detector
position.

Refit the instrument covers in reverse order, plug the

rear power cable and switch on the GC.

Using the front GC keypad, press the Configure, Front

Det or Back Det (depending on where the hardware has
been installed), then press Mode/Type and Enter.

On pressing enter a caution message will appear asking

for a reboot of the GC. To reboot the GC press Options,
Communications, Enter, and scroll down the Reboot the
GC?. Press On/Yes twice to reboot the GC and ensure the
changes take effect.

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 uECD Detector – Installation

Once the detector has been configured it will be

recognised as the uECD on the GC display, and all the
parameters related to the uECD will appear in the scroll
down menus for control of the uECD.

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.

When the EPC had been calibrated, configure both

pressure and gas type, then connect up the gas lines, and
leak check.

Fit the insulation cup.

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 uECD Detector – Installing a GC column

Installing a Capillary Column

Caution: Take care the oven and inlet parts may still be hot
enough to cause burns to the hands.

Load the general GC maintenance method.

To facilitate the installation of the column, thread a

clean septa onto the column.

Thread an inlet nut and ferrule onto the column. Always

use the appropriate nut and ferrule according to the id of
the column.

Cut the end of the column using a ceramic wafer to

ensure a clean square cut is achieved. The ceramic wafer
has a serrated and sharp side, use the sharp side to cut
the column. Inspect the quality of the cut using an eye
glass.

The column should always be cut after the nut and

ferrule have been threaded on.

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 uECD Detector – Installing a GC column

Installing a Capillary Column

Wipe the column with lint free tissue soaked with

a little methanol to remove any contamination.

Install the column into the detector, see table

below for instructions.
Column id ≥200um Column id ≤200um
Push column into adapter Use the septa to fix the depth.
until it stops at the
indentation
Retract 1-2mm From the tip of the ferrule to the
septa the column length needs to be
70mm (+/- 1mm)
Tighten column nut 5/16 Insert the column into the adapter
inch spanner on adapter and holding the septum, tighten the
and ¼ inch spanner on column nut until finger tight
column nut
Using 5/16 inch spanner on the
adapter and ¼ inch spanner the
column nut tighten the nut
 After heating up the detector leak check the
fitting using a leak checker.

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 uECD Detector – Installing a GC column

Installing a Capillary Column

 After heating up the detector leak check the

fitting using a leak checker.

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 uECD Detector – Maintenance

Replacing the Fused Silica Mixing Liner

Caution : The following safety measures are required
when working with the µECD – see agilent.com.
Wear clean, lint free gloves for this procedure.
(Need to take more pictures of this, maybe when course is being given).

 Load the GC maintenance program and wait until the

GC is ready.

Remove the insulation cup from the bottom of the

detector (inside the oven) if one is fitted.

Remove the GC column if it is installed, so that the

makeup gas adapter is left behind.

Remove the makeup gas adapter using a 9/16 spanner

to loosen the nut. Then carefully pull the makeup gas
adapter from the detector taking care not to bend the
tubing. The gas adapter fitting remains connected to the
gas supply tubing and it is ok for it to be left suspended in
the oven, whilst replacing the mixing liner.

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 uECD Detector – Maintenance

Replacing the Fused Silica Mixing Liner

 Take note there is a ¼ inch ferrule above the adapter

nut.

 Remove the adapter cap.

Carefully remove the mixing liner. Replacement is

required if the mixing liner is broken, chipped, or
contaminated.

 Clean the adapter cap using MeOH, by placing it into a

clean glass beaker with some MeOH and sonicating for 5-
10mins or until visibly clean. Also clean the outer surfaces
of the makeup gas adapter with MeOH and a lint free
tissue or lint free Q-tip.

 Fit a new mixing liner making sure the indentation of

the liner is the cap end (top) of the detector. Place the
cap on top of the mixing liner.

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 uECD Detector – Maintenance

Replacing the Fused Silica Mixing Liner

 Fit a new ¼ inch ferrule along with a new ¼ inch

swage lock fitting, make sure the correct orientation of
the ferrule.

Carefully push the adapter into the detector if needed

wiggle the adapter to ensure it is seated correctly into the
detector fitting. Take care not to chip the GC column end.

