Microwave-assisted digestion of organic samples: How simple can it become?

TALANTA

卷:98

Article

Nobrega, J. A.¹  Pirola, C.²  Fialho, L. L.¹  Rota, G.²  de Campos Jordao, C. E. K. M. A.³  Pollo, F.⁴ 

[1] Univ Fed Sao Carlos, Dept Quim, BR-13560970 Sao Carlos, SP, Brazil

[2] Milestone Srl, I-24010 Sorisole, BG, Italy

[3] Embrapa Pecuaria SE, BR-13560970 Sao Carlos, SP, Brazil

[4] Anacom Cient, BR-09892100 Sao Bernardo Do Campo, SP, Brazil

关键词: Microwave-assisted digestion;    Single reaction chamber;    Diluted nitric acid solutions;    Temperature of digestion;    Residual Carbon;    Residual Acidity;   

DOI  :  10.1016/j.talanta.2012.06.079

来源: Elsevier

【 摘 要 】

Advancements in sample preparation for performing trace analysis of inorganic analytes are coming from the dissemination of microwave-assisted procedures, but there is still room for improvements by looking for simple and easily applied procedures. Recently it was proposed a new approach called single reaction chamber with capability for digestions at high pressures and temperatures using simple vials and racks. This was a limitation of former cavity microwave ovens with closed vessels. It was demonstrated here that the use of single reaction chamber approach allows the implementation of efficient digestions using diluted solutions of nitric acid and also allows addressing a critical need of sample preparation for inorganic analysis by running mixed batches of samples. The feasibility of this procedure was demonstrated for organic samples and accuracy was proved by using certified reference materials of apple leaves, bovine liver and whole milk powder. Digestions performed of whole milk powder and bovine liver using 2.0 mol L-1 nitric acid solution plus concentrated hydrogen peroxide at 240 degrees C led to residual carbon contents of 0.825 and 1.50% and residual acidities of 1.04 and 0.618 mol L-1, respectively. These parameters are fully compatible with further measurements using ICP OES or ICP-MS. Al, Cu, Fe, Mn, Mo, Rb, Se, Sr, and Zn were accurately determined by ICP OES or ICP-MS depending on their concentrations in digests. (C) 2012 Elsevier B.V. All rights reserved.

【 授权许可】

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