Novel calibration technique for headspace analysis of semivolatile compounds

Dindal, Amy; Yu, Cheng; Skeen, J.T.; Jenkins, Roger A.

doi:10.1016/s0021-9673(97)00925-4

Cited by 3 publications

(3 citation statements)

References 10 publications

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“…Three SG sorption tubes were randomly selected from the batch of 10 tubes, described above, and tested. Each tube to be tested was spiked with an analyte mixture, using a validated method, and then thermally desorbed as described above. Thermal desorption recoveries were determined relative to liquid injections of the same quantity of analyte.…”

Section: Resultsmentioning

confidence: 99%

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Performance Evaluation of an In-Injection Port Thermal Desorption/Gas Chromatographic/Negative Ion Chemical Ionization Mass Spectrometric Method for Trace Explosive Vapor Analysis

Sigman

Ilgner

2001

Anal. Chem.

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A gas chromatographic method utilizing thermal desorption of Tenax TA and sol-gel sorbent traps has been developed and validated for the analysis of trace explosive vapor with negative ion chemical ionization mass spectrometric detection. Sorbent tubes were packed with Tenax TA and sorbent particles prepared in-house by the sol-gel process. Thermal desorption was performed within a split/splitless injection port with minimal instrument modification. Performance was characterized by relative thermal desorption recovery, precision (reproducibility), linearity of the calibration, and method detection limits. Method validation was performed with a series of dinitrotoluenes, dinitrobenzene, trinitrotoluene, trinitrobenzene, two aminodinitrotoluenes, three nitroesters, and two nitramines. The performance of Tenax TA and the sol-gel sorbents is evaluated based on the method validation data. The method was applied to the analysis of trace explosive vapor collected and concentrated with sol-gel solid sorbent traps from the headspace of a smokeless gunpowder sample.

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Section: Resultsmentioning

confidence: 99%

“…Sorbent Tube Loading with Calibration Standards. Each explosive standards mix was prepared as a solution in benzene and spiked onto SG traps using a validated method . The trap was attached to the base of a preheated (170 °C) injection port with the split vent closed.…”

Section: Methodsmentioning

confidence: 99%

Performance Evaluation of an In-Injection Port Thermal Desorption/Gas Chromatographic/Negative Ion Chemical Ionization Mass Spectrometric Method for Trace Explosive Vapor Analysis

Sigman

Ilgner

2001

Anal. Chem.

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“…Tenax traps were analyzed by reconfiguring the injection port of a gas chromatograph for thermal desorption, similar in configuration to those reported previously by our laboratory. [5][6] The analyses were performed on a Varian 3400 gas chromatograph with a nitrogen-phosphorus detector. The carrier gas, which originally flowed into the injection port, was redirected to the top of the desorption unit to serve as the desorption purge flow.…”

Section: Instrumental Conditionsmentioning

confidence: 99%

Determination of cocaine and heroin vapor pressures using commercial and illicit samples

Dindal

Buchanan

Jenkins

et al. 2000

Analyst

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The establishment of drug vapor pressure reference values provides valuable information in the development of vapor sensing devices for drug detection. The purpose of this work was to determine equilibrium headspace vapor pressures for commercial and illicit drug samples for use in such applications. Samples of cocaine, both free base and hydrochloride forms, and heroin hydrochloride were evaluated. The procedure used to measure the vapor pressures was a modification of a previously published method. Vapor pressure values at 20 degrees C previously reported for cocaine free base range from 0.37 x 10(-7) to 1.20 x 10(-7) Torr. The vapor pressure value determined in this study was 2.96 x 10(-7) Torr. It is likely that the discrepancies are due to differences in experimental conditions, varying sources of samples, and uncertainty in the methodologies. When the values were compared for commercial (99% purity) and illicit (unknown purity) sources of cocaine free base, there were no statistical differences in the projected room temperature (20 degrees C) vapor pressure values. However, the commercial and illicit samples of cocaine hydrochloride did show statistical differences. Although no comparison was made with the vapor pressure values for a pure, commercial sample, the vapor pressures of heroin hydrochloride (81% purity) at various temperatures were determined using the method developed for cocaine and are reported in this paper.

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