岩矿测试
巖礦測試
암광측시
Rock and Mineral Analysis
2015年
5期
528-532
,共5页
杨珍%贺攀红%张延玲%孙银生%荣耀%张伟
楊珍%賀攀紅%張延玲%孫銀生%榮耀%張偉
양진%하반홍%장연령%손은생%영요%장위
含铀地质样品%微量铅%双毛细管%在线干扰校正%电感耦合等离子体发射光谱法
含鈾地質樣品%微量鉛%雙毛細管%在線榦擾校正%電感耦閤等離子體髮射光譜法
함유지질양품%미량연%쌍모세관%재선간우교정%전감우합등리자체발사광보법
geological samples with uranium%trace lead%double capillary%on-line interference correction%Inductively Coupled Plasma-Optimal Emission Spectrometry
应用电感耦合等离子体发射光谱法测定地质样品中的铅时,基体元素的干扰会使测量结果偏低。本文用氢氟酸、硝酸、高氯酸、盐酸溶解样品,采用等径双毛细管在线干扰校正的方法测定了含铀地质样品中的微量铅。首先通过双毛细管确定了样品溶液中的Fe、Al对铅有负干扰,而一定浓度的U、Ba、Ti、Ca、Mn、K、Mg、Na等基体元素没有干扰或可以忽略,由此在线双毛细管根据样品中Fe、Al的含量使用不同的校正试液建立标准曲线,测定未知样品时同步进行稀释,降低了Fe、Al的基体效应。方法检出限为1.5μg/g,精密度( RSD)小于5%。与普通干扰校正法相比,双毛细管在线干扰校正法可根据不同基体的样品使用不同的干扰校正试液,快速建立标准曲线进行复杂样品的测定,且避免了二次稀释,节省试剂,适合测定基体成分接近的批量样品。
應用電感耦閤等離子體髮射光譜法測定地質樣品中的鉛時,基體元素的榦擾會使測量結果偏低。本文用氫氟痠、硝痠、高氯痠、鹽痠溶解樣品,採用等徑雙毛細管在線榦擾校正的方法測定瞭含鈾地質樣品中的微量鉛。首先通過雙毛細管確定瞭樣品溶液中的Fe、Al對鉛有負榦擾,而一定濃度的U、Ba、Ti、Ca、Mn、K、Mg、Na等基體元素沒有榦擾或可以忽略,由此在線雙毛細管根據樣品中Fe、Al的含量使用不同的校正試液建立標準麯線,測定未知樣品時同步進行稀釋,降低瞭Fe、Al的基體效應。方法檢齣限為1.5μg/g,精密度( RSD)小于5%。與普通榦擾校正法相比,雙毛細管在線榦擾校正法可根據不同基體的樣品使用不同的榦擾校正試液,快速建立標準麯線進行複雜樣品的測定,且避免瞭二次稀釋,節省試劑,適閤測定基體成分接近的批量樣品。
응용전감우합등리자체발사광보법측정지질양품중적연시,기체원소적간우회사측량결과편저。본문용경불산、초산、고록산、염산용해양품,채용등경쌍모세관재선간우교정적방법측정료함유지질양품중적미량연。수선통과쌍모세관학정료양품용액중적Fe、Al대연유부간우,이일정농도적U、Ba、Ti、Ca、Mn、K、Mg、Na등기체원소몰유간우혹가이홀략,유차재선쌍모세관근거양품중Fe、Al적함량사용불동적교정시액건립표준곡선,측정미지양품시동보진행희석,강저료Fe、Al적기체효응。방법검출한위1.5μg/g,정밀도( RSD)소우5%。여보통간우교정법상비,쌍모세관재선간우교정법가근거불동기체적양품사용불동적간우교정시액,쾌속건립표준곡선진행복잡양품적측정,차피면료이차희석,절성시제,괄합측정기체성분접근적비량양품。
Measured lead contents in geological samples were commonly lower than real values because of matrix elements interference during Inductively Coupled Plasma-Optical Emission Spectrometry( ICP-OES )analyses. In this study,U-bearing geological samples were dissolved by hydrofluoric acid,nitric acid,perchloric acid,and hydrochloric acid. Trace lead was determined by ICP-OES with double capillary on-line interference correction. The interferences of matrix elements on lead were studied using double capillary. Fe and Al had negative interferences on lead,whereas a specific concentration of U,Ba,Ti,Ca,Mn,Mg,K and Na almost had no interferences on lead. The standard curve was established using double capillary according to the contents of Fe and Al in different test solution. The unknown sample was diluted simultaneously,which reduced the matrix effects of Fe and Al. The detection limit was 1. 5 μg/g,and the RSD was less than 5%. Compared with the common interference correction method,the double capillary on-line interference correction method can establish a standard curve quickly using different interference correction test solutions according to different matrices. Moreover,sample solution does not need to be secondly diluted,saving the reagent. This method is suitable for rapid determination of batch samples with similar matrices.