Determination of zirconium,niobium,hafnium,tantalum,lithium, beryllium,vanadium,phosphorus,uranium and manganese in geological samples by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion
SUN Menghua, LI Xiaojing, WANG Wenjuan, WANG Xin*, YU Congling
1. Hebei Research Center for Geoanalysis, Baoding 071051, China; 2. Hebei Provincial Key Laboratory of Mineral Resources and Ecological Environment Monitoring, Baoding 071051, China
Abstract：The accurate determination of Zr, Nb, Hf, Ta, Li, Be, V, P, U and Mn in geological sample is beneficial to the study of geological environments such as geochemistry and petrogenesis. The sample was treated by alkali fusion with sodium peroxide and acidification with hydrochloric acid. 6Li was selected to correct Li and Be. 103Rh was selected to correct V, P, Zr, Nb and Mn. 185Re was selected to correct Ta, Hf and U. The method for determination of these elements in geological sample by inductively coupled plasma mass spectrometry (ICP-MS) was established. The sample fusion experiments showed that 0.100 0 g of geological sample could be fully fused by 1.0 g of sodium peroxide in muffle furnace at 750 ℃ for 8 min. The matrix interference tests showed that the mass concentration of Na+ in testing solution was less than 1.0 mg/mL after dilution for 10 times, and the interference caused could be ignored. The interference of major elements in sample including K, Ca, Fe, Mg and Al could be also ignored. The standing time of testing solution was optimized, which should be within 1 d. Under the optimized experimental conditions, the linear correlation coefficients of calibration curves for ten testing elements were all higher than 0.999. The limits of detection were between 0.10 μg/g and 2.64 μg/g. The limits of quantification were between 0.33 μg/g and 8.80 μg/g. The contents of Zr, Nb, Hf, Ta, Li, Be, V, P, U and Mn in certified reference materials of soil, stream sediments and rocks as well as actual samples were determined according to the experimental methods. The results showed that the determination results of certified reference materials were basically consistent with the certified values. The relative standard deviations (RSD) were not more than 4.8%, and the relative errors (RE) were not more than 5.1%. The RSDs of actual samples were all not more than 4.9%.
孙孟华, 李晓敬, 王文娟, 王昕, 于聪灵. 过氧化钠碱熔-电感耦合等离子体质谱法测定地质样品中锆铌铪钽锂铍钒磷铀锰[J]. 冶金分析, 2022, 42(1): 78-84.
SUN Menghua, LI Xiaojing, WANG Wenjuan, WANG Xin, YU Congling. Determination of zirconium,niobium,hafnium,tantalum,lithium, beryllium,vanadium,phosphorus,uranium and manganese in geological samples by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion. , 2022, 42(1): 78-84.
[1] 李冰,杨红霞.电感耦合等离子体质谱原理及应用[M].北京:地质出版社,2005. [2] 李晓敬,边朋沙,金倩,等.高压微波消解-电感耦合等离子体质谱法测定地质样品中分散元素镓铟铊锗碲镉[J].冶金分析,2019,39(4):38-44. LI Xiaojing,BIAN Pengsha,JIN Qian,et al.Determination of dispersed elements of gallium,indium,thallium,germanium,tellurium and cadmium in geological samples by inductively coupled plasma mass spectrometry with high-pressure microwave digestion[J].Metallurgical Analysis,2019,39(4):38-44. [3] 李霞雪,刘爱平,陈亚,等.微波消解-电感耦合等离子体质谱法测定蔬菜中铬、镉、砷、铅、汞的含量[J].理化检验(化学分册),2019,55(1):39-45. LI Xiaxue,LIU Aiping,CHEN Ya,et al.ICP-MS determination of chromium,cadmium,arsenic,lead and mercury in vegetables with microwave digestion of samples[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2019,55(1):39-45. [4] 金倩,李晓敬,陈庆芝,等.碱熔-强酸型阳离子交换树脂分离-电感耦合等离子体质谱法测定地质样品中硼锗钼锡碘钨[J].冶金分析,2020,40(7):52-59. JIN Qian,LI Xiaojing,CHEN Qingzhi,et al.Determination of boron,germanium,molybdenum,tin,iodine and tungsten in geological samples by alkaline fusion-strong acid cation exchange resin separation-inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2020,40(7):52-59. [5] 徐小梅,程庆兵,陈扣宝,等.电感耦合等离子体质谱法测定苦瓜药材中16种无机元素[J].化学分析计量,2019,28(6):60-65. XU Xiaomei,CHENG Qingbing,CHEN Koubao,et al.Determination of 16 inorganic elements in fructus momordicae charantiae by inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage,2019,28(6):60-65. [6] 申玉民,边朋沙,李晓敬,等.电感耦合等离子体质谱法测定地质样品中痕量铼[J].冶金分析,2018,38(12):7-12. SHEN Yumin,BIAN Pengsha,LI Xiaojing,et al.Determination of trace rhenium in geological samples by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2018,38(12):7-12. [7] 门倩妮,沈平,甘黎明,等.敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪[J].岩矿测试,2020,39(1):59-67. MEN Qianni,SHEN Ping,GAN Liming,et al.Determination of rare earth elements and Nb,Ta,Zr,Hf in polymetallic mineral samples by inductively coupled plasma-mass spectrometry coupled with open acid dissolution and lithium metaborate alkali fusion[J].Rock and Mineral Analysis,2020,39(1):59-67. [8] 刘环,康佳红,王玉.碱熔-电感耦合等离子体质谱法测定地质样品中铍铯镓铊铌钽锆铪铀钍[J].冶金分析,2019,39(3):26-32. LIU Huan,KANG Jiahong,WANG Yu.Determination of beryllium,cesium,gallium,thallium,niobium,tantalum,zirconium,hafnium,uranium and thurium in geological sample by inductively coupled plasma mass spectrometry with alkali fusion[J].Metallurgical Analysis,2019,39(3):26-32. [9] 郝冬梅,张翼明,许涛,等. ICP-MS法测定稀土铌钽矿中铍、铀、铌、钽、锆、铪量[J].稀土,2010,31(5):67-69. HAO Dongmei,ZHANG Yiming,XU Tao,et al.Determination of beryllium,uranium,niobium,tartalum,zirconium and hafnium in rare earth-niobium mineral by ICP-MS[J].Chinese Rare Earths,2010,31(5):67-69. [10] 程祎,李志伟,于亚辉,等.高压密闭消解-电感耦合等离子体质谱法测定地质样品中铌、钽、锆、铪和16种稀土元素[J].理化检验(化学分册),2020,56(7):782-787. CHENG Yi,LI Zhiwei,YU Yahui,et al.Determination of 16 kinds of rare earth elements,niobium,tartalum,zirconium and hafnium in geological sample by inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2020,56(7):782-787. [11] 郭爽,刘忠胜.碳酸钠-硼酸熔融酒石酸介质ICP-MS测定地质样品中铌、钽、锆、铪[J].吉林地质,2017,36(3):58-60. GUO Shuang,LIU Zhongsheng.Determination of niobium,tantalum,zirconium and hafnium in geological samples by sodium carbonate-boric acid fusion tartaric acid solution in ICP-MS[J].Jilin Geology,2017,36(3):58-60.
