高含量氯化铷ICP-OES法分析测定  

Determination of High Concentrations of Rubidium Chloride by ICP-OES

作　　者：钟远[1] 孙柏[1] 李海军[1] 王涛[1,2] 李武 宋彭生[1] 

机构地区：[1]中国科学院青海盐湖研究所,青海西宁810008 [2]中国科学院大学,北京100049

出　　处：《光谱学与光谱分析》2015年第1期223-228,共6页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(20773152);青海省科技创新能力促进计划项目(2009-Z-725)资助

摘　　要：目前电感耦合等离子体发射光谱法（ICP-OES）常用于痕量或微量铷元素的分析,针对常量组分铷的分析未见文献报道。通过样品用容量法连续稀释的方法测定常量组分铷离子含量时,会引进较大的误差。本研究通过质量稀释和优化仪器参数的方法,采用ICP-OES直接测定氯化铷溶液中的高含量铷,减少了稀释次数和稀释引进的误差,提高了分析结果的准确度。实验对铷离子的三条检测谱线的灵敏度、线性相关系数和测定结果的相对偏差进行分析,确定铷的合适检测谱线为780.023nm。实验发现ICP-OES仪器参数（雾化器流量、分析泵速和高频功率）对高含量铷的测定结果影响较大,这是由于仪器参数影响雾化效率和谱线的发射强度,进而影响铷的测定结果。通过正交试验分析各仪器参数对铷测定的影响顺序,进一步依靠单因素试验确定较优的仪器参数。优化的仪器参数组合为雾化器流量0.60L·min^-1、分析泵速60r·min^-1、高频功率1 150 W。在优化的仪器参数条件下进行间隔一周的重复实验,结果发现当RbCl浓度在0.09%~0.18%范围内时,测定结果的相对偏差〈0.5%,可以保证较高的准确度。当RbCl浓度为0.06%时,测定结果的相对偏差为-1.7%。实验比较了高浓度氯化锂、氯化钾和氯化铷溶液ICP-OES法的分析测定,在相近的仪器参数条件下氯化锂的测定结果优于氯化钾和氯化铷。本研究的ICP-OES方法操作简便且快速,适合于含铷体系的相化学研究以及高含量铷产品的分析。The method of ICP-OES for the direct determination of high content of rubidium in rubidium chloride solutions was studied through mass dilution method and optimizing parameters of the instrument in the present paper .It can reduce the times of dilution and the error introduced by the dilution ,and improve the accuracy of determination results of rubidium .Through ana-lyzing the sensitivity of the three detection spectral lines for rubidium ion ,linearly dependent coefficient and the relative errors of the determination results ,the spectral line of Rb 780.023 nm was chosen as the most suitable wavelength to measure the high content of rubidium in the rubidium chloride solutions .It was found that the instrument parameters of ICP-OES such as the at-omizer flow ,the pump speed and the high-frequency power are the major factors for the determination of rubidium ion in the ru-bidium chloride solutions .As we know instrument parameters of ICP-OES have an important influence on the atomization effi-ciency as well as the emissive power of the spectral lines of rubidium ,they are considered as the significant factors for the deter-mination of rubidium .The optimization parameters of the instrument were obtained by orthogonal experiments and further single factor experiment ,which are 0.60 L·min^-1 of atomizer flow ,60 r·min^-1 of pump speed ,and 1 150 W of high-frequency pow-er .The same experiments were repeated a week later with the optimization parameters of the instrument ,and the relative errors of the determination results are less than 0.5% when the concentration of rubidium chloride ranged from 0.09% to 0.18% .As the concentration of rubidium chloride is 0.06% ,the relative errors of the determination results are -1.7% .The determination＆amp;nbsp;of lithium chloride and potassium chloride in the high concentration of the aqueous solutions was studied under the condition of similar instrument parameters .It was found by comparison that the determination results of lithium chloride are better than that of potas

关 键 词：氯化铷 ICP-OES 仪器参数 

分 类 号：O657.6[理学—分析化学]