偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱法测定土壤中14种成分  

Determination of 14 components in soil by inductively coupled plasma atomic emission spectrometry with lithium metaborate and lithium tetraborate fusion

作　　者：席秀丽 王生进[1] 高艳敏 刘春虎 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)

机构地区：[1]河北省地质矿产勘查开发局第九地质大队,河北邢台054000

出　　处：《冶金分析》2024年第4期65-72,共8页Metallurgical Analysis

摘　　要：准确测定土壤矿物质成分可以了解土壤肥力状况,有助于合理施肥、改善土壤质量。实验通过样品前处理条件的优化,建立了偏硼酸锂-四硼酸锂混合熔剂(m∶m=33∶67)熔融,盐酸-酒石酸提取,电感耦合等离子体原子发射光谱法(ICP-AES)测定土壤中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、K_(2)O、Na_(2)O、CaO、MgO、TiO_(2)、MnO、P_(2)O_(5)、Ba、V、Sr、Zr14项主要成分的测定方法。试验结果表明:熔剂与样品质量比为5∶1时熔融效果较好;使用盐酸-酒石酸为提取液可以抑制Ti、Zr水解;采用基体匹配法绘制校准曲线可消除基体效应的影响。14种成分校准曲线的线性相关关系均在0.999以上;各成分的检出限为0.32~39.27μg/g。采用实验方法测定土壤成分分析标准物质GBW07402,各成分测定值与认定值基本一致,相对误差(RE)为-0.43%~1.88%,相对标准偏差(RSD,n=6)为0.05%~3.7%;土壤实际样品分析结果的相对标准偏差(RSD,n=6)为0.15%~6.2%。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 SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),K_(2)O,Na_(2)O,CaO,MgO,TiO_(2),MnO,P_(2)O_(5),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 0.32-39.27μg/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%.

关 键 词：偏硼酸锂 四硼酸锂 碱熔 电感耦合等离子体原子发射光谱法(ICP-AES) 土壤 盐酸-酒石酸提取 

分 类 号：O657.31[理学—分析化学]