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目的建立尿中锡的原子荧光分光光度测定方法。方法取2.50 m L尿样加入1.50 m L浓硝酸后,用石墨消解仪消化,以体积分数为4.00%的盐酸溶液定容至10.00 m L,加入质量浓度为100 g/L的硫脲-抗坏血酸2.50 m L,以体积分数为4.00%的盐酸溶液定容至25.00 m L(相当于稀释尿样10倍)后,取1.00 m L样品采用原子荧光光度法进行测定。结果尿中锡在质量浓度为4.00~200.00μg/L范围内线性关系良好,相关系数为0.999 5;方法检出限为0.20μg/L,加标回收率为100.20%~100.84%,批内相对标准偏差(RSD)为0.11%~2.01%,批间RSD为1.37%~5.58%;样品在4℃条件下可保存7 d。结论本方法灵敏度高,准确性好,操作简便,适用于人尿中锡的日常监测。
Objective To establish a method for the determination of tin in urine by atomic fluorescence spectrometry. Methods 2.50 m L urine sample was added with 1.50 m L concentrated nitric acid and then digested with graphite digestion device. The volume content of 4.00% hydrochloric acid solution was fixed to 10.00 m L, and the concentration of thiourea-ascorbic acid 2.50 m L to a volume of 4.00% hydrochloric acid solution to 25.00 m L (equivalent to 10 times diluted urine samples), take 1.00 m L samples were determined by atomic fluorescence spectrometry. Results The urinary tin showed a good linearity in the range of 4.00-200.00 μg / L with a correlation coefficient of 0.999 5. The detection limit of the method was 0.20 μg / L, and the spiked recoveries ranged from 100.20% to 100.84% The standard deviation (RSD) ranged from 0.11% to 2.01%, and the inter-assay RSD ranged from 1.37% to 5.58%. The samples were stored at 4 ℃ for 7 days. Conclusion The method is sensitive, accurate and easy to operate. It is suitable for daily monitoring of tin in human urine.