内标元素强度筛选法在激光诱导击穿光谱定量分析铝合金样品中的应用  

Application of internal standard element strength-screening method in quantitative analysis of aluminum alloy samples by laser induced breakdown spectroscopy

作　　者：王华丽 赵书瑞 卢孟柯 赵志巍 WANG Hua-li;ZHAO Shu-rui;LU Meng-ke;ZHAO Zhi-wei(College of Automobile and Electronic Engineering,Baoding University,Baoding 071000,China)

机构地区：[1]保定学院汽车与电子工程学院,河北保定071000

出　　处：《冶金分析》2020年第3期9-15,共7页Metallurgical Analysis

基　　金：河北省高等学校科学技术研究青年基金项目(QN2015313)。

摘　　要：利用激光诱导击穿光谱技术进行光谱定量分析时,由于实验条件不稳定造成的测量结果检测限差、测量准确度低的问题一直备受研究者的关注。实验选取铝合金标准样品为分析样品,以输出波长为1064 nm的Nd∶YAG激光器为激发光源,设置脉冲重复频率1 Hz,通过激光诱导击穿光谱实验装置采集样品在260~300 nm、300~330 nm范围内的等离子体光谱。采用以内标法为基础的内标元素强度筛选法处理数据,分析了铝合金待测样品E113中Mn、Mg、Fe和Cu元素的含量,并且与常规的数据平均法进行了比较。测得其质量分数分别为5.92、4.79、4.06、39.00 mg/g,测量结果的相对误差由数据平均法的9.80%、3.70%、13.30%、3.47%分别降为5.52%、0.40%、4.92%、3.23%;Mn、Mg、Fe、Cu各元素的检测限由数据平均法的0.205、0.207、0.755、6.150 mg/g下降为0.163、0.176、0.674、1.71 mg/g。此结果说明根据内标元素谱线强度进行数据筛选的数据预处理法同样适用于基体元素含量近似相同的铝合金样品分析,实验结果基本符合金属样品定量分析的要求,此数据处理方法为实验条件不稳定下的元素定量分析提供了一种新的思路。During the quantitative analysis by laser induced breakdown spectroscopy(LIBS),some problems such as poor limit of detection and low measurement accuracy were usually caused due to unstable experimental conditions,which have been concerned by researchers.The aluminum alloy certified reference materials were selected as the analytical samples.The Nd∶YAG laser with wavelength of 1064 nm was employed as the excitation source,and the pulse repetition frequency was set at 1 Hz.The plasma spectra of samples in range of 260-300 nm and 300-330 nm were collected by the laser induced breakdown spectroscopy.The data were processed with internal standard element strength-screening method based on internal standard method.The contents of Mn,Mg,Fe and Cu in aluminum alloy sample E113 were analyzed and compared with the results obtained by conventional data averaging method.The measured mass fraction for Mn,Mg,Fe and Cu was 5.92,4.79,4.06 and 39.00 mg/g,respectively.The relative error of determination results was reduced from 9.80%,3.70%,13.30% and 3.47% of the data averaging method to 5.52%,0.40%,4.92% and 3.23%,respectively.Meanwhile,the limit of detection of Mn,Mg,Fe and Cu was reduced from 0.205,0.207,0.755 and 6.150 mg/g of the data averaging method to 0.163,0.176,0.674 and 1.71 mg/g,respectively.The results indicated that the data pretreatment method by data screening based on spectral line strength of internal standard elements was also suitable for the analysis of aluminum alloy samples with similar contents of matrix element.The experimental results could basically meet the requirements of quantitative analysis for metal samples.This data processing method provided a new idea for the quantitative analysis of elements under unstable experimental conditions.

关 键 词：激光诱导击穿光谱 内标法 检测限 内标元素强度筛选法 数据平均法 

分 类 号：O657.38[理学—分析化学]