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采用Chromosorb 108固相萃取法对环境样品中的铬形态进行分析。

Chromium speciation in environmental samples by solid phase extraction on Chromosorb 108.

作者信息

Tuzen Mustafa, Soylak Mustafa

机构信息

Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat, Turkey.

出版信息

J Hazard Mater. 2006 Feb 28;129(1-3):266-73. doi: 10.1016/j.jhazmat.2005.08.046. Epub 2005 Oct 19.

DOI:10.1016/j.jhazmat.2005.08.046
PMID:16236441
Abstract

In the present work, a solid phase extraction system has been proposed for speciation of Cr(III) and Cr(VI) in the real samples. The procedure based on the adsorption of chromium(III) as dithizonate chelate on the Chromosorb 108 resin. After reduction of Cr(VI) by concentrated H2SO4 and ethanol, the system was applied to the total chromium. Cr(VI) was calculated as the difference between the total Cr content and the Cr(III) content. The influences of the analytical parameters including pH of the aqueous solution, amounts of dithizone, eluent type, sample volume and flow rates of the sample and eluent solution were investigated. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The adsorption capacity of sorbent was 4.50 mg/g Cr(III). The detection limit of Cr(III) is 0.75 microg/L. The proposed method was applied to the speciation of chromium in environmental samples including natural waters and total chromium preconcentration in microwave digested Turkish tobacco, coffee and soil samples with satisfactory results. In order to verify the accuracy of the method, two certified reference materials (NIST SRM 1573a Tomato Leaves and RTC-CRM 025-050 Metals on Soil) were analyzed and the results obtained were in good agreement with the certified values. The relative errors and relative standard deviations were below 5% and 9%, respectively.

摘要

在本工作中,提出了一种用于实际样品中Cr(III)和Cr(VI)形态分析的固相萃取系统。该方法基于铬(III)作为双硫腙螯合物吸附在Chromosorb 108树脂上。用浓硫酸和乙醇将Cr(VI)还原后,该系统用于测定总铬。Cr(VI)通过总铬含量与Cr(III)含量之差计算得出。研究了分析参数的影响,包括水溶液的pH值、双硫腙的用量、洗脱剂类型、样品体积以及样品和洗脱剂溶液的流速。在铬形态分析中,未观察到其他所研究的阴离子和阳离子有明显干扰。吸附剂对Cr(III)的吸附容量为4.50 mg/g。Cr(III)的检测限为0.75 μg/L。所提出的方法应用于环境样品中铬的形态分析,包括天然水,以及微波消解的土耳其烟草、咖啡和土壤样品中总铬的预富集,结果令人满意。为了验证该方法的准确性,分析了两种有证标准物质(NIST SRM 1573a番茄叶和RTC-CRM 025-050土壤中的金属),所得结果与认证值吻合良好。相对误差和相对标准偏差分别低于5%和9%。

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