Determination of 14 components in soil by inductively coupled plasma atomic emission spectrometry with lithium metaborate and lithium tetraborate fusion
XI Xiuli, WANG Shengjin, GAO Yanmin, LIU Chunhu
The Ninth Geological Brigade of Hebei Bureau of Geology and Mineral Exploration and Development,Xingtai 054000,China
Abstract：The accurate determination of mineral components in soil can know the soil fertility status,and is helpful for the reasonable fertilization and improvement of soil quality.Through the optimization of sample pretreatment conditions,the fusion method with mixed flux of lithium metaborate and lithium tetraborate(m∶m=33∶67) was established.After extraction with hydrochloric acid and tartaric acid,the determination method of 14 components in soil(including SiO2,Al2O3,Fe2O3,K2O,Na2O,CaO,MgO,TiO2,MnO,P2O5,Ba,V,Sr and Zr) by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established. The results showed that the fusion effect was good when the mass ratio of flux and sample was 5∶1.The extractant of hydrochloric acid-tartaric acid could inhibit the hydrolysis of Ti and Zr.The matrix matching method was used to draw the calibration curve to eliminate the influence of matrix effect.The linear correlation coefficients of calibration curves for 14 components were all above 0.999,and the limits of detection were in the range of 0.32-39.27 μg/g.The certified reference material of soil for composition analysis(GBW07402) was determined according to the experimental method,and the found results of each component were basically consistent with the certified values.The relative errors(RE) were in the range of -0.43%-1.88%,and the relative standard deviations(RSDs, n=6) were in the range of 0.05%-3.7%.The proposed method was applied to the analysis of soil sample,and the RSDs(n=6) of the measurement results were between 0.15% and 6.2%.
[1] 黄昌勇,徐建明.土壤学[M].4版.北京:中国农业出版社,2019:27-28. [2] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 14506.3~14506.11—2010硅酸盐岩石化学分析方法[S].北京:中国标准出版社,2010. [3] 刘凤枝,李玉浸.土壤监测分析技术[M].北京:化学工业出版社,2015:386-392. [4] 吕胜男,卢兵,赵文志,等.X射线荧光光谱法同时测定土壤和水系沉积物中23种主次痕量组分[J].理化检验(化学分册),2023,59(7):764-770. LÜ Shengnan,LU Bing,ZHAO Wenzhi,et al.Simultaneous determination of 23 major,minor and trace components in soil and stream sediment by X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2023,59(7):764-770. [5] 胡梦颖,张鹏鹏,刘彬,等.高压制样-激光诱导击穿光谱技术测定土壤中的硅铝铁钾[J].光谱学与光谱分析,2023,43(7):2174-2180. HU Mengying,ZHANG Pengpeng,LIU Bin,et al.Determination of Si,Al,Fe,K in soil by high pressure pelletised sample and laser-induced breakdown spectroscopy[J].Spectroscopy and Spectral Analysis,2023,43(7):2174-2180. [6] 王佳翰,李正鹤,杨峰,等.偏硼酸锂碱熔-电感耦合等离子体质谱法同时测定海洋沉积物中48种元素[J].岩矿测试,2021,40(2):306-315. WANG Jiahan,LI Zhenghe,YANG Feng,et al.Simultaneous determination of 48 elements in marine sediments by ICP-MS with lithium metaborate fusion[J].Rock and Mineral Analysis,2021,40(2):306-315. [7] 李华昌,符斌.化验员手册[M].北京:化学工业出版社,2020:117-120. [8] 冯旭,宋晓红,段伟亚,等.双向观测电感耦合等离子体发射光谱法测定土壤中的常微量元素[J].环境化学,2015,34(1):200-201. FENG Xu,SONG Xiaohong,DUAN Weiya,et al.Determination of trace elements in soil by inductively coupled plasma emission spectrometry[J].Environmental Chemistry,2015,34(1):200-201. [9] 孙红宾,刘贵磊,赵怀颖,等.偏硼酸锂熔融-ICP-AES法测定含刚玉铝土矿中主成分[J].分析试验室,2017,36(12):1429-1434. SUN Hongbin,LIU Guilei,ZHAO Huaiying,et al.Determination of main components in corundum-bearing bauxite by ICP-AES with lithium metaborate fusion method[J].Chinese Journal of Analysis Laboratory,2017,36(12):1429-1434. [10] 蒲雪萍.