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GC3-Natural Gas Analysis Advanced User Guide


Manual Information




Author(s):

C. Bennight

Reviewer(s):

L. Brandt, C. Neal, K. Marsaglia

Editor(s):

K. Graber, L. Peters

Management Approval (Name, Title, Date):

D.J. Houpt, Supervisor of Analytical Systems, 9/24/2010

Audience:

Research Specialists, Laboratory Technicians

Origination date:

5/12/2008

Current version:

Version 1.0 09/24/2010

Revised:

 

Domain:

Chemistry

System:

Gas Chromatography

Keywords:

Hydrocarbons, headspace gas, methane, ethane

...

Summarize requested modifications to this user guide in an e-mail and/or annotate the PDF file and e-mail change requests to techdoc@iodp.tamu.edu.


User Guide Contents




Topic

See page…

Introduction

Instrument Installation & Setup

GC3 & NGA Startup

LIMS Data Upload

Maintenance & Troubleshooting (HP6890GC)

...




Introduction


Overview


The absolute quantity of hydrocarbons combined with the potential for trapping and accumulating hydrocarbons is the primary safety risk during shipboard operations. Gas monitoring via gas chromatography (GC) analysis is a means of quanitfying the risk posed by these factors. Figure 1 depicts the safe ranges for gas concentrations (C1/C2) vs. temperature.
anchor
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Anchor_Ref302630297_Ref302630297
Figure 1. Risk Assessment for Drilling Safety (IODP).
Hydrogen sulfide (H2S) is another significant risk factor for individuals working in the area. Early detection of H2S is accomplished by emergency monitors on the drill floor, and later quantification is performed on the natural gas analyzer (NGA).

...

Catagenesis, the principal zone of oil formation, refers to a temperature range of 50°C~150°C. Liquid and gaseous hydrocarbons together with organic compounds with heteroatoms (oxygen, sulfur, and nitrogen) are released from the kerogen (Figure 2), so the catagenesis stage is called the "oil window."


Metagenesis


The last stage of sedimentary organic matter alteration is metagenesis. Dry gases (mainly methane) are derived from liquid hydrocarbon accumulation in the crust (Figure 3). C1–C4 hydrocarbons may be generated in significant quantities in sediment via biogenic and thermogenic processes.

...

...


Image Added
Figure 2. Hydrocarbon Formation Pathways in Geological Situations (Rullkotter, 1993).

...


Image Modified

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Figure 3. Hydrocarbon Generation Resulting from Burial of Organic Matter during Geologic Time.


Hydrogen Sulfide


Sulfate reducing bacteria produce H2S in euxinic sediments (Raiswell and Berner, 1985). Biogenic alteration of organic matter may occur in a relatively shallow part of the sediment. Thermochemical sulfate reduction of sulfate by hydrocarbons in reservoirs occurs under high temperature (>127°C ~ 140°C) (e.g., Orr, 1974; Worden et al., 1995).

...

  • Methane (CH4)
  • Ethene (C2H4)
  • Ethane (C2H6)
  • Propene (C3H6)
  • Propane (C3H8)


...

The GC3 instrument has a 1/6-inch VALCO union injector with a 2 µm stainless steel screen and a 10 port VALCO valve that is electrically switched (Figure 4). An 80/100 mesh 8 ft HaySep "R" packed column (2.0 mm ID x 1/8 inch OD) is installed in the oven.
Image Modified

...


Figure 4. Schematic of Sample Gas Line in the GC3.


NGA


The NGA is used to determine the concentrations of nonhydrocarbon gases along with hydrocarbons from C1 to C7. The analytes measured on this instrument are:

...

The TCD flow path contains the following columns (Figure 5):


  • 6 ft x 2.0 mm ID stainless steel column packed with Poropak T (50/80 mesh)
  • 3 ft x 2.0 mm ID stainless steel column packed with molecular sieve 13x (60/80 mesh)
  • 6 ft x 2.0 mm ID stainless steel column packed with 80/100 mesh HaySep R (acid wash)


...

The FID flow path has a 60 m x 0.25 mm ID with 0.25 µm film thickness DB-1 capillary column.

