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Yang X.J.,Environmental Forensic and Analytical Science Section | Yang X.J.,Beijing University of Chemical Technology | Wan P.,Beijing University of Chemical Technology | Foley R.,Environmental Forensic and Analytical Science Section
Clean - Soil, Air, Water | Year: 2012

Inductively coupled plasma atomic emission spectrometry and inductively coupled plasma MS are the major analytical tools for trace elements in environmental matrices, however, the underestimate of certain trace elements in analysis of air particulate matter by these two techniques has long been observed. This has been attributed to incomplete sample digestion. Here, we demonstrate that the combined effects of sample digestion, air filter impurities, and post-adsorption of the analytes contribute to the interference of the analysis. Particular attention should be paid to post-adsorption of analytes onto air filters after acid digestion. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gray M.J.,Environmental Forensic and Analytical Science Section | Jahani S.,Environmental Forensic and Analytical Science Section | Low G.K.-C.,Environmental Forensic and Analytical Science Section
Journal of Chromatography A | Year: 2012

This paper explores the changes in the electrospray signal response of 39 structurally different compounds caused by the quality of the methanol, when used as a component in a gradient elution mobile phase. When three batches of LC-MS grade methanol from one manufacturer were evaluated, the largest variation in the electrospray signal responses of the 39 compounds examined was 18%. However, significant enhancement of the electrospray signals of up to 106% were observed among different brands of LC-MS grade methanol from different manufacturers. The effect of methanol quality on signal response was found to be compound dependent. This study also demonstrated that the senescence of the methanol was important. Using an expired batch of LC-MS grade methanol, electrospray signals were suppressed by as much as 95% for all compounds measured using positive mode electrospray. Conversely, the negative mode electrospray signals of compounds such as 4-octyl benzoic acid showed an enhancement of up to 96% when using the same batch of methanol. Linuron was used as a model compound to examine the change in the electrospray response, during gradient elution, when the proportion of an expired batch of methanol was varied. An infusion experiment showed that the linuron signal intensity decreased as the proportion of expired methanol increased in the mobile phase, which was in direct contrast to the increase in linuron signal observed with a non-expired batch of methanol. A series of isocratic experiments also showed that the linuron signal decreased as the proportion of expired methanol increased in the mobile phase. The ion ratios of several of the compounds studied changed significantly when using the expired batch of LC-MS methanol. The change in the ion ratios accentuates the difficulty of identifying compounds from in-source spectral libraries. A protocol is recommended for assessing the quality of methanol for LC-MS applications. © 2011.

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