6850/6890 GC Column Installation and

Instrument Setup Guide - PPIP/TCD

July 14, 2004
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GC Setup and Capillary Column Preparation
Inlets:

Split/Splitless Capillary Inlet

PPIP - Purged - Packed Injection Port

PCOC - Programmable Cool on Column

PTV - Programmable Temperature Vaporization Inlet
LVI - Large Volume Injection

VI - Volatiles Interface

GSV - Gas Sampling Valve


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GC Capillary Column Preparation
Created 5//02
Ceramic Column Cutter
Rough Edge
New Column Ferrule
Column Nut
Septum to mark
Column Position
1) Slide a used Septum over the
column as a marker
2) Slide a Column Nut onto the
column
3) Slide a new Column Ferrule
onto the column
4) Score the column and snap off
the end
5) Inspect the column for a clean
cut.
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GC Inlet Systems - Purged Packed Injection Port
Maintenance Parts
Septum Purge Weldment
O Ring
Glass Liner Sleeve
Septum
1/4 Vespel Seal
Heater/Sensor
Assembly
Column Nut/Ferrule
Column Adapter
Septum Purge Weldment
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GC Inlet Systems - Purged Packed Injection Port
Column Adapters/liners - Capillary Column Installation
Capillary Packed Glass Insert
1-2mm
2
0
22
cm
Column Adapters/liners Capillary Column Installation
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6890 GC Inlets - Purged Packed Injection
Port
Maintenance:
Replace Septum
Replace Glass Liner
Replace Septum Purge Weldment O-Ring
Perform Inlet Leak Test
Run Customer Sample or Agilent Checkout
Replace 1/4 Vespel Ferrule
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Electronic Pneumatic Control.PPIP
Packed Column/Flow Control Mode -
Flow can be set, Pressure readout only
No Column assigned to inlet
Capillary/Pressure Control Mode -
Pressure can be set, Flow readout only
Selected by assigning a capillary column to the inlet (Config Column 1 or 2)
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GC Setup and Capillary Column Installation
Detectors:

FID - Flame Ionization Detector

TCD - Thermal Conductivity Detector

NPD - Nitrogen Phosphorous Detector

ECD/uECD - (micro) Electron Capture Detector

FPD - Flame Photometric Detector


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6850/90 THERMAL CONDUCTIVITY
DETECTOR
Gas Connections
Note: The Reference/Makeup Gas
must be the same as the Carrier
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6890 TCD Setup -
Detector Column Adapters
New Ferrule Design-6850/90
Original 6890 Design
Capillary Adapter
Old Style New Style
G1532-80540
0100-1332
5182-9677- .20/.250
5182-9676- .320
5182-9673- .530
5182-3477
Description Column ID mm Single part# 10 Pack#
Back Ferrule for 1/8" inlet G1530-80400 5182-3477
Frnt Ferr for 0.8mm OD Col 0.53 G1530-80410 5182-9673
Frnt Ferr for 0.53mm OD Col 0.32 G1530-80420 5182-9676
Frnt Ferr for 0.43mm+OD Col 0.25/0.20/0.1 G1530-80430 5182-9677
Front Ferrule, no hole G1530-80440 5182-9679
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6850/90 Setup - TCD Column Installation -
Original Capillary Adapter
6890 Operating Manual -
Volume 1 Chapter 5, Part1
1. 2.
3. 4.
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6850/90 Setup - TCD Column Installation -
New Capillary Adapter
Column Installation - from 6890N User Information
1- Slide the 1/8 swagelok Column Nut,
Back Ferrule and Front Ferrule
onto the column.

2- Trim the end of the column

3- Insert the column into the TCD and
thread the nut onto the fitting

4- Push the column all the way into the
Detector and withdraw 1-2 mm.

5- Tighten the column nut
1/8 Swagelok
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6850/90 TCD - Front Panel Menu
Turns Filament On and Off
Output of Detector. 1 unit = 25uV
Turns polarity between + and -
6890 TCD OPERATION
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6850/90 THERMAL CONDUCTIVITY
DETECTOR
Optimizing Makeup and Reference Flows
0510152025303540455055606570
0.5
1
1.5
2
2.5
3
3.5
Column+Makeupflow(ml/min)
R a t i o o f r e f f l o w t o M U + C o l f l o w
Thermal ConductivityReferenceGasFlow
ColumnFlow=25
Refflow=2X25=50
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6850/90 TCD - Optimizing Makeup and
Reference Flows
Setting TCD Flows in Packed Mode

The Packed Mode describes using the TCD with column flow rates between 15 and 60
ml/min. The reference flow should be set to 1.5 times the combined flow rate of the
column plus make-up gas. Make-up gas is recommended whenever a capillary column
is used. This allows the column to be installed all the way into the detector and
withdrawn one millimeter. If make-up is not used then the end of the column should be
no more than three millimeters above the ferrule. Otherwise excessive tailing will occur.
The minimum make-up flow is 1 ml/min.

.Example 1: 1/8 Stainless Steel Column If the column flow = 30 ml/min, then the
reference flow should be set to (30ml/min) (1.5) = 45 ml/min. Therefore total detector
flow is 30 + 45 = 75 ml/min.

.Example 2: 10 Meter X 530 uM column If the column flow = 15 ml/min and the
make-up flow = 2 ml/min, then the reference flow should be set to (15 ml/min + 2
ml/min) (1.5) = 25.5 ml/min. Therefore the total detector flow is 17 + 25.5 = 42.5 ml/min.


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6850/90 TCD - Optimizing Makeup and
Reference Flows
Setting Flows in Capillary Mode

The Capillary Mode describes using the TCD with a combined column plus make-up
flow of less than 15 ml/min. The combined column plus make-up flow must not be
less than 5 ml/min. The reference flow rate should be set to optimize detector
response. This will result in a reference flow of approximately two times the combined
column plus make-up flow for a column plus make-up flow of 10-15 ml/min. For a column
plus make-up flow of 5 - 10 ml/min, a multiplier of three is used. The detector output will
be within 25% of the maximum response. The response can be further optimized by
adjusting the reference flow. The make-up flow should not be less than 1 ml/min.

.Example 3: 2 Meter X 200 uM capillary column If the column flow rate = .75 ml/min,
then the make-up flow must be at least 4.25 ml/min. Set the make-up flow to 5 ml/min.
The optimum reference flow will be (5.75 ml/min) (3) = 17.25 ml/min. The total detector
flow will be 5.75 + 17.25 = 22.5 ml/min.

.Example 4: 25 Meter X 320 uM capillary column if the column flow rate = 10
ml/min, then the make-up flow should be set low to minimize sample dilution. Set the
make-up to 2 ml/min. The reference flow will = (12 ml/min) (2) = 24 ml/min. The total
detector flow will be 12 + 24 = 36 ml/min.

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6850/90 TCD Checkout Conditions
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6850/90 TCD Checkout Chromatogram
25 uV
(Sampling Rate)
0
10
20
30
40
50
60
70