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在氢化物原子荧光分析中,发现当锑含量高于砷250倍时砷的测定结果明显偏高。另外,大量锑污染仪器管道致使清洗十分困难,从而引起严重的记忆效应。本文采取苯萃取砷(Ⅲ)分离大量锑,然后将砷(Ⅲ)反洗入水相,调节测定液酸度为20％盐酸介质,用氢化物原子荧光法测定砷、该方法避免了大量锑的干扰,同时也解决了锑污染仪器管道等问题。主要仪器和试剂 WYD-2型双道氢化物无色散原子荧光分析仪(江苏宝应无线电厂生产);激发光源:砷无极灯(北京电光源研究所出品);砷标准溶液1μg/mL,20％盐酸介质;碘化钾洗液:2mL 85％KI与98mL HCl(3+1)混合硼氢化钾溶液:1％(微碱性),现用现配。
In the hydride atomic fluorescence analysis, it was found that the determination of arsenic was significantly higher when the content of antimony was 250 times higher than that of arsenic. In addition, a large number of antimony contaminated instrumentation pipes make cleaning very difficult, causing serious memory effects. In this paper, arsenic (Ⅲ) is used to separate a large amount of antimony, and then arsenic (Ⅲ) is backwashed into the aqueous phase. The acidity of the test solution is adjusted to 20% hydrochloric acid. The determination of arsenic by hydride generation atomic fluorescence spectrometry , But also solve the problem of antimony pollution instrument pipeline. The main instrument and reagent WYD-2 type two-channel hydrideless atomic fluorescence spectrometer (Jiangsu Baoying radio factory production); excitation light source: arsenic lamp (produced by Beijing Institute of Light Sources); arsenic standard solution 1μg / mL, 20% Hydrochloric acid medium; potassium iodide lotion: 2mL 85% KI mixed with 98mL HCl (3 + 1) potassium borohydride solution: 1% (slightly alkaline)