...


Image Modified

...


Figure 5. Schematic of a Sample Gas Line in the GC-NGA.

...

...


...

Instrument Installation & Setup


Agilent 6890 GC Specifications

...

  • Air, compressed (Zero-Air +): >50 psi
  • Helium, compressed (99.9995% +): >50 psi
  • Hydrogen, compressed (99.9995% +): >50 psi

...


GC3 Method: GC390FR.M


h7.Injector


  • Injection source: manual
  • Injection location: front

...

  • Initial temperature: 90°C
  • Maximum temp: 250°C
  • Initial time: 0.50 min
  • Equilibration time: 1.00 min
  • Port temp: 100°C
  • Post time: 0.00 min
  • Run time: 8.60 min (run time will automatically be changed based on ramp setting)
  • Temperature program:

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    30.00

    100

    0.00

    2

    15.00

    110

    4.50

    3

    50.00

    150

    1.80

    4

    0.00 (grey lightbulb) (grey lightbulb)

     

     


    h7.Front Inlet

  • Initial temp: 120°C (lightbulb) (lightbulb)
  • Flow: 30.6 mL/min (lightbulb) (lightbulb)
  • Gas type: helium


h7.Column 1

...

  • Packed column (model #: Restek PC3970)
  • HaySep "R" 80/100, 2.00 mm ID x 1/8 inch OD, 6 ft
  • Max temperature: 225°C
  • Mode: ramped flow
  • Initial flow: 30.0 mL/min
  • Initial time: 2.70 min
  • Post flow: 0.0 mL/min
  • Inlet: front
  • Outlet: front detector
  • Outlet pressure: ambient
  • Temperature program:

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    100.00

    40

    3.00

    2

    10.00

    30

    0.30

    3

    100.00

    60

    0.00


    h7.Column 2 (not installed)
    h7.Front detector (FID)

  • Temperature: 250°C (always on)
  • Hydrogen (H2) flow: 40.0 mL/min (on if FID temperature is >150°C, auto control)
  • Air flow 400.0 mL/min (on if FID temperature is >150 °C, auto control)
  • Mode*: constant makeup flow
  • Makeup flow*: 25.0 mL/min
  • Makeup gas type*: nitrogen (*Makeup flow: none; makeup gas: none)
  • Flame: on (auto on when FID temperature reaches 150°C)
  • Electrometer: on
  • Lit offset: 1.0

...

  • Data rate: 5 Hz
  • Type: front detector
  • Save data: On
  • Zero: 0.0 (grey lightbulb) (grey lightbulb)
  • Range: 0
  • Fast peaks: off
  • Attenuation: 0

...

  • Data rate: 20 Hz
  • Type: front detector
  • Save data: Off
  • Zero: 0.0 (grey lightbulb) (grey lightbulb)
  • Range: 0
  • Fast peaks: off
  • Attenuation: 0

...

  • Gas type: helium
  • Initial pressure: 0.00 psi (grey lightbulb) (grey lightbulb)


h7.Valves


  • Valve 5 switching off

...

  • 0.01 min—Valve 5 on; 6.00 min—Valve 5 off

...


...

GC3 Sample Flow Schematics


Standby Mode


Green line shows helium carrier gas flow when GC3 is in standby mode.

...

  • Inlet—injector port—V6—V7—V9—V8—column—V1—V10—FID

...

...


Image Modified
Figure 6. GC3 in Standby Mode.


Injection Mode


He carrier (green) and sample (red) gas flows during injection mode. Sample gas fills the 25 µL sample loop.

...

  • Sample gas: injector—V3—V2—V5—V4—vent
  • Carrier gas: Inlet—injector port—V6—V7—V9—V8—column—V1—V10—FID

...


...

Image Modified
Figure 7. GC3 in Injection Mode.


Run Mode


He carrier (green) and sample (red) gas flows during the sample run. When the valve is turned, helium coming from the inlet pushes the sample gas trapped in the sample loop.

...

  • Sample gas: column—FID
  • Carrier gas: V5—V2—V1—column—V8—V7—V9—V10—FID


Image Modified

...


