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GC Tips Tricks-Agilent (Compatibility Mode)

This document provides tips and tricks for troubleshooting common issues with gas chromatography systems and maintenance of inlets and detectors. It emphasizes the importance of using high purity gases, regularly maintaining and replacing consumables like columns, septa, filters, and traps. Various problems are discussed like peak issues, low response, baseline noise and their potential causes such as leaks, dirty components, or improper flow. Diagnostic procedures are presented for issues like checking for a plugged jet or inlet pressure shutdown.

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Sneha Patel
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566 views

GC Tips Tricks-Agilent (Compatibility Mode)

This document provides tips and tricks for troubleshooting common issues with gas chromatography systems and maintenance of inlets and detectors. It emphasizes the importance of using high purity gases, regularly maintaining and replacing consumables like columns, septa, filters, and traps. Various problems are discussed like peak issues, low response, baseline noise and their potential causes such as leaks, dirty components, or improper flow. Diagnostic procedures are presented for issues like checking for a plugged jet or inlet pressure shutdown.

Uploaded by

Sneha Patel
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 43

Tips and Tricks of Troubleshooting the GC System & Injector Maintenance

Jigar Patel

Page 1

Precautions

Use High(99.9995%) purity gases Perform regular inlet and detector maintenance Replace the consumables Column Reduce the Power switching of GC Maintain the log, Replace the gas line filters regularly

Page 2

Gases and filters

Page 3

GC Installation Carrier Gas, purity 99.9995%


Stainless Steel Diaphragm Tank Regulator 1/8 Swagelok NPT Adapter

1/8 Copper Tubing P/N 5180-4196

Moisture Trap P/N 5060-9084

Indicating O2 Trap P/N IOT-2-HP

Two 0100-2144 1/8-inch ball valves

Page 4

Gas purification panels


Determine desired purity level Keep number of fittings in gas line to a minimum Install purifiers in a convenient location close to the GC Use purifier log books to determine maintenance and cartridge replacement schedules Use indicating traps closest to the GC so you can determine when to change the traps that are upstream

Inline Filters

Page 5

Columns

Page 6

GC Capillary Column Preparation

Rough Edge New Column Ferrule


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.

Ceramic Column Cutter

Column Nut

Septum to mark Column Position

Page 7

Created 5//02

6850/90/7890 Column Installation Dimensions-Inlets


Inlets
Inlet Height PPIP 1-2 mm Split/Splitless 4-6 mm PCOC
All the way - until spring tension is felt

PTV 17 mm

VI 6 mm

Detectors
Detector Height TCD FID NPD uECD FPD 153 mm

All the way All the way All the way All the way back off 1-2 mm back off 1-2 mm back off 1-2 mm back off 1-2 mm

Original ECD
2 mm past tip of MUG adapter

Page 8

6850/90/7890 Column Installation Dimensions-FID Column Installation Video

Capillary Optimized FID

Adaptable FID

0 10 20 30 40 50

0 10 20 mm

mm

48mm

68mm

1mm

30 40 50 60 70

General Rule: Push to tip of Jet Then withdraw 1 mm

Page 9

Column connection to Inlet

Column front end

Page 10

Important..
Electronic Pneumatic Control.Fundamental Principle - 6850/90

Capillary Column Flow is Never Measured by the GC It is always calculated and controlled by Inlet Pressure...
6850/6890 Inlet EPC calculates column flow based on:

Column ID - most effect r2 Squared Function Column Length Film Thickness (usually negligible) Column Oven Temp Inlet Pressure Pressure at exit of column (usually 1 ATM) Ambient Pressure and Temperature (NTP) Fundamental Inlet Specification;
Pressure Accuracy: +/- 2% Full Scale Column Flow - NO SPECIFICATION

Page 11

Consumables

Page 12

Septa

Page 13

Septa related problems

Consumables

Page 14

Ferrule

Page 15

Liners
Split less

Split

Use vapor volume calculator


Page 16

Liner Maintenance
Liners become contaminated with use, collecting non-volatiles, salts, excess reagents, etc., or become damaged/cracked. Should inspect and replace liners often. Handle with gloves and forceps. Insert or remove liners only from cool injection ports. Replacing with a new liner is recommended, to ensure reproducibility

