Purging directly to a capillary column with whole column cryotrapping (P/WCC) for the determination of aqueous volatile compounds

Pankow, James F.

doi:10.1002/jhrc.1240100709

Cited by 21 publications

(4 citation statements)

References 7 publications

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“…On the other hand, V" ^50 mL never plugged this column. As discussed elsewhere (22), similar runs with Vg values of >100 mL carried out with an ice trap to eliminate plugging exhibited chromatography that was as good as those obtained here without an ice trap. Thus, if Vg values of the order of 100 mL are to be used with a 0.53 column, use of an ice trap is recommended.…”

Section: Resultssupporting

confidence: 80%

“…Although WCC is a very straightforward operation with GCs capable of subambient programming, an alternative to WCC for trapping the analytes involves the placement of a portion of the front of a narrow bore column in a zone maintained at liquid nitrogen temperatures during the P&T desorption step (11). This approach has recently been incorporated into an EPA P&T capillary GC method (22). The potential disadvantage in using this trapping method is that short, open tubular zones have not, in general, been found to be 100% effective in trapping volatile analytes (13)(14)(15).…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Determination of volatile compounds in water by purging directly to a capillary column with whole column cryotrapping

Pankow¹,

Rosen²

1988

Environ. Sci. Technol.

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Section: Resultssupporting

confidence: 80%

Section: Introductionmentioning

confidence: 99%

Determination of volatile compounds in water by purging directly to a capillary column with whole column cryotrapping

Pankow¹,

Rosen²

1988

Environ. Sci. Technol.

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“…Trapping can be done using a room-temperature sorbent trap, such as Tenax, − or a cold trap. ,, Sorbent traps often have long desorption times, on the order of 3 min, and can be subject to problems such as thermal degradation and memory effects …”

mentioning

confidence: 99%

High-Speed Gas Extraction of Volatile and Semivolatile Organic Compounds from Aqueous Samples

et al. 1998

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A device is described for high-speed gas extraction of volatile and semivolatile organic compounds from aqueous samples. High-speed extraction is achieved by the use of elevated temperatures. Large quantities of water vapor produced at elevated temperatures are managed with a reflux condenser, which efficiently removes water vapor without sample loss by returning the condensed water along with any cocondensed organic compounds to the extraction cell. The heated extraction cell uses a 1-2-mL sample with an extraction gas flow of typically 30 mL/ min. Extraction temperatures as high as 95 °C can be used while maintaining a dew point temperature of ∼5 °C for the extraction gas and sample vapor leaving the device. Extraction profiles are obtained by connecting the device directly to a flame ionization detector. Extraction profiles for benzene show that quantitative recovery can be achieved in ∼30 s at an extraction temperature of 90 °C. Large increases in recovery at higher extraction temperatures are also demonstrated for tridecane and ethyl alcohol. For analytical studies, the device is interfaced to a commercial cryofocusing inlet system for highspeed gas chromatography. If all the extraction gas is trapped and injected into the separation column, detection limits for volatile organic compounds typically are in the 50-200 parts-per-trillion range.The emergence of high-speed methods using gas chromatography (GC) 1-3 and mass spectrometry (MS) 4,5 for the analysis of volatile and semivolatile organic compounds holds promise for dramatic increases in sample throughput and reductions in analysis costs. However, many environmental samples require extraction and preconcentration prior to analysis. These procedures often require several minutes to several tens of minutes and seriously compromise the effectiveness of high-speed analysis methods. Gas extraction followed by adsorbent trapping (purge and trap) often is used for aqueous samples. Even with protracted extraction times, quantitative extraction may be difficult to achieve.Purge and trap or dynamic gas extraction was first described in 1962. 6 Dynamic gas extraction coupled to capillary GC was first described in 1974. 7 Today, it is commonly used for many applications including food, 8,9 water, 10 soil, 11 and biological fluid 12 analysis. There are several important limitations to dynamic gas extraction. To achieve low detection limits, large sample volumes and long purging times usually are used. Most procedures require 5-50 mL of sample. This can be a problem in some applications. Extraction times typically are in the 10-30-min range. This would significantly limit sample throughput when used with high-speed GC, high-speed GC/MS, or direct MS.Trapping can be done using a room-temperature sorbent trap, such as Tenax, [13][14][15] or a cold trap. 9,15,16 Sorbent traps often have long desorption times, on the order of 3 min, and can be subject to problems such as thermal degradation and memory effects. 15 Capillary cold traps are easily blocked by large amoun...

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“…Recently Pankow [7] and Pankow and Rosen [8] have removed the adsorbent trap from PTlWCC and purge directly onto a cryogeni-cally cooled capillarycolumn. In attempting to maximize simplicity of their method they have not incorporated a procedure for removal ofwater from the purge stream priorto its introduction to the GC column.…”

Section: Introductionmentioning

confidence: 99%

Selective water removal in purge/GC analysis of volatile aromatics in aqueous samples

Cochran

1987

J. High Resol. Chromatogr.

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Purging directly to a capillary column with whole column cryotrapping (P/WCC) for the determination of aqueous volatile compounds

Cited by 21 publications

References 7 publications

Determination of volatile compounds in water by purging directly to a capillary column with whole column cryotrapping

Determination of volatile compounds in water by purging directly to a capillary column with whole column cryotrapping

High-Speed Gas Extraction of Volatile and Semivolatile Organic Compounds from Aqueous Samples

Selective water removal in purge/GC analysis of volatile aromatics in aqueous samples

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