-
- Posts: 12
- Joined: Mon Mar 31, 2014 2:10 pm
Analytes of interest: Methanol, Ethyl Ether, Ethylenediamine, Toluene, 2-Ethyl-2-Oxazoline (monomer)
Solvent: N,N-Dimethylacetamide
Method: Headspace Chromatography
Shimadzu GC-2010 Plus Gas Chromatograph
Flame Ionization Detector
Model: FID-2010
Split/Splitless Injector
Model: SPL-2010
Shimadzu AOC-5000 Plus Autosampler
Serial #: 270884 & 236074
10 or 20 mL Vial Tray – 32 Vial Capacity
Equipment #: 220-91300-02, Shimadzu
Agitator/Incubator
Equipment #: MH 01-00B, CTC Analytics AG Switzerland
Serial #: 13716
Syringe Kit
Equipment #: MSH 02-00B & MSK 02-00A
CTC Analytics AG GC Power Supply
Part #: MN 01-02, PAL
Restek Rtx-Volatile Amine Column
60 meter – Length
.32 mm – Inner Diameter
0 µm – df (film thickness)
290ºC – Max Prog. Temp., 270ºC – Min. Bleed Temp.
Cat #: 18078
Computer with GCSolution Software Version 2.41.00
Septa - Supelco, Sigma-Aldrich/20633
Glass Liner - Shimadzu/220-90784-00
Equipment and Method Settings
Gas Chromatograph Settings
Carrier Pressure: 23.7 psi
Carrier Gas: Helium
Oven Temperature: 40.0°C initial temperature, hold for 4 minutes, ramp at 5.0°C/minute to 200.0°C,hold for 8 minutes
Injector Temperature: 180.0°C
Injection Mode: Split
Flow Control Mode: Linear Velocity
Total Flow: 20.6 mL/min
Column Flow: 3.52 mL/min
Linear Velocity: 40.0 cm/sec
Purge Flow: 3.0 mL/min
Split Ratio: 4.0
Detector: Flame-Ion Detector (FID)
Hydrogen Flow: 40.0 mL/min
Air Flow: 400.0 mL/min
Makeup Gas Flow: 30.0 mL/min
Detector Temperature: 250.0°C
Sampling Rate (FID): 40 msec
Analysis Time: 44.00 minutes
Autosampler Settings
Sample Volume: 1.0 mL
Incubation Temp: 140.0°C
Incubation Time: 6.5 minutes
Agitation Speed: 250 rpm
Agitation On Time: 10s
Agitation Off Time: 2s
Syringe Temperature: 145.0°C
Fill Speed: 1ml/s
Fill Strokes: 3
Pullup Delay: 5.0 s
Inject to: GC Inj1
Inject Speed: 400µl/s
Pre Injection Delay: 100 ms
Post Injection Delay: 100 ms
Syringe Flushing: 30 minutes
Flush Gas: Nitrogen
GC Runtime: 50 minutes
Quantitative & Identification Parameters
Quantitative Method: Standard Addition
Calculated by: Area
Calibration Curve: Linear
Weight Regression: None
Calibration Level#: 6
Concentrations = 0, 40, 60, 80, 100, 120
Through Origin: Not through
Unit: ppm
Window/Band: Window
Default Band Time: ---
Peak Select: All Peaks
Correction RT: No Change
Window: 5%
Identification Method: Absolute
Grouping: None
Compound Approximate Retention Time (RT)
Methanol RT: 5.080 min
Diethyl Ether RT: 9.600 min
Ethylenediamine RT: 16.280 min
Toluene RT: 22.650 min
2-Ethyl-2-Oxazoline RT: 24.430 min
N,N-Dimethylacetamide RT: 26.100 min