Bulut Volkan Numan, Ozdes Duygu, Bekircan Olcay, Gundogdu Ali, Duran Celal, Soylak Mustafa
Department of Chemistry, Karadeniz Technical University, Faculty of Arts & Sciences, 61080 Trabzon, Turkey.
Anal Chim Acta. 2009 Jan 19;632(1):35-41. doi: 10.1016/j.aca.2008.10.073. Epub 2008 Nov 6.
A new, simple, rapid and sensitive separation, preconcentration and speciation procedure for chromium in environmental liquid and solid samples has been established. The present speciation procedure for Cr(III) and Cr(VI) is based on combination of carrier element-free coprecipitation (CEFC) and flame atomic absorption spectrometric (FAAS) determinations. In this method a newly synthesized organic coprecipitant, 5-chloro-3-[4-(trifluoromethoxy) phenylimino]indolin-2-one (CFMEPI), was used without adding any carrier element for coprecipitation of chromium(III). After reduction of chromium(VI) by concentrated H(2)SO(4) and ethanol, the procedure was applied for the determination of total chromium. Chromium(VI) was calculated as the difference between the amount of total chromium and chromium(III). The optimum conditions for coprecipitation and speciation processes were investigated on several commonly tested experimental parameters, such as pH of the solution, amount of coprecipitant, sample volume, etc. No considerable interference was observed from the other investigated anions and cations, which may be found in natural water samples. The preconcentration factor was found to be 40. The detection limit for chromium(III) corresponding to three times the standard deviation of the blank (N=10) was found 0.7 microg L(-1). The present procedure was successfully applied for speciation of chromium in several liquid and solid environmental samples. In order to support the accuracy of the method, the certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) were analyzed, and standard APDC-MIBK liquid-liquid extraction method was performed. The results obtained were in good agreement with the certified values.
已建立一种用于环境液体和固体样品中铬的新型、简单、快速且灵敏的分离、预富集及形态分析方法。目前用于Cr(III)和Cr(VI)的形态分析方法基于无载体元素共沉淀(CEFC)与火焰原子吸收光谱法(FAAS)测定相结合。在此方法中,一种新合成的有机共沉淀剂5-氯-3-[4-(三氟甲氧基)苯基亚氨基]吲哚-2-酮(CFMEPI)被用于在不添加任何载体元素的情况下共沉淀铬(III)。在用浓硫酸和乙醇将铬(VI)还原后,该方法用于测定总铬。铬(VI)通过总铬量与铬(III)量的差值来计算。在几个常用的实验参数(如溶液pH值、共沉淀剂用量、样品体积等)上研究了共沉淀和形态分析过程的最佳条件。在天然水样中可能存在的其他被研究阴离子和阳离子未观察到明显干扰。预富集因子为40。铬(III)对应空白值三倍标准偏差(N = 10)的检出限为0.7 μg L⁻¹。该方法成功应用于多种液体和固体环境样品中铬的形态分析。为了验证该方法的准确性,分析了有证标准物质(CRM-TMDW-500饮用水和CRM-SA-C沙质土壤C),并采用标准APDC-MIBK液液萃取法。所得结果与认定值良好吻合。