The Liquefaction of Oxygen and the Solidification of Carbon Disulphide and Alcohol

The flame ionisation detector response to C6-C11 aliphatic hydrocarbon solutions in carbon disulphide in the concentration range between 1.3-9.5 mg ml-1 retained lineary despite the excess of solvent entering the detector simultaneously with the analyte. Pure carbon disulphide exhibited a small positive detector response which did not interfere in calibration procedure and which, under certain GC conditions, inverted to negative values. This response was not proportional to the injected volume and was strongly influenced by the column temperature and/or bleed. On the basis of these findings, a method compatible with the widely used charcoal tube carbon disulphide desorption procedure was developed and evaluated. It consists of static desorption of the sum of aliphatic alkanes and cycloalkanes from the activated charcoal after which an internal standard is added to the supernatant eluate. The resulting carbon disulphide solution is analysed on a highly polar stationary phase 1,2,3-tris(2-cyanoethoxy)propane where the solvent and the analyte coelute in a single peak, the height of which is practically proportional to the sum of alkanes and cycloalkanes present. This also makes determinations of other substances present in the sample more simple. The field test of the proposed method yielded values comparable in precision and accuracy with a control infrared spectrophotometric method.

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Study on the precision of the activated charcoal solvent desorption procedure - Correlation of desorption efficiencies

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19811332 ◽

1981 ◽

Vol 46 (6) ◽

pp. 1332-1347 ◽

Cited By ~ 2

Author(s):

Martin Koval

Keyword(s):

Activated Charcoal ◽

Carbon Disulphide ◽

Internal Standard ◽

Standard Addition ◽

Published Data ◽

Single Factor ◽

Gas Chromatograph ◽

Model Compounds ◽

Single Factor Analysis ◽

Acceptable Agreement

The described method uses activated charcoal sampling tubes for air sampling. Adsorbed compounds are eluted by the static desorption procedure with 1 ml of carbon disulphide, 0.5 ml of the supernatant is filtered off and, after internal standard addition, analysed on a gas chromatograph. Using synthetic calibration mixtures of model organic compounds with air, cumulative sampling and desorption efficiencies for 24 substances were determined for concentration ranges and sample volumes according to current Czechoslovak hygienic standards. Experimental results were treated with the single factor analysis of variance and the precision of the described procedure was estimated for the studied model compounds on the basis of residual sums of squares. Calculated values of cumulative sampling and desorption efficiencies and their precisions were compared with available published data and an acceptable agreement was found. In addition to that, cumulative sampling and desorption efficiencies were also found to be significantly correlated to molar volumes and other related molecular properties for some types of compounds.

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