 Finger tighten the nut and then tighten using the 9/16
spanner until its snug

Top Tip : If the adapter has been fitted correctly, the

distance between the ¼ inch nut and the base of the
adapter is approx 19mm +/-1mm. However if this
distance is 22-23mm reinstall the adapter into the
detector.

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 uECD Detector – Maintenance

Installing the Insulation Cup

Caution: Take care the oven and detector parts may still be hot
enough to cause burns to the hands.

Load the GC maintenance method.

 To install the insulation cup first cap the detector with a

no hole ferrule and nut or a blanking nut to ensure no
insulation material enters the inlet.

 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.

Remove the no hole ferrule and nut or the blanking nut.

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 uECD Detector – Checks

Bake out Procedure

Caution : Taking apart or cleaning the uECD must be ONLY be
performed by trained and licensed (to handle radioactive
materials) personnel. Trace amounts of radioactive 63Ni maybe
removed using procedures causing possible hazardous exposure to
b- and x- radiation.

The bake out procedure is permitted.

To prevent possible hazardous contamination of the work

area with radioactive material, the µECD detector exhaust
vent must be connected to a fume hood or vented in
compliance with the local radioactive
regulations/agencies.

Obtain the detector output with both the oven and

detector at typical operating temperatures. On the GC
front keypad press either the Front Det or Back Det to
obtain the output value, record this for comparison.

Load the GC maintenance method.

Caution: Take care the oven and detector parts may still be hot enough to
cause burns to the hands.

If the column installed into the detector has a maximum

temperature of <250°C, remove it from the detector and
plug the detector with a no hole ferrule and nut or a
blanking nut.
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 uECD Detector – Checks

Bake out Procedure

If the column is still installed into the inlet, keep the
carrier gas flowing.

Program the µECD temperature to approximately 350°C

to 375°C.

Program the makeup gas flow to 60ml/min.

Program the oven temperature to 250°C, if the column

is installed into the detector. If the column is not installed
into the detector turn the oven off.

Bake out the detector for a number of hours and then

cool to typical operating temperatures.

Check the detector output reading and compare this to

the initial output value. The detector output after bake out
should be lower than the initial detector output.

Be sure to compare like for like, if the initial detector

output was taken with the column installed be sure to re-
install the column before taking the detector output after
bake out.

Reload the analytical method.

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 uECD Detector – Checks

Wipe Test Procedure

In the USA, the uECD must be tested for leakage of
radioactive materials every 6 months. uECD users outside
of the USA need to follow their local regulations and are
advised to contact the Nuclear Agency for advice on how
frequent the wipe test needs to be performed.
The records associated with the wipe test along with the
results need to maintained for possible inspection, by
regulatory bodies.
When the uECD is used heavily then a wipe test may be
perfumed more frequently e.g. every column change.

Wipe test kits are available for purchase from Agilent p/n
18713-60050. Items required for the wipe test are
included in the kit.

Caution : Wear disposable gloves whilst performing the

test, or once the test Is complete wash hands thoroughly.

Take 3 information cards and complete the details

required.

Take 3 pieces of filter paper and label them with pencil.

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 uECD Detector – Checks

Wipe Test Procedure

Sample 1 Detector Entrance

Fitting
Sample 2 Detector Housing
Sample 3 Detector Exit
Remove the column from the detector.

Using the filter paper labeled Sample 1, wipe the inside

and outside of the uECD entrance fitting, column and
adapter connections. Insert the filter paper and the
information card into one of the plastic bags provided in the
kit, and seal it.

Using the filter paper labeled Sample 2, wipe the ECD

housing. Insert the filter paper and the information card
into one of the plastic bags provided in the kit, and seal it.

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 uECD Detector – Checks

Wipe Test Procedure

Disconnect the exhaust tubing for the uECD vent tube.

Using the filter paper labeled Sample 3, wipe the side of
metal uECD exit fitting and/or the inside of the exhaust
tubing. Insert the filter paper and the information card
into one of the plastic bags provided in the kit, and seal it.
Refit the exhaust tubing.

Once all the filter papers are bagged remove gloves and
wash hands thoroughly with mild soap and water.

In the USA the uECD wipe samples must be analysed by

an NRC authorised company who have the facility to
analyse the samples. uECD users outside of the USA need
to follow their local regulations and are advised to contact
the Nuclear Agency for advice.

You will require written results from the wipe test

samples which can be documented and stored safely for
possible inspection.

