Determination of Pb, As in Liquid Cosmetics and Cl in Bath Salts by X-Ray Fluorescence Spectrometry
摘 要
用聚焦式X射线荧光光谱仪测定液体化妆品中的铅、砷,以及浴盐中氯的含量,并提出了一种新的进样方法——瓶口贴膜法。对液体样品可直接进样分析,对一些固体样品,如浴盐,需经灼烧灰化后以1∶5的质量比溶于水中再行测定。方法中选用体积为2 mL,且其瓶口高度误差在0.2 mm以内,具有带孔瓶盖的小瓶作为进样瓶。将液体样品装入瓶中,使液面略超瓶口,随即将2.5 μm聚酯(Mylar)膜覆盖于上,拧上瓶盖并使膜紧贴液面,保持平整。将进样瓶置于样品台上,移动样品台,用激光对焦,采用扩展康普顿散射模型进行基体校正和校准曲线拟合。结果表明:常量氯元素的测定值的相对标准偏差(n=11)为0.65%;痕量铅和砷的测定值的相对标准偏差(n=11)均小于5.0%,其检出限分别为3.0,1.0 mg·L-1。测定结果均与标准方法测定结果相符。
Abstract
The focusing X-ray fluorescence spectrometer was used to determine Pb and As in liquid cosmetics and Cl- in bath salt, and a new method of sample introduction-film mounted sample bottle method was proposed. Liquid samples could be introduced directly for analysis, but for solid sample, e.g. bath salt, it should be ignited, ashed and dissolved in water by the mass ratio of 1 to 5, and the solution was then used for analysis. As described in the method, small bottles having its volume of 2 mL, keeping the deviation of height of its bottle mouth within 0.2 mm and attached with holed caps were selected for use as sample introduction bottles (abbre. as SIB). Liquid sample (or solution) was transferred into the SIB with the liquid surface a little higher over the bottle mouth. A piece of 2.5 μm Mylar film was mounted on the liquid sample, and the cap was screwed on, keeping the Mylar film to adhere tightly to the liquid surface and to be level and smooth. The SIB was then moved onto the sample tab and focused with laser. The extended Compton scattering model was used for matrix correction and fitting of calibration curve. As shown by the results, RSD (n=11) of the major contents of chlorine was 0.65%. RSDs (n=11) for traces of Pb, As were both less than 5.0%, and detection limits for Pb and As were 3.0, 1.0 mg·L-1, respectively. The results obtained by this method were consistent with those found by the standard method.
中图分类号 O657.34 DOI 10.11973/lhjy-hx201804003
所属栏目 试验与研究
基金项目 宁波出入境检验检疫局项目(甬K04-2015)
收稿日期 2017/4/8
修改稿日期
网络出版日期
作者单位点击查看
联系人作者郑琳(693161902@qq.com)
备注杨乐萍,硕士,主要从事化妆品有害物质检测的工作
引用该论文: YANG Leping,WENG Donghai,XU Jiaming,GAO Jianan,ZHENG Lin,REN Fei,WANG Qian. Determination of Pb, As in Liquid Cosmetics and Cl in Bath Salts by X-Ray Fluorescence Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(4): 383~387
杨乐萍,翁东海,许佳明,高佳男,郑琳,任飞,王谦. X射线荧光光谱法测定液体化妆品中铅、砷和浴盐中氯的含量[J]. 理化检验-化学分册, 2018, 54(4): 383~387
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参考文献
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【4】BONING P, BARD E, ROSE J. Toward direct, micron-scale XRF elemental maps and quantitative profiles of wet marine sediments[J]. Geochemistry Geophysics Geosystems, 2007,8(5):2637-2655.
【5】袁静,罗立强.同步辐射微区X射线荧光光谱法原位分析蚯蚓中K,Ca,Zn和Pb[J].分析化学, 2016,44(5):792-798.
【6】SITKO R, KOCOT K, ZAWISZA B, et al. Liquid-phase microextraction as an attractive tool for multielement trace analysis in combination with X-ray fluorescence spectrometry:An example of simultaneous determination of Fe, Co, Zn, Ga, Se and Pb in water samples[J]. Journal of Analytical Atomic Spectrometry, 2011,26(10):1979-1985.
【7】IGARASHI S, TAKAHASHI A, UEKI Y, et al. Homogeneous liquid-liquid extraction followed by X-ray fluorescence spectrometry of a microdroplet on filter-paper for the simultaneous determination of small amounts of metals[J]. Analyst, 2000,125(5):797-798.
【8】MILLER T C, HASTINGS E P, HAVRILLA G J. Automated printing technology as a new tool for liquid sample preparation for micro X-ray fluorescence (MXRF)[J]. X-Ray Spectrometry, 2010,35(2):131-136.
【9】MCINTOSH K G, NEAL J A, NATH P, et al. Microfluidic sample preparation for elemental analysis in liquid samples using micro X-ray fluorescence spectrometry[J]. X-Ray Spectrometry, 2014,43(6):332-337.
【10】国家食品药品监督管理总局.化妆品安全技术规范(2015年版)[A/OL].[2015-12-23]. 2015. http://www.sda.gov.cn/WS01/CL1870/140161.html.
【11】QB/T 2744.1-2005浴盐第1部分:足浴盐[S].
【12】QB/T 2744.2-2005浴盐第2部分:沐浴盐[S].
【13】王纪华,刘晓丽,高龙,等.X射线荧光光谱法测定镍电解液中的镍、氯、硫酸根[J].冶金分析, 2012,32(12):29-33.
【14】樊兴涛,詹秀春,巩爱华.偏振激发-能量色散X射线荧光光谱法测定卤水中主量元素硫氯钾钙[J].岩矿测试, 2007,26(2):109-112.
【15】王谦,王群威,张建波,等.汽油中微量元素的X射线荧光光谱分析[J].石油学报(石油加工), 2008,24(3):360-364.
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