A simple method for concentrating dilute high-boiling samples for capillary gas chromatography

Novotný, Miloš V.; Farlow, Raleigh

doi:10.1016/s0021-9673(00)83795-4

Cited by 38 publications

(19 citation statements)

References 28 publications

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“…Prior to gas chromatography, 0.15 ml of methylene chloride was added to each sample and a 5-pl aliquot transferred onto a precolumn (7) consisting of 2 mg of a specially deactivated solid support packed into a 1-mm. i.d.…”

Section: Methodsmentioning

confidence: 99%

Profiles of the polynuclear aromatic fraction from engine oils obtained by capillary-column gas-liquid chromatography and nitrogen-selective detection

Lee¹,

Bartle²,

Novotný³

1975

Anal. Chem.

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TiOY2-solutions may then be stored for a long time (over a month) without any special care.Current efficiency for electrolytic generation of Ti(II1) may be evaluated by the Lingane Method ( 1 1 ) from the current density potential graphs plotted in Figures 2 and 3 for platinum and mercury electrodes, respectively. A very good current efficiency (>0.996) is obtained with the mercury electrode throughout the current density region available with our apparatus (Figure 4, curve a ) but with the platinum it is never as good (Figure 4, curve b ) and falls down sharply when the current density is high, because of competition of hydrogen ion reduction.Titration Efficiency. The homogenous reoxidation of electrogenerated Ti(II1) to Ti(1V) by a variety of organic or inorganic oxidants is very fast and quantitative. It is therefore possible to carry out a series of coulometric titrations with the same Ti(1V) electrolytic solution in the same vessel.For example, we report here experimental results on the titration of samples of aromatic nitroso compounds (Table 11) performed successively in the same electrolytic solution.Titration efficiency is better than 99% for all the compounds but the last. The lack of purity of the products available probably accounts for these results.Application of these results to selective coulometric titrations of organic compounds are presented elsewhere (22, 23). LITERATURE CITED(1) J.

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Section: Methodsmentioning

confidence: 99%

Profiles of the polynuclear aromatic fraction from engine oils obtained by capillary-column gas-liquid chromatography and nitrogen-selective detection

Lee¹,

Bartle²,

Novotný³

1975

Anal. Chem.

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“…The bias may have been caused by a slight drift in the MS tune. In contrast to the work [24] with steroids where considerable attention to deactivating the precolumn packing material was required, the only precaution taken in this workwas the use of silanized glass wool. The fact that this less rigorous approach proved acceptable for the PCBs and PBBs may be due to the chemical inertness of these compounds.…”

Section: Desorption Ease and Efficiency With Glass Wool/ Tenax-ta Carmentioning

confidence: 99%

“…Heating transfers the analytes to the column. Precolumns of uncoated packing [23], coated packing [23,24], Chromosorb 101 [26], and Tenax-TA [27] have been used. The advantages of highly deactivated, coated packings have been discussed [24] for steroids; Tenax-GC has been found to be unsuitable for use with such compounds [24].…”

Section: Introductionmentioning

confidence: 99%

“…As has been noted [24], with SRTD: 1) a large fraction of the extract can be placed on the precolumn and desorbed to the column, thereby improving sensitivity; 2) chromatographic complications caused by the injection of large amounts of solvent are avoided; 3) low volatility materials present in the extract that might damage the column tend to remain in the precolumn; and 4) the volumes of extract that are injected are relatively large, thereby increasing precision.…”

Section: Introductionmentioning

confidence: 99%

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Solvent removal/thermal desorption (SRTD) for extract concentration and capillary column injection

Hart¹,

Pankow²

1987

J. High Resol. Chromatogr.

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SummaryMany solvent extracts must be concentrated prior to analysis. Both Kuderna-Danish (K-D) concentration and inert gas blowdown are commonly used. Significant losses often occur with the latter. Solvent removaVthermal desorption (SRTD) on a precolumn was investigated here as an alternative or supplement to these methods. The compounds studied included polychlorinated biphenyls (PCBs) and polybrominated biphenyls (PBBs).SRTD wascarriedout by injecting 100pLofextractintoa cartridge-type precolumn, selectively volatilizing the solvent with a stream of carrier gas, then thermally desorbing the analytes to a fused silica capillary gas chromatography (GC) column. The mean total recoveries and mean standard errors obtained were 109 and t 12%, respectively. SRTD was found to give sharper peaks than were obtainable with on-column injection. Method detection limits accessible for PCBs by capillary GC with electron impact mass spectrometry with the assistance of SRTD were estimated. Overall, SRTD was found to be an effective, rapid, high recovery concentration method for solvent extracts.

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“…Almost all analyses of head space gases are started this way. In addition, cold trapping is an essential step in more specific techniques, -E 20- such as the falling needle method [12], injection onto precolumns [13] …”

Section: Cold Trappingmentioning

confidence: 99%

Splitless injection and the solvent effect

Grob

1978

J. High Resol. Chromatogr.

199

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SummarySplitless injection is based on the solvent effect as a mechanism condensing large vapour clouds down to infinitely shortened bands. The effect is controlled by the parameters column temperature, volatility and amount of solvent, and rate of injection. By properly selecting the variables the effect can easily be optimized for any combination of sample and column. It is the purpose of this paper to provide the mechanistic understanding as required for this optimization, as well as some rules for the experimental realization. Potentialities and limitations of splitless injection are discussed, and the role of the solvent effect in on-column injection is emphasized.

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A simple method for concentrating dilute high-boiling samples for capillary gas chromatography

Cited by 38 publications

References 28 publications

Profiles of the polynuclear aromatic fraction from engine oils obtained by capillary-column gas-liquid chromatography and nitrogen-selective detection

Profiles of the polynuclear aromatic fraction from engine oils obtained by capillary-column gas-liquid chromatography and nitrogen-selective detection

Solvent removal/thermal desorption (SRTD) for extract concentration and capillary column injection

Splitless injection and the solvent effect

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