工作场所空气中砷原子荧光光谱法分析方法改进
|
摘要
目的对工作场所空气中砷的原子荧光光谱分析方法进行改进。方法以硝酸—高氯酸溶液作为消化体系,在自动控温电热板上280℃直接消化处理样品,使用原子荧光光谱仪和标准曲线法对工作场所空气中砷浓度进行测定。结果该方法在0～20μg/L的砷浓度范围内,标准曲线回归方程为y=60.660 3x–16.099 0,相关系数为0.999 5,方法的检出限为0.021 9μg/L,定量下限为0.073μg/L,批内精密度(相对标准偏差)为0.51%～1.02%,批间精密度为2.25%～4.38%,加标回收率为100.36%～102.35%。结论该方法具有灵敏、准确、稳定、检出限低、操作简单、耗时短等优点,具有一定推广价值。
Objective To improve method for detection of arsenic in workplace air with atomic fluorescence spectrometry. Methods With a nitric acid-perchloric acid solution digestion system, the samples were directly digested at280 ℃ on an automatic temperature-controlled electric heating plate, and the arsenic in the workplace air samples was determined with standard curve method of atomic fluorescence spectrometer. Results Within the concentration of arsenic ranging from 0 μg/L to 20 μg/L, the regression equation of standard curve was y = 60.660 3 x – 16.099 0; the correlation coefficient was 0.999 5; the detection limit of arsenic was 0.021 9 μg/L; the lower limit of quantitation was 0.073 μg/L.Relative standard deviation of precision within a batch was 0.51% – 1.02% and relative standard deviation of inter batches precision was 2.25% – 4.38%. The recovery rate was between 100.36% and 102.35% for the detections. Conclusion The method is accurate and stable, with low detection limit, simple operation and short time consuming, and could be applied in practical detection.
Objective To improve method for detection of arsenic in workplace air with atomic fluorescence spectrometry. Methods With a nitric acid-perchloric acid solution digestion system, the samples were directly digested at280 ℃ on an automatic temperature-controlled electric heating plate, and the arsenic in the workplace air samples was determined with standard curve method of atomic fluorescence spectrometer. Results Within the concentration of arsenic ranging from 0 μg/L to 20 μg/L, the regression equation of standard curve was y = 60.660 3 x – 16.099 0; the correlation coefficient was 0.999 5; the detection limit of arsenic was 0.021 9 μg/L; the lower limit of quantitation was 0.073 μg/L.Relative standard deviation of precision within a batch was 0.51% – 1.02% and relative standard deviation of inter batches precision was 2.25% – 4.38%. The recovery rate was between 100.36% and 102.35% for the detections. Conclusion The method is accurate and stable, with low detection limit, simple operation and short time consuming, and could be applied in practical detection.
引文
[1]余慧珍.氢化物原子荧光仪测定样品中砷含量常见问题的初步探讨[J].现代预防医学,2007,34(12):2333.
[2]李永新,黎源倩,渠凌丽.电热消解-原子荧光光谱法测定土壤中的砷[J].现代预防医学,2008,35(13):2482-2483.
[3]杜洪月,沈月华,张坤.湿法消解-原子荧光光谱法同时测定油脂样品中砷和汞[J].中国卫生检验杂志,2005,15(9):1060-1064.
[4]罗晓芳,郭玮,秦文华.氢化物原子荧光法同时测定工作场所空气中的砷和锑[J].工业卫生与职业病,2008,34(3):182-184.
[5]中华人民共和国国家卫生和计划生育委员会,GBZ/T 300.47-2017工作场所空气有毒物质测定:砷及其无机化合物的酸消解一原子荧光光谱法[S].北京:国家标准出版社,2017.
[6]中华人民共和国卫生部,GBZ/T 160.31-2004工作场所空气有毒物质测定:砷及其化合物的氢化物发生一原子荧光光谱法[S].北京:国家标准出版社,2004.
[7]刁春霞,刘波,杨华梅.两种预还原剂对化妆品中砷测定结果的比较[J].现代预防医学,2008,35(3):541-542.
[8]陈素军,王玉江.L-半胱氨酸作还原剂测定肉及肉制品中无机砷[J].现代仪器,2008,14(6):66-67.
[9]余波,伊萍,高岩,等.原子荧光法测定车间空气中总砷[J].中国公共卫生,2004,20(2):199.
[10]中华人民共和国卫生部,GBZ/T 210.4-2008职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法[S].北京:国家标准出版社,2008.
[11]中华人民共和国卫生部,GBZ/T 2.1-2007工作场所有害因素职业接触限值:工作场所空气中化学物质容许浓度[S].北京:国家标准出版社,2007.
[2]李永新,黎源倩,渠凌丽.电热消解-原子荧光光谱法测定土壤中的砷[J].现代预防医学,2008,35(13):2482-2483.
[3]杜洪月,沈月华,张坤.湿法消解-原子荧光光谱法同时测定油脂样品中砷和汞[J].中国卫生检验杂志,2005,15(9):1060-1064.
[4]罗晓芳,郭玮,秦文华.氢化物原子荧光法同时测定工作场所空气中的砷和锑[J].工业卫生与职业病,2008,34(3):182-184.
[5]中华人民共和国国家卫生和计划生育委员会,GBZ/T 300.47-2017工作场所空气有毒物质测定:砷及其无机化合物的酸消解一原子荧光光谱法[S].北京:国家标准出版社,2017.
[6]中华人民共和国卫生部,GBZ/T 160.31-2004工作场所空气有毒物质测定:砷及其化合物的氢化物发生一原子荧光光谱法[S].北京:国家标准出版社,2004.
[7]刁春霞,刘波,杨华梅.两种预还原剂对化妆品中砷测定结果的比较[J].现代预防医学,2008,35(3):541-542.
[8]陈素军,王玉江.L-半胱氨酸作还原剂测定肉及肉制品中无机砷[J].现代仪器,2008,14(6):66-67.
[9]余波,伊萍,高岩,等.原子荧光法测定车间空气中总砷[J].中国公共卫生,2004,20(2):199.
[10]中华人民共和国卫生部,GBZ/T 210.4-2008职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法[S].北京:国家标准出版社,2008.
[11]中华人民共和国卫生部,GBZ/T 2.1-2007工作场所有害因素职业接触限值:工作场所空气中化学物质容许浓度[S].北京:国家标准出版社,2007.