Figure 8. GC3 in Run Mode.


NGA Method: NGA_CS.M


h7.Injector


  • Injection source: manual
  • Injection location: front


h7.Oven


  • Initial temp: 50°C
  • Maximum temp: 300°C
  • Initial time: 2.00 min
  • Equilibration time: 1.00 min
  • Port temp: 50°C
  • Post time: 0.00 min
  • Run time: 14.80 min (run time will be changed based on ramp setting)
  • Temperature program:

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    8.00

    70

    0.00

    2

    25.00

    200

    5.10

    3

    0.00 (grey lightbulb) (grey lightbulb)

    NA

    NA

    h7.

    Front Inlet

  • Flow: 21.0 mL/min (lightbulb) (lightbulb)
  • Gas type: helium


h7.Back inlet


  • Initial temp: 80°C (lightbulb) (lightbulb)
  • Initial time: 0.00 min
  • Cryo: off
  • Cryo type: compressed air
  • Pressure: 20.75 psi (On)
  • Gas type: helium
  • Temperature program:

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    0.00 (grey lightbulb) (grey lightbulb)

    NA

    NA

    h7.

    Column 1: Not installed

    h7.Column

           Column 2

  • Capillary column (model #: Agilent 122-1062)
  • Agilent DB-1 (dimethylpolysiloxane) 60.0 m x 0.25 mm diameter x 0.25 µm film thickness
  • Max temperature: 325°C
  • Mode: constant flow, 2.0 mL/min
  • Inlet: back inlet
  • Outlet: back detector
  • Outlet pressure: ambient


h7.Front detector (FID)


  • Temperature: 250°C (always on)
  • Hydrogen (H2) flow: 40.0 mL/min
  • Air flow 400.0 mL/min
  • Mode*: constant makeup flow
  • Makeup flow*: 50.0 mL/min
  • Makeup gas type*: helium
  • Flame: On
  • Electrometer: on
  • Lit offset: 2.0


h7.Back detector (TCD)


  • Temperature: 200°C (always on)
  • Reference flow: 45.0 mL/min (lightbulb) (lightbulb)
  • Mode: constant makeup flow
  • Makeup flow: 3.0 mL/min
  • Makeup gas type: helium
  • Filament: on
  • Negative polarity: off



h7.Signal 1


  • Data rate: 5 Hz
  • Type: back detector
  • Save data: on
  • Zero: 0.0 (grey lightbulb) (grey lightbulb)
  • Range: 0
  • Fast peaks: off
  • Attenuation: 0


h7.Signal 2


  • Data rate: 5 Hz
  • Type: front detector
  • Save data: on
  • Zero: 0.0 (grey lightbulb) (grey lightbulb)
  • Range: 0
  • Fast peaks: off
  • Attenuation: 0


h7.Column comp 1


  • Derive from front detector


h7.Column comp 2


  • Derive from back detector


h7.Thermal AUX 1 & 2


  • Use: valve box heater
  • Initial temp: 110°C
  • Initial time: 0.00 min

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    0.00 (grey lightbulb) (grey lightbulb)

    NA

    NA

    h7.

    AUX pressure 3

  • Gas type: helium
  • Initial time: 4.50 min

    Ramp

    Rate (°C/min)

    Final Temperature (°C)

    Final Time (s)

    1

    30.00

    22.20

    0.00

    2

    1.10

    27.50

    0.00

    3

    0.00 (grey lightbulb) (grey lightbulb)

    NA

    NA

    h7.

