火焰原子吸收法测定酸洗废液中重金属的应用研究
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摘要
针对采用火焰原子吸收法直接测定酸洗废液中铬、镍、铅3种重金属数据准确性较差的问题,研究了酸洗废液重金属测定存在的干扰因素及采用标准加入法消除干扰的可行性。结果表明,若用火焰原子吸收法直接测定酸洗废液会受到来自基体的干扰,铬、镍、铅的回收率分别为54.0%、84.9%、89.5%,均出现了回收率不达标的情况。通过干扰试验可知,铬主要受到Fe~(2+)的化学干扰及溶液的物理干扰,镍和铅主要受溶液的物理干扰作用,均使测定结果偏低。镍、铅可直接采用标准加入法测定,R~2分别可达0.999 1、0.999 7,镍、铅的回收率分别为97.5%、101.5%;但对于铬,需先优化测定条件和加入干扰抑制剂后,才能采用标准加入法测定,此时铬的相对标准偏差为1.41%,回收率为104.9%。该测定方法精确度和准确度良好,可用于酸洗废液中重金属的测定。
In view of the poor accuracy of determination of heavy metals such as Cr,Ni and Pb in waste pickling acid by flame atomic absorption spectrophotometry directly,the interference factors in the determination of heavy metals in waste pickling acid and the feasibility of eliminating interference by standard addition method were studied in this paper.The results showed that the recovery rate of Cr,Ni and Pb were 54.0%,84.9% and 89.5%,respectively,if the waste pickling acid was directly determined by atomic absorption spectrophotometry.The recovery rate of Cr,Ni and Pb could not reach the standard.Through the interference test,it was known that Cr was mainly affected by the chemical interference of Fe~(2+) and physical interference of solution,Ni and Pb were mainly affected by physical interference of solution,resulting in the low determination results.Ni and Pb could be directly determined by standard additon method,R~2 were 0.999 1 and 0.999 7,respectively,and the recovery rate of Ni and Pb were 97.5% and 101.5%,repectively,but for Cr,the determination conditions should be optimized and interference inhibitors should be added.The relative standard deviation of Cr was 1.41%,and the recovery rate was 104.9%.The method was accurate and precise,and could be used for the determination of heavy metals in waste pickling acid.
In view of the poor accuracy of determination of heavy metals such as Cr,Ni and Pb in waste pickling acid by flame atomic absorption spectrophotometry directly,the interference factors in the determination of heavy metals in waste pickling acid and the feasibility of eliminating interference by standard addition method were studied in this paper.The results showed that the recovery rate of Cr,Ni and Pb were 54.0%,84.9% and 89.5%,respectively,if the waste pickling acid was directly determined by atomic absorption spectrophotometry.The recovery rate of Cr,Ni and Pb could not reach the standard.Through the interference test,it was known that Cr was mainly affected by the chemical interference of Fe~(2+) and physical interference of solution,Ni and Pb were mainly affected by physical interference of solution,resulting in the low determination results.Ni and Pb could be directly determined by standard additon method,R~2 were 0.999 1 and 0.999 7,respectively,and the recovery rate of Ni and Pb were 97.5% and 101.5%,repectively,but for Cr,the determination conditions should be optimized and interference inhibitors should be added.The relative standard deviation of Cr was 1.41%,and the recovery rate was 104.9%.The method was accurate and precise,and could be used for the determination of heavy metals in waste pickling acid.
引文
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[15]国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2002.
[16]鲁丹,陈海青.火焰原子吸收法测定水中总铬的影响因素探讨[J].中国公共卫生,2004,20(4):417-418.
[2]杜豪.铁系混凝剂的制备及在废水处理中的应用研究[D].青岛:青岛理工大学,2015.
[3]张文学.酸洗废液资源化:纳米四氧化三铁的制备及性能研究[D].哈尔滨:哈尔滨师范大学,2015.
[4]袁敏,武建超,于劲松,等.水中重金属检测方法的研究进展[J].应用化工,2015,44(4):724-728.
[5]杨军,李丽,周育香.火焰原子吸收测定中的背景吸收和基体干扰[J].油气田环境保护,1999,9(4):26-28.
[6]陈万明.重金属原子吸收分析中的干扰及消除[D].长沙:湖南农业大学,2005.
[7]王增焕,王许诺.萃取分离-原子吸收光谱法测定海水中镉铜铅锌铬镍[J].冶金分析,2014,34(2):44-47.
[8]彭彩红,张平,陈永亨,等.火焰原子吸收光谱法测定工业废水中铊、铅、镉时高盐分的干扰[J].理化检验:化学分册,2016,52(8):952-954.
[9]刘晓杰,王燕霞,于勇海.空气-乙炔火焰原子吸收光谱法测定钐钴永磁合金中钙量[J].冶金分析,2018,38(3):51-55.
[10]卢洁.标准加入法在仪器分析中的应用释疑[J].广西农业生物科学,2008,27(增刊1):100-103.
[11]张千强,黄惠珠.高基体对测定铜精矿中氧化镁干扰的研究[J].铜业工程,2017(6):77-79,83.
[12]巫方才.火焰原子吸收光谱法同时测定金属酸洗废液中铜、铁、锌、镍的含量[J].安徽农业科学,2004,32(4):645-645.
[13]李瑜华,莫胜钧.空气-乙炔火焰原子吸收测定铬时与浓度有关的化学干扰的研究---Ⅰ、铁、钴对铬的干扰[J].分析测试通报,1991,10(1):32-35.
[14]HJ 757-2015,水质铬的测定火焰原子吸收分光光度法[S].
[15]国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2002.
[16]鲁丹,陈海青.火焰原子吸收法测定水中总铬的影响因素探讨[J].中国公共卫生,2004,20(4):417-418.
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