College of Marine Science, University of South Florida, St. Petersburg, FL 33701, United States.
J Hazard Mater. 2012 Jun 15;219-220:247-52. doi: 10.1016/j.jhazmat.2012.04.001. Epub 2012 Apr 7.
Determination of chromate at low concentration levels in drinking water is an important analytical objective for both human health and environmental science. Here we report the use of solid phase extraction (SPE) in combination with a custom-made portable light-emitting diode (LED) spectrophotometer to achieve detection of chromate in the field at nanomolar levels. The measurement chemistry is based on a highly selective reaction between 1,5-diphenylcarbazide (DPC) and chromate under acidic conditions. The Cr-DPC complex formed in the reaction can be extracted on a commercial C18 SPE cartridge. Concentrated Cr-DPC is subsequently eluted with methanol and detected by spectrophotometry. Optimization of analytical conditions involved investigation of reagent compositions and concentrations, eluent type, flow rate (sample loading), sample volume, and stability of the SPE cartridge. Under optimized conditions, detection limits are on the order of 3 nM. Only 50 mL of sample is required for an analysis, and total analysis time is around 10 min. The targeted analytical range of 0-500 nM can be easily extended by changing the sample volume. Compared to previous SPE-based spectrophotometric methods, this analytical procedure offers the benefits of improved sensitivity, reduced sample consumption, shorter analysis time, greater operational convenience, and lower cost.
测定饮用水中低浓度的铬酸盐对于人类健康和环境科学都是非常重要的分析目标。在这里,我们报告了固相萃取(SPE)与定制的便携式发光二极管(LED)分光光度计结合使用,在现场实现纳米级别的铬酸盐检测。测量化学基于酸性条件下 1,5-二苯卡巴肼(DPC)与铬酸盐之间的高选择性反应。在反应中形成的 Cr-DPC 络合物可以在商业 C18 SPE 小柱上被萃取。浓缩的 Cr-DPC 随后用甲醇洗脱并用分光光度法检测。分析条件的优化包括对试剂组成和浓度、洗脱液类型、流速(样品加载)、样品体积以及 SPE 小柱稳定性的研究。在优化条件下,检测限约为 3 nM。仅需 50 毫升的样品即可进行分析,总分析时间约为 10 分钟。通过改变样品体积,可以轻松扩展目标分析范围 0-500 nM。与以前基于 SPE 的分光光度法相比,该分析方法具有提高的灵敏度、减少样品消耗、更短的分析时间、更大的操作便利性和更低的成本的优势。