Page 17

Turn Top Inlet Sealing System on NEW 7890

- Fast/Easy Split/Splitless Inlet Maintenance

changing liners has never been easier

Page 18

Replace BecauseMost Common Causes of Leaks


Re-use and mis-installation.
Leak from O-ring, Gold Seal, ferrules, column nuts O-rings are elastomer compression fittings designed for one use, not perfectly elastic. Gold seals are designed for one use, knife edge cuts into gold layer giving leak tight seal w/o shrinkage or potential organic contaminants from polyimide out-gassing/degradation. Re-using could result in overlap in seal rings, resulting in a leak. Over-tightening of fittings

Page 19

Split Vent Trap

Page 20

Replacing the Split Vent Trap


Finger Tight Nut

G1544-80530

Page 21

FID Jet Selection Guide


There are two types of FID available. capillary optimized FID is only used with capillary columns, and adaptable FID fits packed columns and can be adapted to fit capillary columns.

Jets for the Capillary-Optimized FID


Jet type Capillary Capillary - High-temperature Part no. G1531-80560 G1531-80620 Jet tip id 0.29 mm (0.011-inch) 0.47 mm (0.018-inch)

Jets for the Adaptable FID


Jet type Capillary Capillary - High-temperature (use with simulated distillation) Packed Packed wide-bore (use with high-bleed applications) Part no. 19244-80560 19244-80620 Jet tip id 0.29 mm (0.011-inch) 0.47 mm (0.018-inch)

18710-20119 18789-80070

0.47 mm (0.018-inch) 0.030-inch

Page 22

GC Inlets

Page 23

Page 24

Where Does it Get Dirty?


Here Here Here

Here

Here
Maintenance??

Page 25

Inlet S/SL GC6890/50/7890 Shutdown!!

Fault: Back inlet pressure shutdown

Fault: Back inlet pressure shutoff

Mode: Temp 250 Pressure 3.2 Split Ratio Split Flow Tot Flow 205.0 Gas Saver Saver Flow Saver Time

Split 250 10.0 100 200 205.0 ON 50.0 0.5

Mode: Temp 250 Pressure 9.2 Split Ratio Split Flow Tot Flow 205.0 Gas Saver Saver Flow Saver Time

Split 250 2.6 100 200 205.0 ON 50.0 0.5

Page 26

GC Detector- FID

Page 27

Detector-FID
FID Flow Measurement Tool

FID Air

Column/M akeup and H2 Flows

Inlet EPC/Carrier Control

H2 and Makeup Gas From FID EPC module Flow between the jet and the outside of the column

Page 28

6850/6890 Jet Plugging Diagnostic can also be run from 6890 Front Panel or GC Chemstation
1 Set H2 to 75 ml/min Column can remain installed OR the FID can be capped keep in mind that jet plugging can be due to a column that is installed all the way to the tip of the Jet!

Page 29

6850/6890 Jet Plugging Diagnostic


2 Turn Makeup Gas to OFF

Page 30

6850/6890 Jet Plugging Diagnostic


3 Monitor Makeup Flow readout (or actual pressure)

Page 31

6850/6890 Jet Plugging Diagnostic


3 Monitor Makeup Flow readout (or actual pressure) If the Jet is not plugged all H2 flow will exit the jet and Makeup pressure will be close to 0 PSI (display reading 0 ml/min.)

Page 32

6850/6890 Jet Plugging Diagnostic


3 Monitor Makeup Flow readout (or actual pressure) If the Jet is plugged, or the column is installed too high H2 pressure will back up and be indicated as a flow/pressure on the Makeup Gas Channel

A positive Pressure (Flow Readout) will be indicated on Makeup Gas Sensor

Page 33

Flame Ignition problem


Measure flow H2, Air Jet Chocking How to clean? Does ignitor glow plug working? Are column and fittings are leak free? Cylinder pressures are enough?

Page 34

General problems

Page 35

Troubleshooting and Precautions

RT Variation Area variation Noise/Spikes Low response Peak splitting Inlet pressure shutdown

Page 36

RT Variation

Improper flow Jet chocking Column Parameters

Page 37

Area variation

Peak pattern/column issue ALS maintenance-Inj. Vol. variation

Page 38

Pressure variation

Leak EPC

Page 39

Low response

Sample Inj. volume Leak Jet chocking

Page 40

Peak splitting

Column Column connection Inlet-Liner

Page 41

Baseline noise/spikes

Detector cleaning Column conditioning Inlet cleaning Gas Purity

Page 42

Questions

All videos are available at below link


http://www.chem.agilent.com/en-US/Support/Installation/Pages/default.aspx

Page 43

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