Comment puis-je analyser les Tubes Getxent avec des appareils analytiques?
Les tubes Getxent peuvent être analysés sur des équipements analytiques. Les deux principaux sont :
- La chromatographie en phase gazeuse couplée à la spectrométrie de masse (GC-MS)
- La chromatographie en phase liquide couplée à la spectrométrie de masse (LC-MS)
GC-MS
Les tubes peuvent être analysés directement par GC-MS selon les méthodes suivantes :
- SPME (micro-extraction sur phase solide)
- Headspace (espace de tête)
Un exemple de méthode SPME est disponible ci-dessous.
LC-MS
L’analyse LC-MS des Tubes Getxent nécessite une extraction de leur contenu à l’aide de solvants. Nous recommandons les solvants suivants à température ambiante :
- Méthanol
- Diméthylformamide
- Acétone
- Iso-octane
- Solution d’acide sulfurique à 10 %
- Solution de soude caustique à 10 %
Méthode GC-MS splitless
Temps d’incubation : 25 minutes
Agitation : 250 rpm
Température d’incubation : 40 °C
No Sample Prep method has been assigned to this method.
=============================================================================
6890 GC METHOD
=============================================================================
OVEN
Initial temp: 40 'C (On) Maximum temp: 260 'C
Initial time: 1.00 min Equilibration time: 3.00 min
Ramps:
# Rate Final temp Final time
1 10.00 200 5.00
2 0.0(Off)
Post temp: 0 'C
Post time: 0.00 min
Run time: 22.00 min
FRONT INLET (SPLIT/SPLITLESS) BACK INLET (UNKNOWN)
Mode: Splitless
Initial temp: 250 'C (On)
Pressure: 16.00 psi (On)
Purge flow: 70.0 mL/min
Purge time: 3.00 min
Total flow: 73.8 mL/min
Gas saver: Off
Gas type: Helium
COLUMN 1 COLUMN 2
Capillary Column (not installed)
Model Number: SPME 1227062
DB WAX
Max temperature: 260 'C
Nominal length: 60.0 m
Nominal diameter: 250.00 um
Nominal film thickness: 0.25 um
Mode: constant flow
Initial flow: 1.0 mL/min
Nominal init pressure: 16.01 psi
Average velocity: 26 cm/sec
Inlet: Front Inlet
Outlet: MSD
Outlet pressure: vacuum
FRONT DETECTOR (NO DET) BACK DETECTOR (NO DET)
SIGNAL 1 SIGNAL 2
Data rate: 20 Hz Data rate: 20 Hz
Type: test plot Type: test plot
Save Data: Off Save Data: Off
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
(No Detectors Installed) (No Detectors Installed)
THERMAL AUX 2
Use: MSD Transfer Line Heater
Description:
Initial temp: 250 'C (On)
Initial time: 0.00 min
# Rate Final temp Final time
1 0.0(Off)
POST RUN
Post Time: 0.00 min
TIME TABLE
Time Specifier Parameter & Setpoint
GC Injector
Front Injector:
No parameters specified
Back Injector:
No parameters specified
Column 1 Inventory Number : AB002
Column 2 Inventory Number :
MS ACQUISITION PARAMETERS
General Information
------- -----------
Tune File : stune.u
Acquistion Mode : Scan
MS Information
-- -----------
Solvent Delay : 3.00 min
EMV Mode : Gain Factor
Gain Factor : 0.80
Resulting EM Voltage : 1094
[Scan Parameters]
Low Mass : 35.0
High Mass : 500.0
Threshold : 150
Sample # : 2 A/D Samples 4
Plot 2 low mass : 50.0
Plot 2 high mass : 550.0
[MSZones]
MS Source : 230 C maximum 250 C
MS Quad : 150 C maximum 200 C
END OF MS ACQUISITION PARAMETERS
TUNE PARAMETERS for SN: US10442350
-----------------------------
Trace Ion Detection is OFF.
EMISSION : 34.610
ENERGY : 69.922
REPELLER : 19.904
IONFOCUS : 74.973
ENTRANCE_LE : 0.000
EMVOLTS : 1058.824
Actual EMV : 1200
GAIN FACTOR : 1.72
AMUGAIN : 2027.000
AMUOFFSET : 127.000
FILAMENT : 1.000
DCPOLARITY : 0.000
ENTLENSOFFS : 17.067@ 3 17.067@ 50 14.557@ 69 17.820@131 15.310@219 17.067@414 17.067@502 17.067@799
MASSGAIN : -69.000
MASSOFFSET : -9.000
END OF TUNE PARAMETERS
------------------------------------
END OF INSTRUMENT CONTROL PARAMETERS
------------------------------------
COLUMN 1 COLUMN 2
Capillary Column (not installed)
Model Number: SPME 1227062
DB WAX
Max temperature: 260 'C
Nominal length: 60.0 m
Nominal diameter: 250.00 um
Nominal film thickness: 0.25 um
Mode: constant flow
Initial flow: 1.0 mL/min
Nominal init pressure: 16.05 psi
Average velocity: 26 cm/sec
Inlet: Front Inlet
Outlet: MSD
Outlet pressure: vacuum
FRONT DETECTOR (NO DET) BACK DETECTOR (NO DET)
SIGNAL 1 SIGNAL 2
Data rate: 20 Hz Data rate: 20 Hz
Type: test plot Type: test plot
Save Data: Off Save Data: Off
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
(No Detectors Installed) (No Detectors Installed)
THERMAL AUX 2
Use: MSD Transfer Line Heater
Description:
Initial temp: 220 'C (On)
Initial time: 0.00 min
# Rate Final temp Final time
1 0.0(Off)
POST RUN
Post Time: 0.00 min
TIME TABLE
Time Specifier Parameter & Setpoint
GC Injector
Front Injector:
No parameters specified
Back Injector:
No parameters specified
Column 1 Inventory Number : AB002
Column 2 Inventory Number :
MS ACQUISITION PARAMETERS
General Information
------- -----------
Tune File : atune.u
Acquistion Mode : Scan
MS Information
-- -----------
Solvent Delay : 3.00 min
EMV Mode : Gain Factor
Gain Factor : 10.00
Resulting EM Voltage : 1341
[Scan Parameters]
Low Mass : 35.0
High Mass : 500.0
Threshold : 150
Sample # : 2 A/D Samples 4
Plot 2 low mass : 50.0
Plot 2 high mass : 550.0
[MSZones]
MS Source : 230 C maximum 250 C
MS Quad : 150 C maximum 200 C
END OF MS ACQUISITION PARAMETERS
TUNE PARAMETERS for SN: US10442350
-----------------------------
Trace Ion Detection is OFF.
EMISSION : 34.610
ENERGY : 69.922
REPELLER : 32.468
IONFOCUS : 88.259
ENTRANCE_LE : 14.500
EMVOLTS : 952.941
Actual EMV : 952.941
GAIN FACTOR : 0.59
AMUGAIN : 2030.000
AMUOFFSET : 128.000
FILAMENT : 1.000
DCPOLARITY : 0.000
ENTLENSOFFS : 19.075
MASSGAIN : -76.000
MASSOFFSET : -8.000
END OF TUNE PARAMETERS
------------------------------------
END OF INSTRUMENT CONTROL PARAMETERS
------------------------------------