    Aux pressure 4 & 5

  • Gas type: helium
  • Initial pressure: 0.00 psi (grey lightbulb) (grey lightbulb)



h7.Valves (1 to 4, initial): Switching off


  • Valve control time program

    Time (min)

    Valve control

    0.00

    valve 1: off

     

    valve 2: off

     

    valve 3: off

     

    valve 4: off

    0.01

    valve 4: on


    0.07

    valve 1: on

     

    valve 2: on

    1.80

    valve 3: on

    1.83

    valve 4: off

    8.50

    valve 3: off

    9.10

    valve 1: off

     

    valve 2: off

    AnchorRTF39323538363a203348656164RTF39323538363a203348656164


    NGA Sample Flow Schematics

    Standby Mode

    He gas flow for standby mode (green lines).
  • Line 1: Aux-3—V1-4—V2-5—V2-3—capillary column—V2-4—V2-1—FID
  • Line 2: Aux-4—sample inlet—V1-2—V1-3—V1-6—V1-1—V3-3—V3-4—V3-1—V4-3—V4-2—V4-5—V4-4—Vent
  • Line 3: Front inlet—V3-5—V3-6—HaySep R column—V3-8—V3-7—V4-9—V4-8—TCD
  • Line 4: Back inlet—V4-6—V4-7—MolSieve column—V4-1—V4-10—Vent

...

...


Image Modified
Figure 9. NGA in Standby Mode.


Injection mode


He carrier gas (green line) and sample gas (red line) flows in the NGA in injection mode. Sample gas fills the sample loops connected to V1 (25 µL), V3 (1 cm3), and V4 (0.5 cm3). He flushes the separation columns.
He gas flow (green):

...

  • Sample inlet—V1-2—V1-3—V1-6—V1-1—V3-3—V3-4—V3-1—V3-2—V4-3—V4-2—V4-5—V4-4—Vent

...


...

Image Modified
Figure 10. NGA in Injection Mode.


Run Mode at 0.01 min (open Valve V4)

...

  • V4-5—V4-2—V4-1—MolSieve column—V4-7—V4-8—TCD

...

...


Image Modified
Figure 11. NGA in Run Mode: 0.01 min after starting run.


Run Mode at 0.07 min (open Valves V1 and V2)

...

  • V4-8—TCD
  • V1-3—V1-6—V1-5—V2-3—V2-4—capillary column—V2-2—V2-1—FID
  • V1-1—V3-3


Image Modified

...

Figure 12. NGA in Run Mode: 0.07–1.79 min after starting run.


Run Mode at 1.80 min (open Valve V3)

...

  • Capillary column—V2-2—V2-1—FID
  • B3-4—V3-1—V3-8—HaySep R column—V3-6—V3-7

...



Figure 13. NGA in Run Mode: 1.80–1.82 min after starting run.


Run Mode at 1.83 min (close Valve V4)

...

  • Line 4: Back inlet—V4-6—V4-7—MolSieve column—V4-1—V4-10—vent


Image Modified
Figure 14. NGA in Run Mode: 1.83–8.49 min after starting run.


Run Mode at 8.50 min (close Valve V3)

...

  • Line 3: Front inlet—V3-5—V3-6—HaySep R column—V3-8—V3-7—V4-9—V4-8—TCD

...


Image Modified
Figure 15. NGA in Run Mode: 8.50–9.09 min after starting run.


Run Mode at 10.0 min (close Valves V1 and V2)

...

  • Line 1: Aux-3—V1-4—V1-5—V2-3—V2-2—capillary column—V2-4—V2-1—FID
  • Line 2: Aux-4—V1-2—V1-3—V1-6—V1-1—V3-3—V3-4—V3-1—V3-2—V4-3—V4-2—V4-5—V4-4—out
  • Line 3: Front inlet—V3-5—V3-6—HaySep R column—V3-8—V3-7—V4-9—V4-8—TCD
  • Line 4: Back inlet—V4-6—V4-7—MolSieve column—V4-1—V4-10—vent

...


Image Modified
Figure 16. NGA in Run Mode: 9.09–10.0 min after starting run.

...


GC3 & NGA Startup


Overview


The chromatography application ChemStation controls GC data acquisition and processing. It can be run either online or offline. Offline mode can be run without communication with the GCs, so it is useful for reintegrating or reprocessing chromatograms. Online mode requires communication with the GC.

...

Starting up GC3/GC-NGA and ChemStation





Start ChemStation software and load the appropriate method for the analysis (see Starting up ChemStation and GC Ovens).


