多元谱线拟合-电感耦合等离子体原子发射光谱法测定土壤中铍  

Determination of beryllium in soil by inductively coupled plasma atomic emission spectrometry with multi-component spectral fitting

作　　者：刘跃 王记鲁 王鑫 林冬 李静 LIU Yue;WANG Jilu;WANG Xin;LIN Dong;LI Jing(Tianjin Eco-Environmental Monitoring Center,Tianjin 300191,China)

机构地区：[1]天津市生态环境监测中心,天津300191

出　　处：《冶金分析》2023年第9期62-68,共7页Metallurgical Analysis

摘　　要：采用电感耦合等离子体原子发射光谱法(ICP-AES)测定土壤中铍时,选择Be 313.042 nm和Be 313.107nm为分析谱线,均会受到基体钛和铌的特征谱线Ti 313.079nm和Nd 313.079nm的部分光谱重叠干扰,从而导致很难准确测定铍的含量。实验采用盐酸、硝酸、氢氟酸和高氯酸处理样品,选择Be 313.042nm和Be 313.107nm作为分析谱线,选用多元光谱拟合(MSF)校正光谱干扰,建立了ICP-AES测定土壤中铍的方法。对ICP-AES工作条件进行了优化,选择射频功率为1450W、雾化气流量为0.6L/min,蠕动泵转速为1.6mL/min。土壤中铍质量分数在1.3~16.5mg/kg范围内与其发射强度呈线性关系,线性相关系数均为0.9990;方法检出限均为0.02mg/kg,定量限均为0.08mg/kg。按照实验方法对土壤标准物质中铍进行测定,测定值在认定值允许的范围内,相对标准偏差(RSD,n=6)为0.7%~3.7%。按照实验方法对土壤样品进行测定,测定值的相对标准偏差(n=6)为1.3%~3.6%;t检验法结果表明,实验方法测定值与电感耦合等离子体质谱法(ICP-MS)无显著性差异。During the determination of beryllium in soil by inductively coupled plasma atomic emission spec trometry(ICP-AES),the analytical lines of Be 313.042nm and Be 313.107nm are both interfered by partial spectral overlap from the characteristic spectral lines of Ti 313.079nm and Nd 313.079nm for the matrix of titanium and niobium.As a result,it is difficult to determine the content of beryllium accurately.The samples were treated with hydrochloric acid,nitric acid,hydrofluoric acid and perchloric acid.Then the spectral interference was corrected by Multi-component Spectral Fitting(MSF).Consequently,an analysis method for determination of beryllium in soil was established by ICP-AES with Be 313.042nm and Be 313.107nm as the analytical lines,respectively.The working parameters of ICP-AES were optimized:the radio-frequency power was 1450W,the nebulizer gas flow was 0.6L/min,and the peristaltic pump speed was 1.6mL/min.The mass fraction of beryllium in soil in range of 1.3-16.5mg/kg had a good linear relationship with its corresponding emission intensity.The linear correlation coefficient were both 0.9990.The limit of detection and limit of quantitation were both 0.02mg/kg and 0.08mg/kg,respectively.The content of beryllium in certified reference materials of soil were determined according to the proposed method.The results were within allowable range of the certified values,and the relative standard deviations(RSD,n=6)were between 0.7%and 3.7%.The content of beryllium in soil samples were determined according to the proposed method,the relative standard deviations(n=6)were between 1.3%and 3.6%.The t-test results showed that there was no significant difference between the results determined by the proposed method and inductively coupled plasma mass spectrometry(ICP-MS).

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 土壤 铍 多元谱线拟合(MSF) 

分 类 号：O657.31[理学—分析化学] X833[理学—化学]