Determinação de As em amostras orgânicas de interesse ambiental por espectrometria de absorção atômica com atomização eletrotérmica após combustão em bomba de O2

A microwave-induced combustion (MIC) procedure was applied for coal digestion for subsequent determination of As, Cd and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and Hg using cold vapor (CV) generation coupled to ICP-MS. Pellets of coal (500 mg) were combusted using 20 bar of oxygen and ammonium nitrate as aid for ignition. The use of nitric acid as absorbing solution (1.7, 3.5, 5.0, 7.0 and 14 mol L(-1)) was evaluated. For coal samples with higher ash content, better results were found using 7.0 mol L(-1) HNO(3) and an additional reflux step of 5 min after combustion step. For coal samples with ash content lower than 8%, 5.0 mol L(-1) nitric acid was suitable to the absorption of all analytes. Accuracy was evaluated using certified reference material (CRM) of coal and spikes. Agreement with certified values and recoveries was better than 95 and 97%, respectively, for all the analytes. For comparison of results, a procedure recommended by the American Society of Testing and Materials (ASTM) was used. Additionally, a conventional microwave-assisted digestion (MAD) in pressurized vessels was also performed. Using ASTM procedure, analyte losses were observed and a relatively long time was necessary for digestion (>6h). By comparison with MAD procedure, higher sample mass can be digested using MIC allowing better limits of detection. Additionally, the use of concentrated acids was not necessary that is an important aspect in order to obtain low blank levels and lower limits of detection, respectively. The residual carbon content in digests obtained by MAD and MIC was about 15% and <1%, respectively, showing the better digestion efficiency of MIC procedure. Using MIC it was possible to digest completely and simultaneously up to eight samples in only 25 min with relatively lower generation of laboratory effluents.

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An overview on analytical methods for quantitative determination of multi-element in coal samples

Mketo

Nomngongo

Ngila

2016

TrAC Trends in Analytical Chemistry

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Determinação de As em amostras orgânicas de interesse ambiental por espectrometria de absorção atômica com atomização eletrotérmica após combustão em bomba de O2

Cited by 5 publications

References 4 publications

Sample preparation techniques based on combustion reactions in closed vessels — A brief overview and recent applications

Sample preparation techniques based on combustion reactions in closed vessels — A brief overview and recent applications

Determination of toxic elements in coal by ICP-MS after digestion using microwave-induced combustion

An overview on analytical methods for quantitative determination of multi-element in coal samples

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