干法灰化-发射光谱法测定植物样品中B和Sn  

Determination of B,Sn in Plant Samples by Emission Spectrometry with Dry Ashing

作　　者：郝志红[1,2] 刘彬 杜雪苗[1,2] 陈卫明 唐瑞玲[1,2] 胡梦颖[1,2] 朱文静 徐进力[1,2] HAO Zhihong;LIU Bin;DU Xuemiao;CHEN Weiming;TANG Ruiling;HU Mengying;ZHU Wenjing;XU Jinli(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang,Hebei 065000,China;UNESCO International Centre on Global-Scale Geochemistry,Langfang,Hebei 065000,China;Regional Geology Survey Institute of Hebei Province,Langfang,Hebei 065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000 [2]联合国教科文组织全球尺度地球化学国际研究中心,河北廊坊065000 [3]河北省区域地质调查院,河北廊坊065000

出　　处：《中国无机分析化学》2023年第12期1437-1443,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：地质大调查项目(DD20230121,DD20221770)。

摘　　要：一般土壤样品中的元素硼和锡属于难溶易挥发元素,湿法样品前处理技术相对较难,基本以一米光栅发射光谱法测定为主,其固体进样方式可以避免复杂的样品前处理,实现对地质样品中元素硼和锡的绿色分析。通过研究内标法、截取曝光时间、背景扣除、重叠摄谱等技术,同时考察干法灰化的温度对测定结果的影响,针对特殊植物样品,将样品在马弗炉中450℃的高温条件下灰化60 min,体积和质量均产生富集并制备成灰分,称取样品灰分成分和基准物、缓冲剂(比例1∶1∶2)经过研磨充分混匀,使其基体成分保持一致,在优化的实验条件下,以国家一级合成硅酸盐光谱分析标准物质制作校准曲线,构建植物样品中硼和锡的分析方法。结果表明:硼和锡的检出限分别为0.042、0.019μg/g;方法经过国家一级标准物质验证,硼方法精密度5.6%~13.0%,正确度(RE)的绝对值均小于10%;锡方法精密度7.2%~18%,正确度(RE)的绝对值均小于28%。植物样品经过干法灰化富集后,对植物样品中元素硼基本能够实现精准测定,对元素锡含量接近于检测下限值的测定结果相对较差,对高含量值也能够实现精准测定,方法具有较好的推广应用价值。The elements of boron and tin in most of soil samples are insoluble and volatile elements.It is relatively difficult to determine their content by wet sample pretreatment technology.At present,it is mainly determined by one-meter grating emission spectrometry.The solid injection method avoids complex sample pretreatment and realizes green analysis of element boron and tin in geochemical samples.The sample was ashed in a high-temperature furnace at 450℃for 60 minutes,and the volume and mass were all enriched which could be prepared into ash.The ash components of the samples,the base material and the buffer(the ratio was 1∶1∶2)were fully mixed after grinding,keeping their matrix composition consistent,and then under the optimized experimental conditions,the calibration curve was made by using the certified reference materials of synthetic silicate for spectral analysis,and finally the analysis method of boron and tin in plant samples was established.The detection limits of boron and tin were 0.042 and 0.019μg/g,respectively.According to the verification of the certified reference materials,the method precision of boron was 5.6%—13.0%,and the absolute value of accuracy(RE)was less than 10%.At the same time,the method precision of tin was 7.2%—18%,and the absolute value of accuracy(RE)was less than 28%.The experimental results showed that after dry ashing and enrichment of plant samples,the element boron in the plant samples could be accurately determined.The determination results of the element tin content in the sample close to the lower limit of detection were relatively poor,while the high content value could be accurately determined,indicating that the method has good application value.

关 键 词：干法灰化 发射光谱 植物样 硼 锡 

分 类 号：O657.31[理学—分析化学] TH744.12[理学—化学]