Condition the GC (see Conditioning the GC). If the GC has been turned off for longer than a week, then bake the column for 8 hr with gas flowing (manually set the oven temperature to 175°C for GC3 or 275°C for NGA).


Run a calibration curve (see GC3/NGA User Guide).


Run a calibration verification standard (see GC3/NGA User Guide)


Run a test sample (see GC3/NGA User Guide)

...






Starting up ChemStation and GC Ovens



Turn on the GC. WARNING: Before turning on the GC, make sure the gas lines are open.
The 6890 GC performs a comprehensive self-evaluation and shows real-time diagnostics on the screen. Warning, Fault, or Bad Main Board & Fatal Error messages require troubleshooting before moving to the next step (see Maintenance & Troubleshooting (HP6890GC)).


Turn on the PC.


Click the GC3 Online or NGA Online icon to start ChemStation. The Method and Run Control window opens. At startup, ChemStation uses the method last used (shown on the main screen). In addition, the GC LCD shows the loaded settings from ChemStation.
Settings changed on the GC using the GC control panel are also made to ChemStation, and parameter changes entered into ChemStation are made to the GC. ChemStation will prompt to save changes.


To load a different method in Chemstation:

  • Click Method > Load Method, select the method from the list, and press OK or
  • Click the Method tab on the left side of the window and select a method to load

The system automatically loads the new method selected in ChemStation to the appropriate GC. Oven and detector temperatures may increase immediately after a new method is loaded, and the FID will ignite when the detector temperature reaches 150°C. Sometimes, the GC beeps because the FID flame is out, especially after a long idle period. See Maintenance & Troubleshooting (HP6890GC).




GC3 Methods


Method Title

Definition

GC390FR.M

Standard operation method since November 2007.

def_gc.m

Default for ChemStation. This method must be kept in the Method folder permanently.

cbt.m

Default method for training.

estd_ex.m

Default method for training.

istd_ex.m

Method created onshore to make conditions for GC3.




NGA Methods


Method title

Definition

NGA_CS

Standard operation method since November 2007.

NGA_308

Method for IODP phase 1, Expedition 308.

def_gc.m

Default for ChemStation. This method must be kept in the Method folder permanently.

cbt.m

Default method for training.

estd_ex.m

Default method for training.

istd_ex.m

Method created onshore to make conditions for GC3.

...


Conditioning the GC



To condition the GCs, in the Main menu click RunControl > Sample Info.


Fill in the following fields:

  • Operator name: your last name
  • Sample name: "cond" for conditioning
  • Comment: "Conditioning"
    Click OK to close window and save information.

Prepare laboratory air (5000 µL) and inject it into the GC when the ChemStation software shows Ready.


Press the Start button on the GC control panel to start the run.


Confirm the chromatogram on the screen shows no peaks. If peaks are present, the system contamination must be found (injector, detector, sample loop, etc.).

...




...

LIMS Data Upload


Overview


Data is uploaded from the GC3 and NGA in one of two modes:

...

If MUT is not running when the GC finishes, files will queue in the data directory for manual upload.

...


Maintenance & Troubleshooting (HP6890GC)


Overview


Use the Status and Info keys on the GC keypad as a first check when something goes wrong.

...

Column Size and Carrier Gas Flow Rate




Column type

Column ID

Carrier gas flow rate (mL/min)

 

 

 

Hydrogen

Helium

Packed

1/8 inch

 

30

 

1/4 inch

 

60

Capillary

50 µm

0.5

0.4

 

100 µm

1.0

0.8

 

200 µm

2.0

1.6

 

250 µm

2.5

2.0

 

320 µm

3.2

2.6

 

530 µm

5.3

4.2

These flow rates at normal temperature and pressure (25°C and 1 atm) are recommended for all column temperatures.
For capillary columns, flow rates are proportional to column diameter and are 20% lower for helium than for hydrogen.

 

 

 

...




