酸碱两种方法消解-电感耦合等离子体发射光谱法(ICP-AES)分析空气滤膜样品中的19种元素  

Analysis of nineteen elements in air filter membrane samples by inductively coupled plasma atomic emission spectroscopy(ICP-AES)with acid-and alkali-dissolution

作　　者：乔爱香[1] 江冶[1] 李如燕 曹磊[1] 袁秀雪 Qiao Aixiang;Jiang Ye;Li Ruyan;Cao Lei;Yuan Xiuxue(Geological Survey of Jiangsu Province,Nanjing 210018,Jiangsu,China)

机构地区：[1]江苏省地质调查研究院,江苏南京210018

出　　处：《地质学刊》2022年第4期441-446,共6页Journal of Geology

基　　金：国家重点研发计划项目“典型矿产标准物质研制”(2016YFF020110303)。

摘　　要：特氟龙空气滤膜试样用反王水浸泡预消解,电热板加热,反王水-高氯酸-氢氟酸四酸体系分解滤膜样品吸附的空气颗粒物。在无合适监控样品的情况下,采用国家一级标准物质GBW07401模拟滤膜吸附的空气颗粒物与空白滤膜一起消化分解、上机测定,优化ICP-AES光谱仪的最佳测试条件,分析样品中的Ba、Cr、Cu、Li、Mn、Ni、P、Pb、Sr、Ti、V、Zn、Al、Ca、Fe、K、Mg、Na共18种元素,测定值与标准物质的认定值相符,各元素分析结果的相对标准偏差RSD在1.42%~9.21%之间,方法回收率在89%~112%之间,元素检出限在0.0020~0.35μg/g之间。滤膜中的Si元素测定采用微波马弗炉碱熔法,水提取酸化定容,同步采用国家一级标准物质GBW03105a模拟空气颗粒物样品加入空白滤膜,灰化碱熔,进行ICP-AES测定。相对标准偏差RSD为7.68%,检出限为0.12μg/g。采用酸溶法和碱熔法2种方法分解样品,实现了空气滤膜样品中19个多元素的快速测定。The samples of Teflon air filter membrane were pre-digested by soaking in reverse aqua regia,heated by electric heating plate,and the air particles adsorbed by air filter membrane samples were decomposed by the system of reverse aqua regia,perchloric acid and hydrofluoric acid.In the absence of suitable monitoring samples,the national standard material GBW07401 was used to simulate the digestion and decomposition of air particles adsorbed by the filter membrane and the blank filter membrane,and the test conditions of ICP-AES spectrometer were optimized.A total of 18 elements(Ba,Cr,Cu,Li,Mn,Ni,P,Pb,Sr,Ti,V,Zn,Al,Ca,Fe,K,Mg,Na)were analyzed in the samples.The measured values are consistent with the recognized values of the reference materials,and the relative standard deviations of each element are from 1.42%to 9.21%.The recovery rate ranges from 89%to 112%,and the detection limits are from 0.0020μg/g to 0.35μg/g.The Si element in the filter membrane was determined by microwave Muffle furnace alkaline melting method,and then was extracted,acidized and set to constant volume.The national standard material GBW03105a was used to simulate the air particulate samples and was added to the blank filter membrane,and the ash alkali melting was performed for ICP-AES determination.The relative standard deviation(RSD)is 7.68%,and the detection limit is 0.12μg/g.The rapid determination of 19 elements in the air filter membrane samples is achieved by two methods:acid dissolution and alkali dissolution.

关 键 词：电感耦合等离子体发射光谱法 特氟龙滤膜 多元素 四酸 碱熔 电热板 

分 类 号：P575.4[天文地球—矿物学]