This document provides instructions for installing gas chromatography (GC) columns and setting up GC inlets and detectors, including the purged packed injection port (PPIP) and thermal conductivity detector (TCD). It describes how to prepare and install capillary columns, set flows for the PPIP and TCD, and outlines checkout conditions and chromatograms to test the instruments. The document contains detailed steps, diagrams and examples to optimize the GC setup and component configurations.
This document provides instructions for installing gas chromatography (GC) columns and setting up GC inlets and detectors, including the purged packed injection port (PPIP) and thermal conductivity detector (TCD). It describes how to prepare and install capillary columns, set flows for the PPIP and TCD, and outlines checkout conditions and chromatograms to test the instruments. The document contains detailed steps, diagrams and examples to optimize the GC setup and component configurations.
This document provides instructions for installing gas chromatography (GC) columns and setting up GC inlets and detectors, including the purged packed injection port (PPIP) and thermal conductivity detector (TCD). It describes how to prepare and install capillary columns, set flows for the PPIP and TCD, and outlines checkout conditions and chromatograms to test the instruments. The document contains detailed steps, diagrams and examples to optimize the GC setup and component configurations.
This document provides instructions for installing gas chromatography (GC) columns and setting up GC inlets and detectors, including the purged packed injection port (PPIP) and thermal conductivity detector (TCD). It describes how to prepare and install capillary columns, set flows for the PPIP and TCD, and outlines checkout conditions and chromatograms to test the instruments. The document contains detailed steps, diagrams and examples to optimize the GC setup and component configurations.
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6850/6890 GC Column Installation and
Instrument Setup Guide - PPIP/TCD
July 14, 2004 Title of Presentation Date Agilent Restricted Page 2 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
Title of Presentation Date Agilent Restricted Page 3 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. Title of Presentation Date Agilent Restricted Page 4 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 Title of Presentation Date Agilent Restricted Page 5 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 Title of Presentation Date Agilent Restricted Page 6 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 Title of Presentation Date Agilent Restricted Page 7 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) Title of Presentation Date Agilent Restricted Page 8 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
Title of Presentation Date Agilent Restricted Page 9 6850/90 THERMAL CONDUCTIVITY DETECTOR Gas Connections Note: The Reference/Makeup Gas must be the same as the Carrier Title of Presentation Date Agilent Restricted Page 10 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 Title of Presentation Date Agilent Restricted Page 11 6850/90 Setup - TCD Column Installation - Original Capillary Adapter 6890 Operating Manual - Volume 1 Chapter 5, Part1 1. 2. 3. 4. Title of Presentation Date Agilent Restricted Page 12 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 Title of Presentation Date Agilent Restricted Page 13 6850/90 TCD - Front Panel Menu Turns Filament On and Off Output of Detector. 1 unit = 25uV Turns polarity between + and - 6890 TCD OPERATION Title of Presentation Date Agilent Restricted Page 14 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 Title of Presentation Date Agilent Restricted Page 15 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.
Title of Presentation Date Agilent Restricted Page 16 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.
Title of Presentation Date Agilent Restricted Page 17 6850/90 TCD Checkout Conditions Title of Presentation Date Agilent Restricted Page 18 6850/90 TCD Checkout Chromatogram 25 uV (Sampling Rate) 0 10 20 30 40 50 60 70