二苯硫脲泡塑富集一原子吸收光谱法连续测定化探样品中金和银.pdf

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1、2012年l0月岩矿测试Vo1．31．No．5October2012R0CKANDMINERALANALYSIS829～833文章编号：0254—5357(2012)05—0829—05苯硫脲泡塑富集一原子吸收光谱法连续测定化探样品中金和银孙文军(河南省地质矿产勘查开发局第一地质调查队实验室，河南洛阳471023)摘要：传统的发射光谱、化学光谱、泡塑富集分离一原子吸收光谱法测定化探样品中的金和银，分析结果不稳定，效率低。本研究提出用50％的王水分解化探样品，负载二苯硫脲泡塑吸附金银，石墨炉和火焰原子吸收

2、光谱法对金和银进行联合测定。在二苯硫脲浓度、吸附酸度、吸附温度、振荡时间等优化的实验条件下，金和银的回收率分别达到97．9％和98．8％，检出限为0．25ng／g和0．038g／g，准确度(RE，n=9)为2．0％～14．0％和7．7％～13．3％，精密度(RSD，n=9)为3．1％～12．4％和5．1％～13．2％。经国家标准物质分析验证，测定值与标准值基本相符。该方法实现了在同一份溶液中同时测定金和银，与现行的石墨炉原子吸收光谱测定金、发射光谱测定银的方法相比，称样量达到10g，样品的代表性显著增加

3、，提高了准确度和精密度，简化了金银分析的程序，化学试剂用量少，分析成本低。关键词：化探样品；金；银；二苯硫脲泡塑；分离富集；石墨炉原子吸收光谱法中图分类号：O614．123；O614．122；0657．31文献标识码：BContinuousDeterminationofGoldandSilverinGeochemicalSamplesbyAtomicAbsorptionSpectrometryConcentratedbyLoadDiphenylthi0ureaFoamSUNWen-jun(TheLabo

4、ratoryoftheFirstGeologicalSurveyTeam，HennanGeologicalExplorationBureau，Luoyang471023，China)Abstract：Theresultsofanalysisbythetraditionalmethodsofgoldandsilverdeterminationingeochemicalsamplesbyemissionspectrometry，chemicalspectroscopyoratomicabsorptionsp

5、ectrometryconcentratedbyloadfoam，isunstableandineficient．Asreportedinthispaper，thesampleshavebeendecomposedby50％aquaregia．AuandAgwereconcentratedbyloadeddipheny1thioureafoamwhichwascleanedwithdeionizedwater．ThetraceamountsofAuandAgwerethensimultaneouslym

6、easuredbyusingGraphiteFurnaceAtomicAbsorptionSpectrophotometry(GFAAS)andFlameAtomicAbsorptionSpectrophotometry(FAAS)．Theexperimentalconditionswereoptimizedbyusingaconcentrationofdiphenylthioureaof7mg／mL。hydrochloricacidconcentrationof8％．oscillationtimeof

7、25minandabsorptiontemperatureof20~C．TherecoveriesofAuandAgwere97．9％and98．8％respectively．Aftertheimprovement，thedetectionlimitsofAuandAgwere0．25ng／gand0．038grespectively，relativeerrorswere2．0％一14．0％and7．7％一13．3％(n=9)，RSDswere3．1％一12．4％and5．1％一13．2％respect

8、ively(n=9)byusingthismethod．Themethodhasbeenverifiedbydeterminationofnationalfirstlevelstandardmaterialwithsatisfactoryresults．ThismethodresolvessimultaneousdeterminationofAuandAginonesolution．ComparedwithdeterminationofAg