I need advice on the necessary adjustments to make for methanol detection after I have made a TCD-FID series connection
I need advice on the necessary adjustments to make for methanol detection after I have made a TCD-FID series connection
Hi obedboakye,
If this was a working method before the series connection, there is really not much to change on the inlet or GC oven. Basically the non destructive detector output (TCD) will go to the FID. Depending on flows, you may no longer need make up gas and may need to make some changes to the FID gases. It would help if you shared the method parameters at this point and we can make suggestions.
Regards
James
Thank you James for the reply
Below is the full method components
Method Information
Method: C:\CHEM32\1\DATA\TEST\OBED#2.M
Modified: 30/12/2019 at 1:03:56 PM
Method Audit Trail
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Run Time Checklist
Pre-Run Cmd/Macro: off
Data Acquisition: on
Standard Data Analysis: on
Customized Data Analysis: off
Save GLP Data: off
Post-Run Cmd/Macro: off
Save Method with Data: off
Injection Source and Location
Injection Source: Manual
Injection Location: Dual
=============================================================================
6890 GC METHOD
=============================================================================
OVEN
Initial temp: 80 'C (On) Maximum temp: 250 'C
Initial time: 15.00 min Equilibration time: 0.50 min
Ramps:
# Rate Final temp Final time
1 0.0(Off)
Post temp: 60 'C
Post time: 0.00 min
Run time: 15.00 min
FRONT INLET (SPLIT/SPLITLESS) BACK INLET (SIM DIST)
Mode: Split Flow: 25.2 mL/min (On)
Initial temp: 50 'C (Off) Gas type: Helium
Pressure: 13.70 psi (Off)
Total flow: 5.6 mL/min
Gas saver: Off
Gas type: Helium
COLUMN 1 COLUMN 2
Capillary Column Packed Column
Model Number: Agilent 19091J-413 Model Number: Altech Haysep/ MS
HP-5 5% Phenyl Methyl Siloxane Haysep A / MS 5A
Max temperature: 325 'C Max temperature: 190 'C
Nominal length: 30.0 m Mode: (see column 1)
Nominal diameter: 320.00 um Nominal initial flow: 22.7 mL/min
Nominal film thickness: 0.25 um Inlet: Back Inlet
Mode: constant flow Outlet: Back Detector
Initial flow: 2.5 mL/min Outlet pressure: ambient
Nominal init pressure: 12.77 psi
Average velocity: 42 cm/sec
Inlet: Back Inlet
Outlet: Back Detector
Outlet pressure: ambient
FRONT DETECTOR (FID) BACK DETECTOR (TCD)
Temperature: 250 'C (On) Temperature: 250 'C (On)
Hydrogen flow: 40.0 mL/min (On) Reference flow: 45.0 mL/min (On)
Air flow: 450.0 mL/min (On) Mode: Constant makeup flow
Mode: Constant makeup flow Makeup flow: 0.0 mL/min (Off)
Makeup flow: 25.0 mL/min (Off) Makeup Gas Type: Helium
Makeup Gas Type: Helium Filament: On
Flame: On Negative polarity: Off
Electrometer: On
Lit offset: 2.0
SIGNAL 1 SIGNAL 2
Data rate: 20 Hz Data rate: 20 Hz
Type: front detector Type: back detector
Save Data: On Save Data: On
Zero: 0.0 (Off) Zero: 0.0 (Off)
Range: 0 Range: 0
Fast Peaks: Off Fast Peaks: Off
Attenuation: 0 Attenuation: 0
COLUMN COMP 1 COLUMN COMP 2
Derive from front detector Derive from back detector
THERMAL AUX 1
Use: Valve Box Heater
Description: Thermal Aux # 1
Initial temp: 100 'C (On)
Initial time: 0.00 min
# Rate Final temp Final time
1 0.0(Off)
VALVES POST RUN
Valve 1 Switching Off Post Time: 0.00 min
Description: MS Column Isolation
Valve 2 Switching Off
Description: Gas Sampling Valve
Valve 3 Off
Description:
TIME TABLE
Time Specifier Parameter & Setpoint
0.01 Valve 2: On
0.50 Valve 2: Off
GC Injector
Front Injector:
No parameters specified
Back Injector:
No parameters specified
========================================================================
Integration Events
========================================================================
------------------------------------------------------------------------
Non signal specific Integration Events
------------------------------------------------------------------------
Event Value
|--------------------------------------------------------|-------------|
Tangent Skim Mode Standard
Tail Peak Skim Height Ratio 0.000
Front Peak Skim Height Ratio 0.000
Skim Valley Ratio 20.000
Baseline Correction Classical
Peak to Valley Ratio 500.000
