Agilent Technologies 6890N Betriebsanleitung

Agilent Technologies

Agilent 6890N

Gas Chromatograph

Troubleshooting

Notices

No part of this manual may be reproduced

in any form or by any means (including

electronic storage and retrieval or transla-

tion into a foreign language) without prior

agreement and written consent from Agi-

lent Technologies, Inc. as governed by

United States and international copyright

laws.

Manual Part Number

G1530-90011

Edition

March 2007

Printed in USA

Agilent Technologies, Inc.

2850 Centerville Road

Wilmington, DE 19808-1610 USA

Warranty

The material contained in this docu-

ment is provided “as is,” and is sub-

ject to being changed, without notice,

in future editions. Further, to the max-

imum extent permitted by applicable

law, Agilent disclaims all warranties,

either express or implied, with regard

to this manual and any information

contained herein, including but not

limited to the implied warranties of

merchantability and fitness for a par-

ticular purpose. Agilent shall not be

liable for errors or for incidental or

consequential damages in connection

with the furnishing, use, or perfor-

mance of this document or of any

information contained herein. Should

Agilent and the user have a separate

written agreement with warranty

terms covering the material in this

document that conflict with these

terms, the warranty terms in the sep-

arate agreement shall control.

Safety Notices

CAUTION

A CAUTION notice denotes a hazard. It

calls attention to an operating

procedure, practice, or the like that, if

not correctly performed or adhered to,

could result in damage to the product

or loss of important data. Do not

proceed beyond a CAUTION notice

until the indicated conditions are fully

understood and met.

WARNING

A WARNING notice denotes a hazard.

It calls attention to an operating

procedure, practice, or the like that, if

not correctly performed or adhered to,

could result in personal injury or death.

Do not proceed beyond a WARNING

notice until the indicated conditions

are fully understood and met.

