Catalytic Polarographic Determination of Micro-amount of Arsenic in Complex Materials with Separation by Distillation
摘 要
提出了用催化极谱法测定复杂物料中微量砷的含量。选择测定的溶液介质中含碲(Ⅳ)硫酸溶液5 mL和150 g·L-1碘化钾溶液5 mL。仪器扫描速率为250 mV·s-1,并采用二阶导数测定。试样(0.01~1.0 g)用氯酸钾0.5 g、氢氟酸5滴、硝酸5~10 mL溶解,用蒸馏法分离其中的砷。砷的质量浓度在0.4 mg·L-1以内与相应的峰电流呈线性关系。按此方法测定了12个矿样中砷含量,其测定值与已知值相符。方法的回收率在97%~100%之间,相对标准偏差(n=6)在2.3%~7.2%之间。
Abstract
It was reported that micro-amount of arsenic in complex materials were determined by catalytic polarography in testing solution containing 5 mL of Te(Ⅳ)-H2SO4 solution and 5 mL of 150 g·L-1 of KI solution. Anodic scanning at the rate of 250 mV·s-1 and 2nd derivative of the measured polarographic wave were adopted in the determination. The sample (0.01-1.0 g) was dissolved in KClO3 (0.5 g), HF (5 drops) and HNO3 (5-10 mL), and As ion was separated by distillation. Linear relationship between values of peak current and mass concentration of As was obtained in the range within 0.4 mg·L-1. Twelve samples of ores were analyzed by the proposed method for their arsenic contents, giving results consistent with the known values. Values of recovery and RSD′s (n=6) found were in the ranges of 97%-100% and 2.3%-7.2%.
中图分类号 O657.14
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收稿日期 2011/12/7
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备注龙萍(1963-),女,云南开远人,教授级高级工程师,主要从事冶金分析与研究工作。
引用该论文: LONG Ping,WU Jian,MAO Yu-ping. Catalytic Polarographic Determination of Micro-amount of Arsenic in Complex Materials with Separation by Distillation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(2): 201~203
龙萍,吴鉴,毛禹平. 蒸馏-催化极谱法测定复杂物料中微量砷[J]. 理化检验-化学分册, 2012, 48(2): 201~203
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参考文献
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【2】高小霞.极谱催化波[M].北京:北京科学出版社, 1991:529-533.
【3】汪尔康,奚治文,刘立尧.示波极谱及应用[M].成都:四川科学技术出版社, 1984:227-228.
【4】龙萍,熊恒,蒋文龙,等.极谱法快速测定铜浮渣中常量砷[J].云南冶金, 2010,39(5):78-80.
【5】毛禹平,石安全.示波极谱法快速测定金属锑中的微量砷[J].分析试验室, 2001,11(5):78-80.
【6】李国童,齐玉.极谱催化波法测定食品中痕量砷[J].齐齐哈尔师范学院学报:自然科学版, 1994,14(2):34-36.
【7】张树朝.极谱催化波法测定纯铝中的微量砷[J].轻金属, 1998,17(2):44-46.
【8】王志婷,陈小燕.催化极谱法测定饮用水中的砷[J].中国卫生检验杂志, 2001,11(5):582-582.
【9】王建琴,梁云生.示波极谱法测定铁矿石中微量砷[J].岩矿测试, 2002,21(3):236-237.
【10】梁云生,毛禹平,朱煜.催化极谱法快速测定高锗物料中的微量砷[J].冶金分析, 2003,23(4):41-42.
【11】张家惠,张永寿.干灰化-催化极谱法测定化妆品中的铅和砷[J].环境与健康杂志, 1992,9(2):84-85.
【12】李婉义.测定生物材料中痕量砷的催化极谱法[J].华中理工大学学报, 1989,17(1):133-136.
【13】范丽汇,毛禹平.示波极谱法快速测定金属铜中微量砷[J].理化检验-化学分册, 2000,36(11):508-509.
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