If the results of the wipe test indicate leakage of ≥0.005

microcuries you must stop using the uECD immediately
and notify NRC or follow your local regulations.

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 uECD Detector – Checks

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.

The following criteria highlight possible

incidents/failures,
however the list is not exhaustive:-
1.High wipe test procedure - ≥0.005 microcuries
2.Temperature runaway – failure of temperature control
circuits in the GC along with the failure of overheat
protection circuits, which could cause the heating of the
detectors to exceed their limits
3.Physical damage – if the uECD is subject to fire, flood,
or any other event that may cause damage to the uECD
4.Modification of the uECD – any drilling, welding
soldering, sawing or other operations
5.Breakage of the uECD – if the inlet fitting or vent
tubing of the uECD is broken off, the uECD must be taken
out of service
6.Lost uECD - if the uECD is lost (including lost in
shipping), misplaced, or accidently disposed of

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 uECD Detector – Calibration

EPC Calibration Procedure

EPC modules can contain either flow sensors or pressure

sensors or both. These sensors are calibrated at
manufacture and are said to be quite stable, however its
recommended by Agilent to periodically update the zero
offset.

The uECD detector uses pressure sensors. It is also

recommended to zero pressure sensors periodically,
Agilent recommends for inlets using columns <0.32id
every 12 months, and for inlets using columns >0.32id
every 3, 6 and 12 months.

With the carrier gas supply disconnected at the rear of

the GC. Just turning the flow off will not adequately zero
the pressure sensor and the valve may leak.

 On the GC front keypad press the Options key.

Scroll to Calibration and press Enter.
Scroll to a zero line and press Info.
At this point you will need to confirm the gas supply is
NOT connected at the back panel of the GC.
Press On/Yes to zero or Clear to cancel

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 Repairs: Ovens

 6890 and 7890 have very similar ovens and

are the most common models
 The 6850 is a completely different design

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 7890 – Flow & Pressure Modules - Overview

The 7890 can use 4 different types of electronic flow or

pressure modules.

1.Inlet Modules
2.Detector Modules
3.Pressure Control Modules, (PCM)
4.Auxiliary Pressure Controllers, (Aux EPC)

All of the modules fit underneath the pneumatics cover.

Underneath the pneumatics cover, the modules fit into

designated slots all of which are numbered.

BACK OF GC

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 7890 – Flow & Pressure Modules - Overview

Under each slot in the pneumatics area of the GC there

are connections for each of the modules, of which each
are labelled. For the GC firmware to recognise which
module is installed the correct connections must be made.

For detector that are installed onto the LHS if viewing

the GC from the front, then it is controlled via EPC6 which
is routed over the top of the oven through the channel
between the pneumatics area and the split vent traps, and
is then feed through an opening in the detector carrier.

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 7890 - Aux EPC and PCM – Tools and
Consumables
Description Part #

Auxiliary Electronic Pressure Control (EPC)

O-rings, package of 6 5181-3344

Blue dot frit, high flow resistance G3430-

80063
Red dot frit, medium flow resistance G3430-
80062
Brown dot frit, low flow resistance G3430-
80061
No frit (brass tube), zero flow resistance G3430-
20011

Pressure Control Module (PCM)

O-rings, package of 12 5180-4181

Proportional valve, Carrier G3430-

67013
Proportional valve, AUX G3430-
67016

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 7890 – Flow & Pressure Modules - Inlet

Inlet Modules

Inlet modules control the amount of carrier gas supplied

to the inlet and septum purge.

Each module associated with an inlet is installed into a

specific slot in the pneumatics area which is dependent on
where the inlet is installed on the GC.

Inlet Position on Slot in Pneumatics Area

GC
FRONT SLOT 1
BACK SLOT 2

back

front

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 7890 – Flow & Pressure Modules - Detectors

Detectors Modules

Each detector module is specific to the detector it is

installed to. When installing detectors do not detach the
module tubing from the detector body.

The reason why each detector has it own modules is due

to the type of gases used. So for example the FID uses
air, hydrogen and makeup gas, however the TCD is
required to control a reference and makeup gas, but also
includes a reference switching valve.

Each module associated with an detector is installed into

a specific slot in the pneumatics area which is dependent
on where the detector is installed on the GC.