复合熔剂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定萤石中钾、钠、硅、铁、磷[J].中国无机分析化学,2019,9(3):28-32. PU Xueping.Determination of K,Na,Si,Fe,and P in fluorite by composite flux melting inductively coupled plasma atomic emission spectrometry(ICP-AES)[J].Chinese Journal of Inorganic Analytical Chemistry,2019,9(3):28-32. [11] 张丽萍,孙启亮,姚明星,等. 偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定石膏中多组分含量[J].中国无机分析化学,2023,13(7):741-747. ZHANG Liping,SUN Qiliang,YAO Mingxing,et al.Determination of multi-component content in gypsum by inductively coupled plasma atomic emission spectrometry with lithium metaborate-lithium tetraborate fusion[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(7):741-747. [12] 封亚辉, 潘生林, 查燕青,等.波长色散X射线荧光光谱法测定钽铁和铌铁矿中钽铌铀钍[J].冶金分析,2022,42(3):7-12. FENG Yahui,PAN Shenglin,ZHA Yanqing,et al.Determination of tantalum,niobium,uranium and thorium in tantalite and niobite by wavelength dispersive X-ray fluorescence spectrometry[J].Metallurgical Analysis,2022,42(3):7-12. [13] 罗海霞,王强.微波消解-电感耦合等离子体原子发射光谱法测定钴铬钨系合金粉末中钨[J].冶金分析,2022,42(2):40-46. LUO Haixia,WANG Qiang.Determination of tungsten in cobalt-chromium-tungsten alloy powder by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Metallurgical Analysis,2022,42(2):40-46. [14] 岩石矿物分析编委会.岩石矿物分析:第2分册[M].4版.北京:地质出版社,2011:4-6. [15] 李贤珍,高小飞,姚明星,等.电感耦合等离子体发射光谱法测定黑钨矿精矿和中矿中的锰[J].岩矿测试,2012,31(3):438-441. LI Xianzhen,GAO Xiaofei,YAO Mingxing,et al.Determination of Mn in black tungsten concentration and middling products by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2012,31(3):438-441. [16] 王龙山,郝辉,王光照,等.偏硼酸锂熔矿-超声提取-电感耦合等离子体发射光谱法测定岩石水系沉积物土壤样品中硅铝铁等10种元素[J].岩矿测试,2008,27(4):287-290. WANG Longshan,HAO Hui,WANG Guangzhao,et al.Determination of 10 elements including silicon,aluminum,iron in rock,stream sediment and soil samples by ICP-AES with lithium metaborate fusion and ultrasonic extraction[J].Rock and Mineral Analysis,2008,27(4):287-290. [17] 王力强,王家松,吴良英,等.偏硼酸锂熔融-电感耦合等离子体原子发射光谱法测定锆矿石中10种元素[J].冶金分析,2020,40(9):63-69. WANG Liqiang,WANG Jiasong,WU Liangying,et al.Determination of W,Mo and other elements in tungsten-molybdenum ores by inductively coupled plasma atomic emission spectrometry with lithium metaborate fusion[J].Metallurgical Analysis,2020,40(9):63-69. [18] 武汉大学.分析化学[M].6版.北京:高等教育出版社,2018:154-155. [19] ]王力强,王家松,魏双,等.偏硼酸锂熔融-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼及11种伴生元素[J].岩矿测试,2021,40(5):688-697. WANG Liqiang,WANG Jiasong,WEI Shuang,et al.Determination of W,Mo and 11 other elements in tungsten-molybdenum ores by inductively coupled plasma optical emission spectrometry with lithium metaborate fusion[J].Rock and Mineral Analysis,2021,40(5):688-697. [20] 曹磊,陈微微,高孝礼,等.基体干扰对ICP-AES分析土壤样品中主、次量元素的影响研究[J].光谱学与光谱分析,2016,36(7):2260-2265. CAO Lei,CHEN Weiwei,GAO Xiaoli,et al.Research on the matrix interference on major and minor elements in soil samples with ICP-AES[J].Spectroscopy and Spectral Analysis,2016,36(7):2260-2265. [21] 金一,安帅,宋丽华.偏硼酸锂熔融-电感耦合等离子体光谱法和质谱法测定东北黑土中32种特征成分的含量[J].理化检验(化学分册),2021,57(12):1074-1081. JIN Yi,AN Shuai,SONG Lihua.Determination of 32 characteristic components in the black soil from Northeast China by inductively coupled plasma spectroscopy and mass spectrometry after melting with lithium metaborate[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2021,57(12):1074-1081.
