水体中铬、镉和铅的X射线荧光光谱同时快速分析方法研究

发布时间：2018-01-01 17:06

本文关键词：水体中铬、镉和铅的X射线荧光光谱同时快速分析方法研究　出处：《光谱学与光谱分析》2017年06期 　论文类型：期刊论文

【摘要】：以氢氧化钠和硫化钠为沉淀剂采用共沉淀法同时富集水体中的Cr,Cd和Pb,通过对Cr(OH)3,Cd(OH)2和PbS沉淀均匀悬浮液抽滤以制成Cr,Cd和Pb均匀分布的薄膜样品并进行能量色散XRF光谱测量,以实现水体中Cr,Cd和Pb的同时快速分析与检测。研究了富集过程中的反应时间和反应物摩尔比对薄膜样品XRF光谱强度的影响,确定了富集过程的最佳反应条件为沉淀反应时间为5min,OH-与Cr3+的最佳摩尔比为5.0,OH-与Cd2+的最佳摩尔比为5.0,S2-与Pb2+的最佳摩尔比为2;对富集后不同浓度的薄膜样品进行了均匀性检验,富集区域6个不同位置荧光强度的相对标准偏差均小于4.8%,说明富集后的薄膜样品具有较好的均匀性;将不同浓度薄膜样品的理论浓度值与ICP-MS方法测得的浓度值进行对比分析,验证了该富集方法对水样中Cr,Cd和Pb的富集率均能达到90%以上;根据薄膜样品的荧光强度与ICP-MS测得的浓度值,建立了基于该富集方法的水体中Cr,Cd和Pb的X射线荧光光谱定量分析方法,Cr,Cd和Pb校准曲线的线性相关系数分别为0.997 3,0.995 0和0.999 8,当实际采集水样体积为50mL时,Cr,Cd和Pb的检出限分别为7.4,29.6和8.5μg·L~(-1),均低于《污水综合排放标准GB 8978—1996》中Cr,Cd和Pb的最高允许排放浓度,因此该方法能够实现工业生产及生活排放污水中Cr,Cd和Pb的同时快速分析与检测。该研究为基于X射线荧光光谱法的水体多种重金属同时快速在线监测提供依据。
[Abstract]:Sodium hydroxide and sodium sulfide as precipitation agent and using the method of enrichment in water Cr co precipitation, Cd and Pb, based on Cr (OH) 3, Cd (OH) 2 and PbS precipitation homogeneous suspension filtration to produce Cr, Cd and Pb films were evenly distributed and energy dispersive XRF spectra, in order to achieve the water in the Cr, Cd and Pb at the same time, the rapid detection and analysis. Effects of the enrichment process, reaction time and molar ratio of reactants on the thin film samples of XRF spectral intensity, the optimum reaction conditions were determined for the enrichment process of precipitation reaction time was 5min, the optimum molar ratio of OH- and Cr3+ was 5, and the optimum molar ratio of OH- Cd2+ is 5, the optimum molar ratio of S2- to Pb2+ was 2; of enrichment thin film samples of different concentration of homogeneity, the relative standard deviation of enrichment area in 6 different positions of fluorescence intensity were less than 4.8%, which shows that the film has a good sample after enrichment The theory of uniformity; concentration of different film samples concentration and ICP-MS measured value were compared and analyzed to verify the method of enrichment in water samples Cr, Cd and Pb accumulation rate could reach more than 90%; according to the fluorescence intensity and the concentration of ICP-MS film samples measured values, established the enrichment the method of Cr in water based on X ray fluorescence quantitative Cd and Pb analysis method, Cr, linear correlation coefficient of Cd and Pb of the calibration curves were 0.997 3,0.995 0 and 0.9998, when the actual volume of water samples were collected for 50mL, Cr, Cd and Pb detection limit were 7.4,29.6 and 8.5 G - L~ (-1), were lower than the "integrated wastewater discharge standard GB 8978 - 1996> Cr, Cd Pb and the maximum allowable emission concentration, so this method can realize the industrial production and living sewage in Cr, Cd and Pb at the same time, the rapid detection and analysis. The research for X ray fluorescence spectrometry based on It provides a basis for the simultaneous rapid online monitoring of a variety of heavy metals in the water body.

【作者单位】：中国科学院安徽光学精密机械研究所中国科学院环境光学与技术重点实验室安徽省环境光学监测技术重点实验室;皖江新兴产业技术发展中心;解放军陆军军官学院;
【基金】：皖江新兴产业技术发展中心企业合作项目(ZNJX-15-01) 国家(863)计划项目(2013AA065502) 安徽省科技攻关计划项目(1501041119) 安徽省科技重大专项项目(15CZZ04125)资助
【分类号】：O657.34;X832
【正文快照】： 1.中国科学院安徽光学精密机械研究所,中国科学院环境光学与技术重点实验室,安徽省环境光学监测技术重点实验室,安徽合肥2300312.皖江新兴产业技术发展中心,安徽铜陵2440003.解放军陆军军官学院,安徽合肥230031引言近年来,社会经济的快速增长和工业进程的快速发展,使得我国环

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