6890GC Messages




Message

Description/Cause

Troubleshooting

Not Ready

"Not Ready" LED lights (a component of the GC is not ready to begin a run)

  • Press Status key for explanation
  • Check for leaks in gas lines
  • Check gas supply delivery pressure
  • Check that oven, inlet, and detector temperatures are not too far apart

Method Mismatch

A loaded method contains parameters that do not match the GC's current configuration

  • If the parameter is set from the keyboard, method will overwrite current parameter and display a message that the parameter has been replaced
  • If the parameter depends on hardware, the method will be ignored and the current setpoints will remain. A message will indicate the method parameter is being ignored.

Follow ChemStation instructions
After method update, open Method parameter to check new setting; edit method if needed

Warning

A serious problem exists.

  • GC will not stop or prevent a run
  • GC emits 1 beep and displays warning message
  • Warning appears at run start
  • Warning is not recorded in run log

Press Status key to view explanation

Shutdown

Shutdown occurs/numbered error message is displayed

Pop-up message briefly explains the nature of the problem

Faults

Hardware problem requires user intervention

  • GC emits no beep or a single beep
  • Ready LED does not light
  • Error message appears

Press Status button for more information

Bad Main Board & Fatal Errors

Main board has malfunctioned; must be replaced

See



Bad Mainboard/Fatal Error Messages


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Common Chromatography Problems




Problem

Cause

Troubleshooting

No peaks on chromatogram

Acquisition aborted

Confirm the method is correct

 

Bad cable or connection

Check cables between GC and PC, detectors and GC

 

Leak in sample line

  • Purge test injectors and detectors
  • Check sample loop and columns for leaks

 

FID flame out

See FID flame out/will not light

 

TCD filament break

Measure TCD filament resistance (~10 ohm)

 

Column break

Check column installation

Retention times inconsistent

Column flow has changed

  • Check for leaks at inlet, liner, column connections
  • Check carrier gas supply pressure
  • Check column installation
  • Check method

 

FID jet contaminated

Remove jet and clean

 

Injector port temperature wrong

Check method

 

Oven temp program changed

Check method

 

Column overload

Inject less sample

Extra peaks on chromatogram

Contamination in system

  • Clean sample loops and injector port with solvent
  • Check gas trap indicators and expiration dates
  • Verify carrier/detector gas purity
  • Check gas supply tubing and fittings
  • Click Start on the control panel of GC without injection to confirm column contamination

 

Contaminated syringe

  • Clean syringe and vials with solvent
  • Click Start on the control panel of GC without injection, then inject laboratory air

Noisy baseline/random spiking

Leaks

  • Check for leaks at column fittings

 

Contamination

  • Verify purity of carrier/detector gases
  • Inspect the jet for contamination
  • Verify column has been conditioned

 

Electrical problem

  • Column is installed too high in detector
  • Electronic interference in laboratory

...




Common Hardware Problems




Problem

Cause

Troubleshooting

FID flame out/will not light

Detector gas flow incorrect

  • Check that gas lines are open
  • Check the gas system for leaks
  • Check air/hydrogen flow rates/mix
  • Check column flow rate
  • Check column/detector fitting for leaks

 

FID temperature too low

Wait 15–20 min for conditioning
Press Front Detector on the GC control panel and light the flame manually

FID flame out/will not light

Bad igniter

Remove heater/sensor assembly from the FID and measure resistance of heater and sensor. Replace ignitor if resistance is too high or too low:

  • Heater resistance = ~22 ohm
  • Sensor resistance = ~109 ohm

 

Jet dirty or partially plugged

Remove jet and clean

 

Flame will not stay lit

Check dessicant state in the hydrogen generator

Oven cannot attain or maintain setpoint temperature

  • Oven flaps
  • Oven fan
  • Oven heater
  • Oven temperature sensor

Contact service representative

 

 

 

 

 

 

 

 

 

...

Bad Mainboard/Fatal Error Messages




Message

Comment

Main FPGA Failure

Contact vendor representative

Static RAM Failure

 

Boot ROM Checksum

 

ROM #2 or #3 Checksum

EEPROM 2 or 3 malfunction

Incorrect ROM #2 or #3

EEPROM 2 or 3 installed in wrong position

ROM #2 or #3 wrong version

EEPROM 2 or 3 does not match other EEPROMs

DMA FPGA Failure

Contact vendor representative

DRAM Failure

 

Exception Vector

 

Bus Error

 

Address Error

 

Illegal Instruction

 

Divide by Zero

 

No 512Hz Interrupt

 

...




