能量色散X射线荧光光谱法测定自来水中痕量氯
|
摘要
采用能量色散X射线荧光光谱法,分别在空气、氮气和氦气气氛下测定自来水中痕量氯,结果表明,在氦气条件下不仅可以消除空气中氩气的干扰,还可以增加探测器接收到的氯谱峰强度,因此选择在氦气条件下采用能量色散X射线荧光光谱法测定自来水中痕量氯。通过研究氯元素峰背比与X光管管压、管流的关系,选择最佳工作条件为:光管管压15kV,光管电流800μA。氯质量浓度为0～200μg/mL时,与其对应的X射线荧光光谱相对强度呈线性,线性相关系数R~2=0.997 5;检出限为2.94μg/mL。按照实验方法测定30μg/mL和10μg/mL氯标准溶液中氯,结果的相对标准偏差(RSD,n=11)分别为11%和16%;对两个自来水实际样品进行加标回收试验,回收率为89%～119%。
The content of trace chlorine in tap water was determined by energy dispersive X-ray fluorescence spectrometry in atmospheres of air,nitrogen and helium,respectively.The results showed that the helium atmosphere could not only eliminate the interference of argon in air,but also enhance the spectral peak intensity of chlorine received by detector.Therefore,the helium atmosphere was selected to determine trace chlorine in tap water by energy dispersive X-ray fluorescence spectrometry.The relationship between peak-to-background ratio and X-ray tube voltage and tube current was studied.The optimal working conditions were obtained as follows:the tube voltage was 15 kV and the tube current was 800μA.When the mass fraction of chlorine was in range of 0-200μg/mL,it had linear relationship to the corresponding Xray fluorescence relative intensity with linear correlation coefficient of R~2=0.997 5.The detection limit was 2.94μg/mL.The content of chlorine in standard solution(30μg/mL and 10μg/mL)was determined according to the experimental method.The relative standard deviation(RSD,n=11)was 11%and 16%,respectively.Two actual tap water samples were used for recovery tests.The spiked recoveries were between 89%and 119%.
The content of trace chlorine in tap water was determined by energy dispersive X-ray fluorescence spectrometry in atmospheres of air,nitrogen and helium,respectively.The results showed that the helium atmosphere could not only eliminate the interference of argon in air,but also enhance the spectral peak intensity of chlorine received by detector.Therefore,the helium atmosphere was selected to determine trace chlorine in tap water by energy dispersive X-ray fluorescence spectrometry.The relationship between peak-to-background ratio and X-ray tube voltage and tube current was studied.The optimal working conditions were obtained as follows:the tube voltage was 15 kV and the tube current was 800μA.When the mass fraction of chlorine was in range of 0-200μg/mL,it had linear relationship to the corresponding Xray fluorescence relative intensity with linear correlation coefficient of R~2=0.997 5.The detection limit was 2.94μg/mL.The content of chlorine in standard solution(30μg/mL and 10μg/mL)was determined according to the experimental method.The relative standard deviation(RSD,n=11)was 11%and 16%,respectively.Two actual tap water samples were used for recovery tests.The spiked recoveries were between 89%and 119%.
引文
[1]中华人民共和国卫生部,中国国家标准化管理委员会.GB 5749-2006生活饮用水卫生标准[S].北京:中国标准出版社,2007.
[2]陈祖兰,李传高,张继.自来水中氯化物检验[J].化工学报(Journal of Chemical Industry and Engineering(China)),2015(6):129-130.
[3]王晓楠,刘昱,潘献辉,等.水中氯化物检测及样品前处理技术研究进展[J].理化检验:化学分册,2014,50(10):1319-1321.WANG Xiao-nan,LIU Yu,PAN Xian-hui,et al.Progress on determination of chloride in drinking water and sample preparation techniques[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(10):1319-1321.
[4]李蓉,胡继红.水中氯化物检验方法概述[J].中国科技博览,2012(4):59-60.
[5]马芝慧,耿淑杰.硝酸银容量法和离子色谱法测定水中氯化物的比较[J].科技展望(Science and Technology),2015(15):58.