Detector Position on GC Slot in Pneumatics

Area
FRONT SLOT 3
BACK SLOT 4

The TCD can be installed onto the 7890 as a third

detector additional to those installed in slot 3 and 4. The
module is installed into the TCD frame which screws onto
the LHS of the GC.

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 7890 – Flow & Pressure Modules - PCM

Pressure Control Module (PCB)

A PCM is module with 2 independent control channels and
these are called 1 and 2. Channel 1 is a forward pressure
regulated channel, that can maintain constant flow through a
fixed resistor.

Channel 2 is either a forward pressure or back pressure

regulator. To switch between forward and back requires
changing the input/output connections. The back pressure
mode is used for gas sampling valves.

PCM’s are referred to as PCM# where the # is a letter,

dictates where the PCM can be installed.

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

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 7890 – Flow & Pressure Modules – Aux EPC

Auxiliary Pressure Controllers

 The Auxiliary pressure controller, (AUX EPC) has 3

independent forward pressure regulated channels.

Each channel is labelled from 1- 9.

Aux EPC 1, 2, 3 goes in slot 6
Aux EPC 4, 5, 6 goes in slot 5
Aux EPC 7, 8, 9 goes in slot 4

BACK OF GC

If a third detector like the TCD is fitted on the LHS

of the GC the Aux EPC is 7, 8, 9.

The auxiliary channels are controlled by pressure so

to provide set pressure points the must be flow
restriction. Each channel has a frit type restrictor
fitted.

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 7890 – Flow & Pressure Modules – Aux EPC

Frit Flow Resistance

Identification
Blue Dot High
Red Dot Medium
Brown Dot Low
None (brass tube) Zero
Installing or Replacing Frits in Aux EPC
Check that the frit being installed is correct for the type of gas to be
used, dangerously high flows of hydrogen could be supplied if insufficient
flow resistance is not provided by the frit.
Turn off the gas supply and select the fit to be installed.
Loosen the captive screw.

Lift the pneumatic tubing block to allow access to the frit

and o ring. Fit the replacement frit along with a new o-ring
and secure the pneumatic tubing block.

Turn the gas supply back on.

When a new frit has been installed, update the PID’s used
in the Aux EPC.

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 Autosampler Repair

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 7683 Autosampler - Installation

 To remove the 7693, disconnect both the tray and the

tower plug from the rear of the GC.

 Lift of the autosampler tower by lifting upwards until it

is clear from the retaining rod.

 Remove the autosampler vial racks by lifting them

upwards to unclick them from their positions

 Remove all 4 autosampler vial racks

 Note there is numbering on the underside of the

autosampler tray, when reinstalling the vial racks be sure
to place the relevant racks into their nominated positions.
Each vial rack is also numbered

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 7683 Autosampler - Installation

 The autosampler is now de-installed. To re-install

reverse the instructions.
The tower can be installed on either the front inlet or the
back inlet position. To enable the tower to work on either
the front or the back inlets, the cable at the rear of the GC
needs to be in either front injector or back injector.

Tower Tower
installe installed
d on on the
the front inlet
back
inlet

Inlet Position Cable Position

Front inlet Front injector
Back inlet Back injector
The 7683 can also be equipped with 2 towers installed at
the same time one on the front inlet and one on the rear
inlet. This enables the user to run samples without having
to physically move the tower from one position to the other.

1 2

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 7683 Autosampler – Installation

Changing the turret

There are 2 turrets which can be fitted.

8 sample vial turret

Bottle Name Bottle Bottle Use

Position
A 11 Solvent A
B 10 Solvent B
WA 9 Waste
1-8 1-8 Sample vials
1 sample vial turret

Bottle Name Bottle Position Bottle Use

Sample 1 Sample Vial
WB 2 Waste B
WB 3 Waste B
WA 4 Waste A
WA 5 Waste A
B3 6 Solvent B3
B2 7 Solvent B2
B 8 Solvent B
A3 9 Solvent A3
A2 10 Solvent A2
A 11 Solvent

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 Run SQT

 Confirm the instrument is back together

properly.
 Set up Empower for ER/ES
 Setup samples for your instrument
configuration
 Using the Wizard run SQT for your
instrument
— Use ER/ES

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 SQT: Check Results

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 GC Repair

 Discuss the policy for repair

 Discuss other detectors and inlets not
available in the lab

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