Speciation analysis by gas chromatography with plasma source spectrometric detection

International audienceState-of-the-art species-selective analysis by gas chromatography (GC) with plasma source spectrometric detection is discussed for organometal and organometalloid compounds. Various plasmas, inductively coupled plasma, microwave induced plasma, capacitatively coupled plasma, direct current plasma and alternating current plasma, are characterized and critically compared as sources of radiation for atomic emission spectrometry and sources of ions for mass spectrometry. Interfaces between gas chromatography (packed, wide-bore, capillary and multicapillary) and plasma source spectrometry are characterized. Particular emphasis is given to applications of GC with plasma source detection to real-world analytical problems, which are comprehensively reviewed. The use of plasmas for the acquisition of auxiliary molecular information such as empirical formulae and structural information is discussed. Recent developments relating to sample preparation and presentation to the hyphenated system are addressed. The most significant trends in speciation analysis are highlighted. © 1997 Elsevier Science B.V

Sensitive speciation analysis of lead in environmental waters by capillary gas chromatography microwave-induced plasma atomic emission spectrometry

International audienceOptimization of microwave-induced plasma atomic emission detection for the speciation of organolead compounds in water samples is described. The absolute detection limits achieved vary from 0.02 to 0.1 pg (as Pb) and are dependent on the volatility of the species determined. Two procedures for the separation and enrichment of organolead in water samples were evaluated. Ionic organolead species were extracted as their diethyldithiocarbamate complexes either with one portion of hexane at pH 8 or twice with pentane at pH 9, with preconcentration in the latter instance by rotary evaporation of the solvent. The detection limits obtained were down to 2 and 0.1 ng l-1, respectively for 100-ml samples. Propylation and butylation were compared for derivatization of organolead species in the extracts. Examples of results for rain and tap water analyses are given

Ultratrace speciation analysis of organolead in water by gas chromatography-atomic emission spectrometry after in-liner preconcentration

International audienceA rapid and sensitive method for the speciation of organolead compounds in water at the sub-ng dm-3 level by gas chromatography-atomic emission spectrometry was developed. Only 100 cm3 of the sample are sufficient for the analysis and no preconcentration step by evaporation is necessary prior to the injection of the sample solution into the system. Sample preparation involves extraction of dithiocarbamate complexes of ionic organolead species into hexane followed by their propylation using a Grignard reaction. A 25 mm3 volume of the derivatized extract is injected on to a Tenax-packed liner. Before rapid, linear heating of the liner, the solvent is purged away at room temperature by a stream of helium while the analytes are trapped on the sorbent. The organolead compounds are separated on a capillary column and detected by an atomic emission detector. A detection limit of 0.1 ng dm-3 (as Pb) can be obtained. The precision of the method is 5% at the 1 ng dm-3 level with 90% recovery. Examples of analyses of tap water and polar snow are shown

Speciation analysis of organotin in water and sediments by gas chromatography with optical spectrometric detection after extraction separation

International audienceThe state of the art of gas chromatography with atomic emission and atomic absorption spectrometric detection as a technique for speciation analysis of organotin in water samples and sediments is discussed. Extraction separation of ionic organotin compounds and their conversion to gas chromatographable species are reviewed. Recent advances in instrumentation with respect to sensitivity, selectivity and applicability to real sample analysis are highlighted. Particular emphasis is given to sources of error and accuracy of the data obtained

Determination of volatile sufur compounds in water samples, beer, coffee with purge and trap gas chromatography microwave induced plasma atomic emission spectrometry

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Determination of volatile sufur compounds in water samples, beer, coffee with purge and trap gas chromatography microwave induced plasma atomic emission spectrometry

International audienceA method for the determination of 13 volatile sulfur compounds including dimethyl sulfide, dimethyl disulfide (DMDS), carbon disulfide and other sulfides and thiols in water samples was developed. The analytes were stripped from the sample by a flow of helium and preconcentrated in a capillary cryogenic trap. This was followed by determination by gas chromatography-microwave-induced plasma atomic emission spectrometry. Detection limits ranged from 8 pg (0.4 ng l-1) for ethanethiol to 17 pg (0.9 ng l-1) for DMDS. The method was successfully applied to the quantitative analysis of fresh and sea water and after slight modifications also to different Belgian beer types and coffee powder. A system for the automated sample delivery was developed for liquid samples