[6]肖学喜.自动电位滴定法测定炼油工业污水中的氯离子[J].化学分析计量,2007,16(5):26-28.XIAO Xue-xi.Determination of chloride ion in oil refining industry sewage by automatic electrictitration method[J].Quantitative Chemical Analysis,2007,16(5):26-28.
[7]王瑞珺.XRF法测定工业循环水中硫和氯[J].光谱实验室,2004,21(3):613-614.WANG Rui-jun.Determination of sulphar and chlorine in industrial circulate water by XRF[J].Chinese Journal of Spectroscopy Laboratory,2004,21(3):613-614.
[8]刘树文,张成伟.X射线荧光光谱法测定东营地区卤水中的氯溴碘[J].中国测试技术,2006,32(5):133-135.LIU Shu-wen,ZHANG Cheng-wei.Determination of Cl,Br and I in bittern by XRF[J].Chemical Analysis and Meterage,2006,32(5):133-135.
[9]乔涛,费利军,鲍元进,等.X射线荧光光谱法测定石化产品中的总氯[J].化学分析计量,2014,23(2):69-71.QIAO Tao,FEI Li-jun,BAO Yuan-jin,et al.Determination of total chlorine in petroleum and chemical products by X-ray fluorescence spectrometry[J].Chemical Analysis and Meterage,2014,23(2):69-71.
[10]顾海波,张大华,雷秦睿,等.X射线荧光光谱法测定汽油中的氯含量[J].石油炼制与化工,2005,46(12):94-97.GU Hai-bo,ZHANG Da-hua,LEI Qin-rui,et al.Determination of chlorine content in gasoline by X-ray fluorescence spectrometry[J].Petroleum Processing and Petrochemicals,2005,46(12):94-97.
[2]陈祖兰,李传高,张继.自来水中氯化物检验[J].化工学报(Journal of Chemical Industry and Engineering(China)),2015(6):129-130.
[3]王晓楠,刘昱,潘献辉,等.水中氯化物检测及样品前处理技术研究进展[J].理化检验:化学分册,2014,50(10):1319-1321.WANG Xiao-nan,LIU Yu,PAN Xian-hui,et al.Progress on determination of chloride in drinking water and sample preparation techniques[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(10):1319-1321.
[4]李蓉,胡继红.水中氯化物检验方法概述[J].中国科技博览,2012(4):59-60.
[5]马芝慧,耿淑杰.硝酸银容量法和离子色谱法测定水中氯化物的比较[J].科技展望(Science and Technology),2015(15):58.
[6]肖学喜.自动电位滴定法测定炼油工业污水中的氯离子[J].化学分析计量,2007,16(5):26-28.XIAO Xue-xi.Determination of chloride ion in oil refining industry sewage by automatic electrictitration method[J].Quantitative Chemical Analysis,2007,16(5):26-28.
[7]王瑞珺.XRF法测定工业循环水中硫和氯[J].光谱实验室,2004,21(3):613-614.WANG Rui-jun.Determination of sulphar and chlorine in industrial circulate water by XRF[J].Chinese Journal of Spectroscopy Laboratory,2004,21(3):613-614.
[8]刘树文,张成伟.X射线荧光光谱法测定东营地区卤水中的氯溴碘[J].中国测试技术,2006,32(5):133-135.LIU Shu-wen,ZHANG Cheng-wei.Determination of Cl,Br and I in bittern by XRF[J].Chemical Analysis and Meterage,2006,32(5):133-135.
[9]乔涛,费利军,鲍元进,等.X射线荧光光谱法测定石化产品中的总氯[J].化学分析计量,2014,23(2):69-71.QIAO Tao,FEI Li-jun,BAO Yuan-jin,et al.Determination of total chlorine in petroleum and chemical products by X-ray fluorescence spectrometry[J].Chemical Analysis and Meterage,2014,23(2):69-71.
[10]顾海波,张大华,雷秦睿,等.X射线荧光光谱法测定汽油中的氯含量[J].石油炼制与化工,2005,46(12):94-97.GU Hai-bo,ZHANG Da-hua,LEI Qin-rui,et al.Determination of chlorine content in gasoline by X-ray fluorescence spectrometry[J].Petroleum Processing and Petrochemicals,2005,46(12):94-97.