Shutdown Messages




Message number

Message

Explanation/Troubleshooting

1

Oven shut off

  • Oven flap malfunction
  • Thermal leaks (missing insulation)
  • Excessive oven load
  • Heater electronics malfunction

2

Oven cryo shutdown

Timeout

3, 5

Inlet pressure shutdown

Inlet does not reach setpoint

4, 6

Inlet flow shutdown

 

5, 8

Front detector fuel gas shutdown

Gas unable to reach/maintain setpoint in time allowed

6, 9

Front detector air/ref shutdown

 

7, 10

Front detector makeup shutdown

 

8, 9, 10

Pres aux shutdown

Pneumatics aux module cannot maintain setpoint

9

Multiposition valve not switching

  • Valve disconnected
  • Valve stuck
  • Switching time too short

10

Can't reach setpoint of multiposition valve

  • Valve position incorrect
  • Invert BCD setpoint incorrect

11, 12

Inlet cryo shutdown

Timeout

12, 14

Aux cryo shutdown

 

13, 14

Inlet heating too slowly

  • Temperature sensor failure
  • Zone heater defective

...




...

Warning Messages




Message number

Message

Explanation/Troubleshooting

100

Oven sensor missing

 

101, 102

Invalid heater power

Invalid heater power for front detector, inlet, or aux 1 or 2

103, 104

Signal buffer full

  • PC network down
  • PC cable disconnected
  • PC turned off
  • PC entered power saver mode
  • PC data collection stopped
  • GC hardware problem

105

Analog out data loss

Possible data loss

106

Signal data loss

 

107, 108

Detector config changed

Correct method to match hardware

109, 110

Inlet config changed

 

111, 112

Column config changed

 

113, 114, 115

Aux method changed

 

116

Log overflow

Capacity = 50 entries

117, 118

Inlet calibration deleted

Returned to default calibration

119, 120

Detector calibration deleted

 

121

Aux calib deleted

 

122

Comm data overrun

Possible data loss

123

Comm data error

 

124

Comm abnormal break

Check connection

125

Sampler data overrun

Possible data loss

126

Sampler data error

 

127

Sampler abnormal break

Check connection

128, 129

Inlet flow calibration fail

Contact vendor representative

130, 131

Aux cryo disabled

Reconfigure cryo

132–137

Sampling end problem

Setpoint conflicts with sampling end time parameter

...




Fault Messages




Message number

Message

Comments

200, 201

Faulty pneumatics board

 

202

Hydrogen shutdown

  • Check gas supply pressure
  • Check for leaks
  • Check for broken column
  • Check for stuck valve stuck

203–207

Signal DSP fault

 

208–211

Out signal path test failed


212, 213

Detector electrometer out of spec


214, 215

Detector flame out

  • Check hydrogen/air flow rates
  • Check for leaks at detector/column fitting
  • Check jet

216–219

TCD filament open or shorted

  • Check wire connections
  • Check cell temperature sensor
  • Replace TCD cell

220, 221

Thermal shutdown

  • Check electrical supply to GC
  • Check zone control electronics
  • Possible shorted temperature sensor
  • Possible shorted heater

222–224

Oven temperature fault

 

225–228

Detector temperature fault

 

229–232

Inlet temperature fault

 

233–236

Aux temperature fault

 

237, 238

Line interrupt fault

 

239, 240

Mux ADC thermal shutdown

 

241

Invalid line sense

 

242–244

Pneu aux module invalid constants

 

245–249

Obsolete EEPROM

 

250–254

Wrong module

 

255–258

Invalid module

 

259, 260

Detector module/board mismatch

 

261

MIO board defective

 

262, 264

RS232 defective

 

263

GPIB defective

 

265–269

Invalid pids

 

270–274

Invalid checksum

 

275–279

Invalid constants from factory calibration

 

280–284

I/O failure

 

285, 286

Detector offset adjustment failed

 

...