溶液阴极辉光放电光谱信号的内标法定量分析研究

发布时间：2018-07-11 10:21

本文选题：溶液阴极辉光放电-原子发射光谱 + 定量分析　；参考：《光谱学与光谱分析》2017年09期

【摘要】：溶液阴极辉光放电-原子发射光谱是一种新颖的快速、高效、实时在线的元素分析方法,它可用于水体金属元素的检测。为提高其测量精确度和稳定性,将内标法应用于溶液阴极辉光放电-原子发射光谱技术。对K元素建立了标准定标曲线和以H_β为内标元素的定标曲线,内标法测得样品的相对误差和相对标准偏差分别为1.11%,2.14%,精确度和稳定性较之标准曲线法有一定的提高。实验考察了元素谱线强度在同一时段的波动情况,发现元素K和H_β的谱线强度变化趋势稍有不同,而同主族元素K和Rb,Ca和Mg的谱线强度有相同的变化趋势,提出选择与待测元素同主族且谱线强度变化趋势较为一致的元素作为内标元素能更大化校正实验波动的观点。同时探讨了K以Rb为内标元素、Ca以Mg为内标元素以及Mg以Ca为内标元素时的内标法测量的精确度和稳定性,得其相对误差分别为0.49%,0.02%和0.30%,相对标准偏差分别为1.11%,1.13%和0.87%,与标准曲线法和以H_β为内标元素的内标法相比效果更佳。测得自来水样品中Ca元素以Mg为内标的相对误差和相对标准偏差为0.58%,1.03%,Mg元素以Ca为内标的相对误差和相对标准偏差为1.57%和1.10%。研究结果表明,将溶液阴极辉光放电-原子发射光谱技术应用于水体金属元素检测时,内标法可以有效校正实验波动的影响,提高测量的精确度和稳定性。
[Abstract]:Solution cathodic glow discharge-atomic emission spectroscopy is a novel, fast, efficient and real-time on-line element analysis method, which can be used for the detection of metal elements in water. In order to improve the measurement accuracy and stability, the internal standard method was applied to the cathodic glow discharge-atomic emission spectrometry. The standard calibration curve of K element and the calibration curve with H _ 尾 as internal standard element were established. The relative error and relative standard deviation of the sample measured by the internal standard method were 1.11 and 2.14, respectively. The accuracy and stability of the method were improved to some extent compared with the standard curve method. The variation trend of spectral line strength of element K and H _ 尾 is slightly different from that of element K, but the intensity of spectral line of elements K, RB, Ca and mg has the same trend. It is pointed out that the selection of elements with the same main family and the same trend of spectral intensity as internal standard elements can be used to correct the experimental fluctuations more greatly. At the same time, the accuracy and stability of the internal standard method for K with RB as internal standard element, Ca with mg as internal standard element and mg with Ca as internal standard element are discussed. The relative error is 0.490.2% and 0.30%, and the relative standard deviation is 1.11% and 0.87%, respectively, which is better than the standard curve method and the internal standard method with H _ 尾 as the internal standard element. The relative error and relative standard deviation of Ca in tap water samples with mg as internal standard and relative standard deviation are 0.58 and 1.03 respectively. The relative error and relative standard deviation of mg element with Ca as internal standard are 1.57% and 1.10% respectively. The results show that when the solution cathodic glow discharge-atomic emission spectroscopy is applied to the detection of metallic elements in water body, the internal standard method can effectively correct the influence of the experimental fluctuation and improve the accuracy and stability of the measurement.
【作者单位】：重庆邮电大学光电工程学院;
【基金】：重庆市基础与前沿研究计划一般项目(cstc2016jcyjA0389);重庆市基础与前沿研究计划重点项目(cstc2015jcyjBX0016) 重庆市教委科技项目(KJ1500436) 留学归国人员科研启动基金项目(教外司留[2015]1098号)资助
【分类号】：O657.31;X832

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