Determination of Trace Arsenic in Smelting Wastewater by Spectrophotometric with Disulfoantipymethane
摘 要
建立了利用二硫代安替比林甲烷光度法测定铅冶炼废水中微量砷的分析方法。在1.8 mol·L-1硫酸介质中,砷与二硫代安替比林甲烷显色剂发生灵敏的显色反应,最大吸收波长为331 nm。考察了显色剂用量、显色反应时间、介质、酸度、不同价态砷对测定结果的影响。结果表明:使用4 cm的比色皿,As3+的质量浓度在0.04~0.6 mg·L-1内与其对应的吸光度之间呈线性关系,线性回归方程为y=1.063 x+0.001,相关系数为0.999 3,表观摩尔吸光系数为2.7×104L·mol-1·cm-1。按照标准加入法进行回收试验,测得回收率为97.0%~105%,相对标准偏差(n=5)为1.3%~2.6%,该方法用于测定铅冶炼废水中微量砷的结果满意。
Abstract
An analytical method for the determination of trace arsenic in lead smelting wastewater by spectrophotometric with disulfoantipymethane. In 1.8 mol·L-1 H2SO4 medium, arsenic reacts with disulfoantipylmethanesensitively with an absorption maximum at 331 nm. The effects of reaction conditions, such as the amount of color reagent, reaction time, reaction medium, acidity and different valence arsenicon the absorbency were investigated. The results showed that linear relationship was found in the range of 0.04-0.6 mg·L-1 As3+ in 10 mL solution using a 4 cm cuvette with the reagent blank as a reference, the linear regression equation was y=1.063 x+0.001, and the correlation coefficient was 0.999 3, the molar absorptivity was 2.7×104L·mol-1·cm-1. Test for recovery was made by standard addition method, giving values of recovery in the range of 97.0%-105%, and values of RSDs (n=5) ranged from 1.3% to 2.6%. The proposed method was applied to the determination of trace arsenic in smelting wastewater with satisfactory result.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202004014
所属栏目 工作简报
基金项目 河南省高等学校重点科研资助项目(16B150008);济源职业技术学院青年骨干教师资助项目
收稿日期 2019/7/31
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备注左国强,副教授,硕士,主要从事光谱分析研究与教学工作,guoqiangzuo@126.com
引用该论文: ZUO Guoqiang,ZHAO Yapeng,YANG Xue,JIN Shasha,SHANG Wenhong. Determination of Trace Arsenic in Smelting Wastewater by Spectrophotometric with Disulfoantipymethane[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(4): 454~458
左国强,赵亚鹏,杨学,晋沙沙,尚文红. 二硫代安替比林甲烷光度法测定铅冶炼废水中的微量砷[J]. 理化检验-化学分册, 2020, 56(4): 454~458
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【3】邢凤晶,陆君,崔巍,等.氢化物发生及冷蒸汽-原子吸收分光光度法测定金银花中砷和汞的含量[J].中国卫生产业, 2016,13(23):104-106.
【4】ZHOU J, DENG D Y, SU Y Y, et al. Determination of total inorganic arsenic in water samples by cadmium ion assisted photochemical vapor generation-atomic fluorescence spectrometry[J]. Microchemical Journal, 2019,146:359-365.
【5】倪润祥,雒昆利.湿消解-原子荧光法测定煤中硒和砷[J].光谱学与光谱分析, 2015,35(5):1404-1408.
【6】修凤凤,樊勇,李俊雨.氢化物发生-原子荧光光谱法测定地球化学样品中的锗[J].中国无机分析化学, 2017,7(2):31-33.
【7】肖亚兵,郑文杰,许泓,等.纳米二氧化钛富集-银盐光度法检测痕量As3+和As5+[J].中国食品卫生杂志, 2005,17(2):154-157.
【8】马丽.电感耦合等离子体原子发射光谱(ICP-AES)法测定锡精矿中8种杂质元素[J].中国无机分析化学, 2016,6(3):39-42.
【9】程浦海,宋才炽.氢化物发生-电感耦合等离子体发射光谱法测定土壤中的微量砷[J].环境化学, 1988,7(6):24-28.
【10】MARCUS M, SIMON L, PHILIPP B, et al. iCAP TQ ICP-MS准确测定环境样品中的砷和硒[J].环境化学, 2017,36(12):2742-2744.
【11】陈婉如,潘教麦,黎平.用二硫代安替比林甲烷(DTPM)分光光度测定微量砷[J].分析化学, 1984,12(5):410-412.
【12】严恒泰,陈婉如,潘教麦.二硫代安替比林甲烷(DTPM)测定炭钢及生铁中砷[J].冶金分析与测试(冶金分析分册), 1985,5(6):10-13.
【13】张振宇,周青,邓明镇.用二硫代安替比林甲烷分光光度法测定尿中砷[J].职业医学, 1986,13(6):52-52.
【14】李在均,王利平,潘教麦.二硫代安替比林甲烷光度法检测化妆品中砷的研究[J].日用化学工业, 2000,30(4):48-49.
【15】REDMAN A D, MACALADY D L, AHMANN D. Natural organic matter affects arsenic speciation and sorption onto hematite[J]. Environmental Science and Technology, 2002,36(13):2889-2896.
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