------------------------------------------------------------------------
Default Integration Event Table "Event"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 1.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.700 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_TCD"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 100.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_ADC"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 20.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FID"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_ECD"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 100.000 Initial
Initial Peak Width 0.080 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_NPD"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 500.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FPD"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_uECD"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 500.000 Initial
Initial Peak Width 0.080 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.000 Initial
Initial Shoulders OFF Initial
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_TCD2B"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 4.743 Initial
Initial Peak Width 0.037 Initial
Initial Area Reject 4.946 Initial
Initial Height Reject 1.108 Initial
Initial Shoulders OFF Initial
Negative Peak ON 2.350
Negative Peak OFF 2.625
Integration ON 7.400
Integration ON 7.800
Apply Manual Integration Events: No
=====================================================================
Calibration Table
=====================================================================
Calib. Data Modified : 06/09/2015 5:12:03 PM
Rel. Reference Window : 5.000 %
Abs. Reference Window : 0.000 min
Rel. Non-ref. Window : 5.000 %
Abs. Non-ref. Window : 0.000 min
Uncalibrated Peaks : not reported
Partial Calibration : Yes, identified peaks are recalibrated
Correct All Ret. Times: No, only for identified peaks
Curve Type : Linear
Origin : Included
Weight : Equal
Recalibration Settings:
Average Response : Average all calibrations
Average Retention Time: Floating Average New 75%
Calibration Report Options :
Printout of recalibrations within a sequence:
Calibration Table after Recalibration
Normal Report after Recalibration
If the sequence is done with bracketing:
Results of first cycle (ending previous bracket)
Signal 1: TCD2 B,
RetTime Lvl Amount Area Amt/Area Ref Grp Name
[min] Sig [ng/ul]
-------|--|--|----------|----------|----------|---|--|---------------
2.450 1 1 5.00000 223.00000 2.24215e-2 H2
2 10.80000 483.47903 2.23381e-2
3 40.00000 2847.00000 1.40499e-2
4 100.00000 8432.00000 1.18596e-2
2.710 1 1 2.00000 4339.62331 4.60869e-4 CO2
2 40.00000 8.16319e4 4.90005e-4
4.027 1 1 1.14000 2522.00537 4.52021e-4 C2H6
7.572 1 1 2.00000e-1 371.78349 5.37947e-4 O2
8.100 1 4 20.00000 4.00141e4 4.99824e-4 N2
1 50.86000 1.03355e5 4.92092e-4
2 60.00000 1.30000e5 4.61538e-4
3 95.00000 1.95000e5 4.87179e-4
9.350 1 1 10.00000 1.71026e4 5.84707e-4 CH4
2 40.00000 6.19067e4 6.46134e-4
10.200 1 1 25.00000 5.23675e4 4.77395e-4 CO
=====================================================================
Peak Sum Table
=====================================================================
***No Entries in table***
=====================================================================
========================================================================
Sample related custom fields
========================================================================
Custom Field Type Mand. Default Value
------------------------------------------------------------------------
None defined
========================================================================
Compound related custom fields
========================================================================
Custom Field Type Mand. Default Value
------------------------------------------------------------------------
None defined
No. We are using the back inlet so the front inlet is off
On Thu., Jan. 2, 2020, 3:08 p.m. james_jenkins, <agilent-x@jiveon.com>
No. We are using the back inlet so the front inlet is off
On Thu., Jan. 2, 2020, 3:08 p.m. james_jenkins, <agilent-x@jiveon.com>
