Abstract:During the determination of beryllium in soil by inductively coupled plasma atomic emission spectrometry (ICP-AES), the analytical lines of Be 313.042 nm and Be 313.107 nm are both interfered by partial spectral overlap from the characteristic spectral lines of Ti 313.079 nm and Nd 313.079 nm 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 313.042 nm and Be 313.107 nm as the analytical lines, respectively. The working parameters of ICP-AES were optimized: the radio-frequency power was 1 450 W, the nebulizer gas flow was 0.6 L/min, and the peristaltic pump speed was 1.6 mL/min. The mass fraction of beryllium in soil in range of 1.3-16.5 mg/kg had a good linear relationship with its corresponding emission intensity. The linear correlation coefficient were both 0.999 0. The limit of detection and limit of quantitation were both 0.02 mg/kg and 0.08 mg/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).
刘跃, 王记鲁, 王鑫, 林冬, 李静. 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[J]. 冶金分析, 2023, 43(9): 62-68.
LIU Yue, WANG Jilu, WANG Xin, LIN Dong, LI Jing. Determination of beryllium in soil by inductively coupled plasma atomic emission spectrometry with multi-component spectral fitting. , 2023, 43(9): 62-68.
[1] 骆金俊,李进,郁春辉.铍的致癌性和遗传毒性[J].微量元素与健康研究,2013,30(5):68-70. LUO Jinjun,LI Jin,YU Chunhui.Carcinogenicity and genotoxicity of beryllium[J].Studies of Trace Elements and Health,2013,30(5):68-70. [2] LIN Hailan,GAN Jie,YU Lei,et al.Determination of beryllium in soil and sediment by graphite furnace atomic absorption with a microwave-acid digestion method[J].Spectroscopy and Spectral Analysis,2015,35(11):3275-3280. [3] 林海兰,宋冰冰,朱日龙,等.微波酸溶-电感耦合等离子体质谱测定土壤和沉积物中Be2+[J].分析科学学报,2016,32(3):427-430. LIN Hailan,SONG Bingbing,ZHU Rilong,et al.Determination of beryllium in soil and sediment by ICP-MS with a microwave-acid digestion method[J].Journal of Analytical Science,2016,32(3):427-430. [4] 杨玮玮.磷酸加王水复溶-电感耦合等离子体质谱(ICP-MS)法测定土壤样品中的20种金属元素[J].中国无机分析化学,2021,11(5):81-85. YANG Weiwei.Determination of 20 metal elements in soil sample by ICP-MS with phosphoric acid and aqua regia[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(5):81-85. [5] 李星,姜云军,张宁,等.混合酸溶解-电感耦合等离子体原子发射光谱法测定土壤中17种元素[J].理化检验(化学分册),2019,55(3):291-296. LI Xing,JIANG Yunjun,ZHANG Ning,et al.Determination of 17 elements in soil by inductively coupled plasma atomic emission spectrometry after dissolution with mixed acid[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2019,55(3):291-296. [6] 张更宇,刘伟,崔世荣,等.分类消解-电感耦合等离子体原子发射光谱法测定环境土壤中15种金属元素的含量[J].理化检验(化学分册),2018,54(4):428-432. ZHANG Gengyu,LIU Wei,CUI Shirong,et al.Determination of 15 metal elements in environmental soil by inductively coupled plasma atomic emission spectrometry with classification degestion[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2018,54(4):428-432. [7] 迟清华,鄢明才.应用地球化学元素丰度数据手册[M].北京:地质出版社,2007. [8] 张亮亮,吴锐红,聂海明,等.干扰系数校正-电感耦合等离子体原子发射光谱法测定镍基合金中铈[J].冶金分析,2021,41(4):73-80. ZHANG Liangliang,WU Ruihong,NIE Haiming,et al.Determination of cerium in nickel-base alloy by inductively coupled plasma atomic emission spectrometry with interference coefficient correction[J].Metallurgical Analysis,2021,41(4):73-80. [9] 魏竞智,郭磊磊,李徐凤.石墨炉原子吸收光谱法和电感耦合等离子体发射光谱法测定土壤中铅和镉的方法比较[J].中国卫生检验杂志,2020,30(7):797-801. WEI Jingzhi,GUO Leilei,LI Xufeng.Comparison of graphite furnace atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry in the determination of Pb and Cd in soil[J].Chinese Journal of Health Laboratory Technology,2020,30(7):797-801. [10] 洪欣,王晓飞,苏荣,等.电感耦合等离子体原子发射光谱法测定河流和湖泊沉积物中11种重金属元素含量[J].理化检验(化学分册),2017,53(7):787-791. HONG Xin,WANG Xiaofei,SU Rong,et al.ICP-AES determination of 11 heavy metal elements in river and lake sediments[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2017,53(7):787-791. [11] 邹智敏,郭宏杰,马洪波,等.多元光谱拟合-电感耦合等离子体原子发射光谱法测定含铌镍基高温合金中铜[J].冶金分析,2016,36(8):78-82. ZOU Zhiming,GUO Hongjie,MA Hongbo,et al.Determination of copper in niobium-bearing nickel-based superalloy by multi-component spectral fitting-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(8):78-82. [12] 颜燕.两种干扰校正方式下电感耦合等离子体原子发射光谱法测定钼铝合金中硅的方法比较[J].冶金分析,2022,42(3):52-58. YAN Yan.Comparison of inductively coupled plasma atomic emission spectrometry for determination of silicon in molybdenum-aluminum alloy with two interference correction methods[J].Metallurgical Analysis, 2022,42(3):52-58. [13] 于英杰,李辉,张重远.多元谱线拟合-电感耦合等离子体原子发射光谱法测定钢中微量铌[J].冶金分析,2022,42(5):74-79. YU Yingjie,LI Hui,ZHANG Zhongyuan.Determination of trace niobium in steel by inductively coupled plasma atomic emission spectrometry with multi-component spectra fitting[J].Metallurgical Analysis,2022,42(5):74-79. [14] 严子心,曲景奎,余志辉,等.多谱线拟合-电感耦合等离子体原子发射光谱法测定高纯镍中痕量钴[J].分析化学,2019,47(3):423-428. YAN Zixin,QU Jingkui,YU Zhihui,et al.Multi-spectral fitting-determination of trace cobalt in high purity nickel by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Analytical Chemistry,2019,47(3):423-428.