Optimization of Methodology for Determination of Inorganic Chromium Species in Sewage Sludge Samples by HPLC-ICP-MS/MS

Journal of the Brazilian Chemical Society

article

Barbosa, Érica S.¹  Cacique, Ane P.¹  Pinho, Gevany P. de¹  Silvério, Flaviano O.¹ 

[1] Instituto de Ciências Agrárias, Universidade Federal de Minas Gerais

关键词: sewage sludge;    chromium;    extraction;    reduction;    inorganic chromium species;   

DOI  :  10.21577/0103-5053.20200124

学科分类：内科医学

来源: SciELO

【 摘 要 】

This study developed a methodology for extracting and speciating Cr III and Cr VI in sewage sludge by high performance liquid chromatography, inductively coupled plasma tandem mass spectrometry (HPLC-ICP-MS/MS). The optimal procedure was solid-liquid extraction in a water bath with stirring at 50 °C for 16 h and 50 mmol L −1 ethylenediaminetetraacetic acid (EDTA) extraction phase at pH 9.5. In the validated method, the recovery in the fortification experiment was greater than 70% and the relative standard deviation was less than 7%. Speciation analyses showed that all Cr VI was spontaneously reduced to Cr III in the sludge sample. The limits of detection and quantification were 0.060 and 0.20 µg L −1 , respectively, and the analyses of Cr III by means of ICP-MS/MS were linear from 0.20 to 50 µg L −1 . The extraction efficiency of Cr specie in this validated method improved from 4.09 to 53.3% compared to the EPA 1311 method. The methodology was successfully applied to quantify Cr III in a sludge sample with a lower concentration than that established by European legislation 80568/4225/91.

【 授权许可】

CC BY