固相萃取用于监测职业接触Cr(III)。

Analytical Chemistry Insights Pub Date : 2007-12-11
S J Shahtaheri, M Khadem, F Golbabaei, A Rahimi-Froushani
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引用次数: 0

摘要

铬是一种重要成分,广泛用于生产各种合成材料的不同工业过程。为了评估工人接触微量有毒金属Cr(III)的情况,环境和生物监测是必不可少的过程,其中样品的制备是分析前最耗时和最容易出错的方面之一。固相萃取(SPE)的使用越来越多,是一种丰富的样品制备技术,因为它比液-液萃取(LLE)产生的结果更好。根据样品pH、配体浓度、负载流速、洗脱溶剂、样品体积、洗脱体积、树脂量和样品基质干扰,优化了使用XAD-4树脂填充的迷你柱的SPE。铬保留在固体吸附剂上,并用2M HNO(3)洗脱,然后通过使用火焰原子吸收光谱法简单测定分析物。金属离子回收率达92%以上。优化的程序也用三个不同的加标尿液样本池进行了验证,并在连续六天和六天内的实验中显示出良好的再现性。通过本研究,获得了合适的相对标准偏差结果,因此,可以认为,该优化方法在简化不同基质中微量铬残留分析的样品制备以评估职业和环境暴露方面是成功的。为了评估职业性铬暴露,根据优化程序采集、制备和分析了16份尿液样本。
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Solid phase extraction for monitoring of occupational exposure to Cr (III).

Chromium is an important constituent widely used in different industrial processes for production of various synthetic materials. For evaluation of workers' exposure to trace toxic metal of Cr (III), environmental and biological monitoring are essential processes, in which, preparation of samples is one of the most time-consuming and error-prone aspects prior to analysis. The use of solid-phase extraction (SPE) has grown and is a fertile technique of sample preparation as it provides better results than those produced by liquid-liquid extraction (LLE). SPE using mini columns filled with XAD-4 resin was optimized regarding to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, amount of resins, and sample matrix interferences. Chromium was retained on solid sorbent and was eluted with 2 M HNO(3) followed by simple determination of analytes by using flame atomic absorption spectrometry. Obtained recoveries of metal ion were more than 92%. The optimized procedure was also validated with three different pools of spiked urine samples and showed a good reproducibility over six consecutive days as well as six within-day experiments. Through this study, suitable results were obtained for relative standard deviation, therefore, it is concluded that, this optimized method can be considered to be successful in simplifying sample preparation for trace residue analysis of Cr in different matrices for evaluation of occupational and environmental exposures. To evaluate occupational exposure to chromium, 16 urine samples were taken, prepared, and analyzed based on optimized procedure.

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