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Highly Sensitive Determination of Butyl Xanthate in Surface and Drinking Water by Headspace Gas Chromatography with Electron Capture Detector

机译:顶空气相色谱-电子捕获检测器高灵敏测定表面和饮用水中的黄原酸丁酯

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摘要

A highly sensitive and convenient method for the determination of butyl xanthate in surface water and drinking water was developed by headspace gas chromatography with electron capture detector (HS-GC-ECD). The analytical method was based on the decomposition of butyl xanthate under an acidic condition, generating carbon disulfide, which could be sensitively detected by gas chromatography with electron capture detector. The signal of CS2 from the decomposition of potassium butyl xanthate was directly proportional to the concentration of potassium butyl xanthate over the range 0.7-100 ng/mL. The detection limit at a signal-to-noise ratio of three (S/N = 3) for potassium butyl xanthate was 0.3 ng/mL (similar to 1.6 x 10(-9) mol/L), which was more than two orders of magnitude lower than the popular UV methods and close to one order of magnitude lower than the similar headspace gas chromatography-mass spectroscopy method. The relative standard deviation (R.S.D.) within a day and in 3 days for potassium butyl xanthate at both 5 and 50 ng/mL was less than 4.7 %, suggesting good analytical performance of the present method. Good recoveries from 93.3 to 104.7 % were obtained from spiked surface and drinking water samples, indicating that the proposed HS-GC-ECD method was applicable for the quantification of butyl xanthate in surface and drinking water. Compared with other reported methods, the present method is highly sensitive, without sample preparation, and easily extended to the analysis of other xanthates.
机译:通过顶空气相色谱-电子捕获检测器(HS-GC-ECD)建立了一种高灵敏,简便的测定地表水和饮用水中黄原酸丁酯的方法。该分析方法基于黄原酸丁酯在酸性条件下的分解,生成二硫化碳,该二硫化碳可以通过电子捕获检测器的气相色谱法灵敏地检测出来。丁基黄药酸钾分解产生的CS2信号与范围在0.7-100 ng / mL的丁基黄药酸钾浓度成正比。丁基黄药钾在信噪比为3(S / N = 3)时的检出限为0.3 ng / mL(类似于1.6 x 10(-9)mol / L),超过两个数量级比常见的紫外光谱法的测量值低一个数量级,比类似的顶空气相色谱-质谱法的测量值低一个数量级。丁基黄药酸钾在5 ng / mL和50 ng / mL的情况下,在一天之内和3天内的相对标准偏差(R.S.D.)均小于4.7%,表明本方法具有良好的分析性能。从加标的地表水和饮用水样品中回收率从93.3%到104.7%,表明所提出的HS-GC-ECD方法可用于定量地表水和饮用水中的黄原酸丁酯。与其他已报道的方法相比,本方法灵敏度高,无需样品制备,并且易于扩展到其他黄药的分析。

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