Cold trapping of volatile organic compounds on fused silica capillary columns

Pankow, James F.

doi:10.1002/jhrc.1240060602

Cited by 26 publications

(11 citation statements)

References 18 publications

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“…They were obtained with WCC at -80, -70, and -6OOC. As observed earlier by Pankow [21] in non-P&T experiments with a 0.25 pm film thickness DB-5 column (J&W Scientific), trapping at -80°C on this type of film thickness…”

Section: Analyte Transfer As a Function Of Desorption Timesupporting

confidence: 56%

“…As employed elsewhere [21], to determine the effects of the WCC temperature on the quantitative efficiency of the trapping, the peakareas of the ions in Figure 4 were ratioed to the mlz = 112 ion peak area for chlorobenzene which appeared later in the chromatograms. Being much less volatile than the Figure 4 compounds, chlorobenzene can be expected to have exhibited quantitative trapping at all three WCC temperatures.…”

Section: Analyte Transfer As a Function Of Desorption Timementioning

confidence: 99%

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Effects of trapping temperature and film thickness in purge and trap with whole column cryotrapping on fused silica columns

Pankow

1986

J. High Resol. Chromatogr.

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SummaryThe effects of trapping temperature and column film thickness were investigated with respect to their ability to promote effective cryofocusing on fused silica capillary columns. The study was a further development of the purge and trap with whole column cryotrapping (P&T/WCC) method. The rates at which compounds could be thermally desorbed from a P&T unit and transferred to a column (with zero split) were first examined. A near quantitative transfer of the desorbable analytes was obtained with a 4 min, 18OoC, 20 mL/min desorption. The compounds tested included naphthalene. Columns with film thicknesses from 0.1 2 to 3.0 pm were then investigated in P&T/ WCC analyses with WCC temperatures ranging from -80 to OOC. Thetrapping tookplacefrom a transfer linegas stream initially at 175OC. The volatilities of the compounds examined varied from that of 1,l -dichloroetheneto 111,2,2-tetrachloroethane. A higher film thickness was found to ease the WCC temperature requirements. Within each column type, the warmest WCC temperatures which allowed good cryotrapping with no significant increases in peak width were: 0.25 pm, -7OOC; 1.0 pm, -5OOC; 3.0 pm, -2OOC. In addition to being quantitative, the trapping provided good chromatography.

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Section: Analyte Transfer As a Function Of Desorption Timesupporting

confidence: 56%

Section: Analyte Transfer As a Function Of Desorption Timementioning

confidence: 99%

Effects of trapping temperature and film thickness in purge and trap with whole column cryotrapping on fused silica columns

Pankow

1986

J. High Resol. Chromatogr.

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“…The thermal desorption process is kinetically slow but when packed columns at low temperatures were used very few problems (2) desorb into a section or loop of capillary tubing cooled to liquid nitrogen temperatures (see Figure 8.29(B)); (3) desorb into a short length of the analytical column or retention gap at cryogenic temperatures; (4) desorb into a cryogenically cooled packed capillary precolumn (used for the quantitative recovery of the most volatile analytes); or (5) desorb into the analytical column with whole column cold trapping [354,384,[410][411][412][413][414]. The use of cold trapping allows the desorbed sample to be refocused and the full resolving power of the open tubular column to be maintained.…”

Section: Semivolatile Organic Compounds In Airmentioning

confidence: 99%

Sample Preparation for Chromatographic Analysis

Poole

1991

Chromatography Today

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“…Cryofocusing of the analyte can also be performed in the inlet of the capillary column [2][3][4][5].…”

Section: Introductionmentioning

confidence: 99%

Matrix effect in the cryotrapping of gas samples in the ppbv range

2000

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SummaryA gas mixture containing ppbv concentrations of volatile chlorinated and aromatic hydrocarbons was prepared in helium, nitrogen, or argon in a plastic (Nalophan) bag, in which it was found the mixture could be safely stored for several days. Samples of the mixture were subsequently analyzed by gas chromatography after direct cryotrapping in an empty metal U-tube. The cooling medium used was liquid nitrogen, liquid argon, or a dry ice acetone slurry (197 K). The efficiency of cryotrapping in liquid nitrogen was over 90 % when the aromatic hydrocarbon mixture was prepared in the helium matrix, but between 50 and 70 % when it was prepared in nitrogen or argon, the recovery from the argon matrix being somewhat higher. The poor recovery in nitrogen at 77 K and argon at 87 K was explained by the reduced rate of diffusion to the wall owing to mist or aerosol formation. At 197 K condensation was negligible if the partial pressures were lower than the saturated vapor pressures.

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Cold trapping of volatile organic compounds on fused silica capillary columns

Cited by 26 publications

References 18 publications

Effects of trapping temperature and film thickness in purge and trap with whole column cryotrapping on fused silica columns

Effects of trapping temperature and film thickness in purge and trap with whole column cryotrapping on fused silica columns

Sample Preparation for Chromatographic Analysis

Matrix effect in the cryotrapping of gas samples in the ppbv range

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