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目的对尿中砷的原子荧光光谱测定法进行样品不同前处理方法的比较以及标准曲线和工作曲线的比较。简化分析程序,使得该法更易推广普及。方法配制两套相同浓度的砷标准系列进行消化与不消化的比较,将两组数据进行统计处理,比较有无显著性差异;尿样采用硝酸高氯酸在自控电热器上消解,用加标回收率评价此消化方法测定的准确度。高、低两个浓度的样品各取6份消化测定,计算精密度,看其消化过程中的稳定性。结果尿砷标准系列消化与不消化没有显著性差异,尿样采用硝酸高氯酸在自控电热消化器上消化,高、低浓度的加标回收率分别为99.8%、104.3%。高、低浓度的样品精密度分别为6.3%、9.5%。结论该法的改进不影响方法的灵敏、准确和稳定性,且大大简化了操作程序,便于操作,减轻了分析人员的工作量,也减少了复杂程序可能带来的误差,使用更少的仪器设备,更利于推广、普及。
OBJECTIVE To compare the different pre-treatment methods of samples with the determination of arsenic in urine by atomic fluorescence spectrometry, and to compare the standard curve with the working curve. Simplify the analysis process, making it easier to promote the law. Methods Two sets of standard series of arsenic at the same concentration were prepared for comparison of digestion and non-digestion. The two groups of data were statistically analyzed for comparison with or without significant difference. Urinary samples were digested with nitric acid perchloric acid on self-controlled electric heaters, Recoveries The accuracy of this digestion method was evaluated. High and low concentrations of the samples taken six digestion, calculate the precision, to see the stability of the digestive process. Results There was no significant difference in digestibility and indigestion of urine arsenic standard series. The urine sample was digested with nitric acid perchloric acid in self-controlled electrothermal digester. The recoveries of high and low concentrations were 99.8% and 104.3% respectively. High and low concentrations of sample precision were 6.3%, 9.5%. Conclusion The improvement of this method does not affect the sensitivity, accuracy and stability of the method, and greatly simplifies the operation procedures, easy to operate, reduce the workload of analysts, but also reduce the possible error of complex procedures, the use of fewer instruments Equipment, more conducive to the promotion and popularization.