Troubleshooting 3

Contents

1 Concepts and General Tasks

Concepts 8

How to troubleshoot using this manual 8

The [Status] key 8

Configurable Items to Always Keep Current 9

Column configuration 9

Automatic Liquid Sampler configuration 9

Gas configuration 9

Information to Obtain Before Calling Agilent for Service 10

2 Hardware Symptoms

Plunger Errors 12

Vial Mishandled by ALS 13

Syringe Needle Bends During Injection into Inlet 14

FID Does Not Ignite 15

FID Ignitor Does Not Glow During Ignition Sequence 16

Corrosion in FID Collector and Ignitor Glow Plug 17

FPD Does Not Ignite 18

NPD Adjust Offset Process Fails 19

3 Chromatographic Symptoms

Retention Times Not Repeatable 22

Peak Areas Not Repeatable 23

Contamination or Carryover 24

Isolate the source 24

Check possible causes—all inlet and detector combinations 24

Larger Peaks Than Expected 25

Peaks Not Displayed/No Peaks 26

Table 1. Detector troubleshooting 26

Baseline Rise During Oven Temperature Program 27

4Troubleshooting

Poor Peak Resolution 28

Peak Tailing 29

NPD 29

Peak Boiling Point or Molecular Weight Discrimination Poor 30

For any inlet operating in split mode with any detector 30

For any inlet operating in splitless mode with any detector 30

Sample Decomposition in Inlet/Missing Peaks 31

Peak Fronting 32

Noisy Detector, Including Wander, Drift, and Baseline Spikes 33

Noisy baseline 33

Baseline wander and drift 34

Baseline spiking 34

Figure 1. Cyclic spiking 35

Figure 2. Random spiking 35

Check for the correct jet. Low Peak Area or Height 36

FID Flame Goes Out During a Run and Attempts to Reignite 38

FID Baseline Output Above 20 pA 39

FPD Flame Goes Out During a Run and Attempts to Reignite 40

FPD Output Too High or Too Low 41

FPD Low Peak Areas 42

FPD Large Peak Width at Half-Height 43

FPD Baseline Output High, > 20 pA 44

NPD Solvent Quenching 45

NPD Response Low 46

NPD Baseline Output > 8 million 47

NPD Adjust Offset Process Not Functioning Properly 48

NPD Low Selectivity 49

Negative Peaks Seen with TCD 50

TCD Baseline Has Dampened Sinusoidal Noise Trailing Peaks (Ringing

Baseline) 51

TCD Peaks Have Negative Dip on Tail 52

4 GC Not Ready Symptoms

GC Never Becomes Ready 54

Flow Never Becomes Ready 55

Troubleshooting 5

Oven Temperature Never Cools Down/Cools Very Slowly 56

Oven Never Heats Up 57

Temperature Never Becomes Ready 58

Cannot Set a Flow or Pressure 59

A Gas Does Not Reach Setpoint Pressure or Flow 60

A Gas Exceeds Pressure Setpoint or Flow 61

The Inlet Pressure or Flow Fluctuates 62

Cannot Maintain a Pressure as Low as the Setpoint on a Split Inlet 63

The Measured Column Flow Does Not Equal the Displayed Flow 64

FID Does Not Ignite 65

FID Ignitor Does Not Glow During Injection Sequence 66

NPD Adjust Offset Process Fails 67

FPD Does Not Ignite 68

5 Shutdown Symptoms

Column Shutdown 70

Hydrogen Shutdown 71

Thermal Shutdowns 72

6 Nonfunctional GC Symptoms

GC Does Not Turn On 74

PC Cannot Communicate with GC 75

7 Checking for Leaks

Leak Check Tips 78

To Check for External Leaks 79

To Check for GC Leaks 81

Leaks in Capillary Flow (Microfluidic) Fittings 82

8 Troubleshooting Tasks

To Measure a Column Flow 84

Measuring FID, TCD, uECD, and FPD column flow 84

Measuring NPD column flow 85

To Measure a Split Vent or Septum Purge Flow 87

To Measure a Detector Flow 89

Measuring FID, TCD, uECD, and FPD flows 89

6Troubleshooting

Measuring NPD flows 90

To Perform the GC Self-Test 92

To Adjust the FID Lit Offset 93

To Verify That the FID Flame Is Lit 94

To Verify FID Ignitor Function During Ignition Sequence 95

To Measure FID Leakage Current 96

To Measure FID Baseline Output 97

To Measure NPD Leakage Current 98

To Verify That the NPD Bead Is Ignited 99

To Verify That the FPD Flame Is Lit 100

To Adjust the FPD Lit Offset 101

Agilent 6890N Gas Chromatograph

Troubleshooting

Agilent Technologies

Concepts and General Tasks

Concepts 8

Configurable Items to Always Keep Current 9

Information to Obtain Before Calling Agilent for Service 10

8Troubleshooting

1Concepts and General Tasks

Concepts

This manual provides lists of symptoms and corresponding

tasks to perform should you experience errors associated with

GC hardware or chromatographic output, GC Not Ready

messages, and other common issues.

Each section describes a problem and provides a bulleted list of

possible causes for you to troubleshoot. These lists are not

intended for use in the development of new methods. Proceed

with troubleshooting under the assumption that method(s) are

working properly.

This manual also includes common troubleshooting tasks as

well as information needed prior to calling Agilent for service.

How to troubleshoot using this manual

Use the following steps as a general approach to

troubleshooting:

1Observe the symptoms of the problem.

2Look up the symptoms in this manual using the Table of

Contents or the Search tool. Review the list of possible causes

of the symptom.

3Check each possible cause or perform a test that narrows the

list of possible causes until the symptom is resolved.

The [Status] key

Be sure to also use the [Status] and [Info] keys on the GC keypad

while using this troubleshooting information. These keys will

display additional useful information related to the status of the

GC and its components.

Concepts and General Tasks 1

Troubleshooting 9

Configurable Items to Always Keep Current

Certain configurable items in the GC must always be kept

current. Failure to do so will lead to reduced sensitivity,

chromatographic errors, and possible safety concerns.

Column configuration

Reconfigure the GC every time a column is trimmed or changed.

Also verify that the data system reflects the correct column

type, length, id, and film thickness. The GC relies on this

information to calculate flows. Not updating the GC after

altering a column causes incorrect flows, changed or incorrect

split ratios, retention time changes, and peak shifts.

Automatic Liquid Sampler configuration

Keep the Automatic Liquid Sampler (ALS) configuration

up-to-date to ensure proper operation. ALS items to keep

current include injector position, installed syringe size, and

solvent and waste bottle usage.

Gas configuration

Reconfigure the GC every time the gas type is changed. If the GC

is configured to a gas other than what is actually being

plumbed, incorrect flow rates will result.

WARNING Always configure the GC appropriately when working with

hydrogen. Hydrogen leaks quickly and poses a safety concern if

too much of it is released into the air or into the GC oven.

10 Troubleshooting

1Concepts and General Tasks

Information to Obtain Before Calling Agilent for Service

Gather the following information before contacting Agilent for

service:

•Symptoms

•Problem description

•Hardware installed and parameters/configuration when the

error occurred (sample, supply gas type, gas flow rates,

detectors/inlets installed, and so forth)

•Any messages that appear on the GC display

•Results of any troubleshooting tests you have run

•Press the [Status] key to display previous Error, Not Ready, and

Shutdown messages.

To obtain service/support contact numbers, see the Agilent Web

site at www.agilent.com/chem.

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