沸水提取-电感耦合等离子体发射光谱法测定土壤有效硼  

Determination of effective boron in soil by boiling water extraction with inductively coupled plasma emission spectrometry method

作　　者：万亚丽 徐辉 张立 赵小学 赵茜 王彦君 黄丽莉 谢楠 WAN Yali;XU Hui;ZHANG Li;ZHAO Xiaoxue;ZHAO Qian;WANG Yanjun;HUANG Lili;XIE Nan(Jiangsu Mineral Resources and Geological Design and Research Institute(Testing Center of China National Administration of Coal Geology),Key Laboratory of Coal measure mineral Resource of China National administration of coal geology,Xuzhou 221006,China;Henan Province Key Laboratory of Heavy-Metal Pollution Monitoring and Remediation,Jiyuan 459002,China)

机构地区：[1]江苏地质矿产设计研究院(中国煤炭地质总局检测中心),中国煤炭地质总局煤系矿产资源重点实验室,江苏徐州221006 [2]河南省土壤重金属污染监测与修复重点实验室,河南济源459002

出　　处：《化学分析计量》2024年第10期28-33,共6页Chemical Analysis And Meterage

基　　金：江苏省碳达峰碳中和科技创新专项项目(BE2023855);徐州市政策引导类计划(创新引领示范专项)项目(KC23381);江苏地质矿产设计研究院科研项目(JSY-2022-J01-1)。

摘　　要：建立了沸水提取-电感耦合等离子体发射光谱法测定土壤中有效硼。称取样品10.0 g,过250μm筛风干,置于石英三角瓶中,加入20.00 mL的提取剂(符合GB/T 6682规定的一级水,水中铁的质量浓度不大于10 mg/L),沸水浴浸10 min,回流冷凝5 min,滤液采用离心过滤,选择硼249.773 nm为分析谱线,用ICP-AES法测定土壤有效硼。经3种土壤标准物质和3种土壤样品验证,土壤有效硼质量浓度在0~2.0 mg/L范围内与光谱强度的线性关系良好,相关系数为0.9999,方法检出限为0.003 mg/kg,定量限为0.012 mg/kg,测定值的相对标准偏差为2.16%~6.46%(n=8),相对误差为1.01%~2.45%。当有效硼质量分数小于0.50 mg/kg时,测定值的最大偏差为0.05 mg/kg;当有效硼质量分数大于0.50 mg/kg时,测定值的最大偏差为0.06 mg/kg,标准物质测定值均在不确定度范围内。该方法检出限低,精密度和准确度较高,可操作性强,适用于批量土壤样品有效硼的测定,质量控制结果满足第三次全国农业土壤普查内业测试和全程质量控制规程的要求。A method was established for the determination of effective boron in soil by boiling water extraction and inductively coupled plasma emission spectrometry(ICP-AES).10.0 g of the sample was weighed,air dried hrough a 250μm sieve,placed in a quartz triangle bottle,and 20.00 mL of extractant(first-grade water complying with the regulations of GB/T 6682,with the concentration of iron in the water was not more than 10 mg/L)was added,and the extract was immersed in a boiling water bath for 10 min,then refluxed and condensed for 5 min,and then centrifugally filtered,with the boron 249.773 nm as the analytical spectral line for determining the effective boron in soil by the method of inductively coupled plasma emission spectrometry.ICP-AES was used to determine the effective boron in soil.After the validation of the three soil standards and three soil samples,the linear relationship between the mass concentration of soil effective boron and the spectral intensity was good in the range of 0-2.0 mg/L with the correlation coefficient of 0.9999.The detection limit of the method was 0.003 mg/kg,and the limit of quantification was 0.012 mg/kg,and the relative standard deviations of the measured values ranged from 2.16%to 6.46%(n=8),and the relative error was 1.01%-2.45%.When the effective boron mass fraction was less than 0.50 mg/kg,the maximum deviation of the determination value was 0.05 mg/kg;when the effective boron mass fraction was more than 0.50 mg/kg,the maximum absolute deviation of the determination value was 0.06 mg/kg,and the determination value of the standard substance was within the uncertainty range.The method has a low detection limit,high precision and accuracy,strong operability,and is suitable for the determination of effective boron in bulk soil samples,and the quality control results meet the requirements of the Third National Agricultural Soil Census for internal testing and the whole process of quality control procedures.

关 键 词：土壤 有效硼 电感耦合等离子体发射光谱法 沸水提取 

分 类 号：O657[理学—分析化学]