激光剥蚀-大气压辉光放电原子发射光谱法中土壤样品分析基质效应研究  

Matrix Effect of Soil Samples in Laser Ablation-Atmospheric Pressure Glow Discharge Atomic Emission Spectrometry

作　　者：葛粉 高亮 彭晓旭 俞进 朱钰方[1] 汪正[2,3] GE Fen;GAO Liang;PENG Xiao-Xu;YU Jin;ZHU Yu-Fang;WANG Zheng(School of Materials Science and Engineering,University of Shanghai for Science&Technology,Shanghai 200093,China;Shanghai Institute of Ceramics,Chinese Academy of Sciences,Shanghai 201899,China;Center of Materials Science and Optoelectronics Engineering,University of Chinese Academy of Sciences,Beijing 100049,China;School of Physics and Astronomy,Shanghai Jiao Tong)

机构地区：[1]上海理工大学材料科学与工程学院,上海200093 [2]中国科学院上海硅酸盐研究所,上海201899 [3]中国科学院大学材料科学与光电工程中心,北京100049 [4]上海交通大学物理与天文学院,上海200240

出　　处：《分析化学》2020年第8期1111-1119,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.21175145);中国科学院科研装备研制项目(No.YZ201539);上海无机材料测试和表征技术平台(No.19DZ2290700)资助。

摘　　要：采用激光剥蚀-大气压辉光放电原子发射光谱法(LA-APGD-AES)研究了土壤样品中基质效应对于Cd和Pb元素检测结果的影响。选取来自不同地区、主成分含量相差较大的实际土壤样品进行研究。在激光能量60 mJ、激光脉冲数20的条件下,对APGD-AES的参数条件进行优化。放电间距为14 mm、气体流速为130 mL/min、放电电流为27 mA时,信号强度及稳定性最佳。在最佳条件下,采用本方法结合单变量校准模型分别对4种复杂基质土壤中的Cd和Pb进行定量检测,并将检测结果拟合在同一校准曲线中进行分析。对4种不同基质土壤检测所得的Cd和Pb的线性相关系数分别为R 2≥0.99和R 2>0.97,两种元素LA-APGD-AES测量值与电感耦合等离子体原子发射光谱法(ICP-AES)测量值的相对误差均在0.4%~11.8%之间;拟合在同一校准曲线中分析所得的Cd和Pb元素的R 2变化不明显,两种元素测量相对误差均在3.0%~13.2%之间。不同基质土壤中Cd和Pb元素的检出限(LOD)变化不明显,测量结果均与配制浓度吻合。结果表明,本方法对复杂基质土壤中Cd和Pb元素的检测结果受基质效应的影响较小。Laser ablation-atmospheric pressure glow discharge atomic emission spectrometry(LA-APGD-AES)was utilized to investigate the effect of matrix effects on the detection results of Cd and Pb in soil samples.Actual soil samples from different regions with large differences in major substances were selected.Under the laser energy of 60 mJ and laser pulse number of 20,the stable signal intensity and high sensitivity were obtained when the discharge distance was 14 mm,the gas flow rate was 130 mL/min,and the discharge current was 27 mA.This method was combined with the univariate calibration model to quantitatively detect Cd and Pb in four different matrix soils.The linear correlation coefficients(R 2)of Cd and Pb were≥0.99 and>0.97,respectively.The relative errors of Cd and Pb measurement were 0.4%-11.8%.When the detection results were combined in the same calibration curve for analysis,the R 2 of Cd and Pb had slight change,and the relative errors of measurement were 3.0%-13.2%.Moreover,the limits of detection(LODs)for Cd and Pb in different matrix soils had not change significantly.The detection results of all the verification values were agreement with values of inductively coupled plasma-optical emission spectroscopy(ICP-AES).Overall,the detection results of Cd and Pb in complex matrix soils were less affected by matrix effects.

关 键 词：大气压辉光放电原子发射光谱 激光剥蚀 基质效应 镉 铅 

分 类 号：O657.31[理学—分析化学] X833[理学—化学]