论文部分内容阅读
针对野外现场分析的要求,选择了微珠比色、微量滴定和蛋膜富集比色三项技术,拟定了30个痕量(或次量、主量)元素的40个分析方法;对方法的准确性、精密度、灵敏度等参数与公认可靠方法进行了对比,或采用标准物质分析进行验证;在方法拟定过程中特别注意了快速方便、降低环境污染、降低成本和提高方法的可操作性。这些方法对实验环境条件要求不高,满足野外现场分析应用。微珠比色法测铜以浴铜灵为显色剂,可不经分离测出各种样品中痕量铜,摩尔吸光系数1×104L·mol-1·cm-1,检出限为5ng,加标回收率为95%～105%,RSD(n=20)为2.2%。微珠比色法测铁以向红菲口罗啉为显色剂,铜干扰测定,可加入Na2S2O3掩蔽,摩尔吸光系数为1×105L·mol-1·cm-1,RSD(n=21)为3.4%,方法适用于测定0.001μg/g以上的Fe,测试结果与其它方法相吻合。微珠比色法测锌以吡啶偶氮萘酚为显色剂,一般矿样、水样、生物样品可直接测定,Cd、Ni、Cu等金属元素含量高时,可利用DDTC-CHCl3小体积萃取法分离锌,检出限1ng,RSD(n=20)为6.9%,用于铅锌矿等国家一级标准物质中锌的测定,结果与标准值相符。
For field analysis, we selected three techniques of microbead colorimetric, microtitration and egg white membrane enrichment and colorimetry, and developed 40 analytical methods for 30 trace (or minor and major) elements. Accuracy, precision, sensitivity and other parameters compared with the recognized reliable methods, or the use of standard material analysis to verify; in the process of formulating special attention to the rapid and convenient, reduce environmental pollution, reduce costs and improve the operability of the method . These methods do not require high experimental environmental conditions to meet the field application field analysis. Microbeads colorimetric method for the determination of copper bronze Ling as a color reagent can be measured without separation of trace amounts of copper in various samples, the molar absorption coefficient of 1 × 104L · mol-1 · cm-1, the detection limit of 5ng, Spiked recoveries ranged from 95% to 105% with RSD (n = 20) of 2.2%. Microbeads colorimetric method to ferulopalin for the color reagent, copper interference determination, can be added Na2S2O3 masking, molar extinction coefficient of 1 × 105L · mol-1 · cm-1, RSD (n = 21) Is 3.4%, the method is suitable for the determination of 0.001μg / g or more of Fe, the test results are consistent with other methods. Microbeads zinc colorimetry zinc pyridine naphthol as color reagent, the general mineral samples, water samples, biological samples can be directly measured, Cd, Ni, Cu and other metal elements when the content can be used DDTC-CHCl3 small volume The extraction method was used to separate zinc with the detection limit of 1 ng and the RSD (n = 20) of 6.9%. The method was applied to the determination of zinc in national first-grade lead-zinc mine and other raw materials. The results were consistent with the standard values.