Overview:
A highly reproducible in-vial standard gas generating system was developed and validated for eventual application in quality control and standardization of GC-MS instrumentation.
- Vials prepared with a silicone oil/XAD-4 based sorbent proved to better retain the standard and were hence decided as the ideal choice for further vial development
- Validation was performed on both GC-MS and GC-FID instrumentation using a modified McReynolds mixture
- Vials were tested for intra/inter-batch reproducibility, storage stability, and depletion rate
- Similar PFPH, PFBB, NEM, n-alkanes, carboxylic acids, aldehydes and BTEX, based vials have been produced
Inter-vial reproducibility of McReynolds standard gas generating vials when 1-minute extractions were performed at 35oC with a DVB/PDMS fiber
Compounds
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Benzene
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2-Pentanone
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1-Nitropropane
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Pyridine
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1-Pentanol
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Octane
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Fvial
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0.85
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0.28
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0.30
|
0.72
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0.11
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0.29
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Fcrit
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3.11
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% RSD
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3.4
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3.5
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3.3
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3.8
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3.7
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3.4
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ANOVA verified that vials prepared from different batches of spiked pump oil were statistically identical at a 95% level of confidence
Vial Validation: Analyte depletion after multiple headspace extractions
Vial Validation: Analyte depletion after multiple headspace extractions
Demonstration of less than 3.3% depletion for all analytes after 208 consecutive extractions were performed for 1 minute at 35 C using a DVB/CAR/PDMS fiber
References:
1: J.J. Grandy, G.A. Gómez-Ríos, J. Pawliszyn, G.A. Gomez-Rios, J. Pawliszyn, Development of a standard gas generating vial comprised of a silicon oil–polystyrene/divinylbenzene composite sorbent, J. Chromatogr. A. 1410 (2015) 1–8. doi:10.1016/j.chroma.