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1、第35卷第2期PreciousMetalsVol.35,No.2碱熔蒸馏分离-催化分光光度法测定超痕量锇、钌来新泽1,王琳1*,牛娜2,王敏捷1,来克冰1(1.河南省岩石矿物测试中心国土资源部贵金属分析与勘查技术重点实验室,郑州450012;2.辽宁省地质矿产研究院,沈阳110032)摘要:研制了新型的锇、钌混合氧化剂K2Cr2O7-NaBrO3和锇稀释剂As2O3-H2SO4,能够降低碱熔蒸馏分离-催化分光光度法测定锇、钌的全流程空白,提高了锇、钌催化As3+-Ce4+体系的灵敏度。在35℃时,
2、通过延长反应时间,提高了方法的稳定性和降低方法的检测下线。使Os、Ru检出限(3σ)分别达到0.010ng/g和0.012ng/g。改进后的蒸馏装置使锇、钌蒸馏的安全性和工作效率极大提高。方法操作简便、效率高、成本低。测定国家铂族元素地球化学一级标准物质中的Os、Ru,相对误差(RE)为-18.0%~+4.40%,12次测定的相对标准偏差(RSD)均小于20.1%,满足地球化学调查样品分析质量要求。关键词:分析化学;蒸馏分离;催化分光光度法;超痕量;锇;钌中图分类号:O657.32文献标识码:A文
3、章编号:1004-0676(2014)02-0050-09DeterminationofUltraTraceOsmiumandRutheniumbyAlkalineFusionDistillationSeparation-CatalyticSpectrophotometricMethodLAIXinze1,WANGLin1*,NIUNa2,WANGMinjie1,LAIKebing1(1.HenanRockMineralTestingCenters,KeyLabofMinistryofLandan
4、dResourcesAnalysisandExplorationofPreciousMetals,Zhenzhou450012,China;2.TheGeologyMineralInstituteforResearchofLiaoningProvince,Shenyang110032,China)Abstract:BydevelopinganewtypemixedoxidantofOsandRu,K2Cr2O7-NaBrO3anddiluentAs2O3-H2SO4ofOs,thefullproc
5、edureblankinthedeterminationofRuandOsbyalkalifusiondistillationseparation-catalyticspectro-photometricmethodwasreduced,andthesensitivitiesofOs,RuinAs3+-Ce4+catalyticsystemwereimproved.Thestabilityofthemethodwasimprovedandthedetectionlimitwasreducedbyp
6、rolongingthereactiontimeat35℃.Detectedlimits(3σ)ofOsandRuwere0.010ng/gand0.012ng/g,respectively.Theresultsshowedthatthesafetyandefficiencyofdistillationweregreatlyimprovedbyimprovethedistillationdevice.Themethodissimpleoperation,highefficiencyandlowco
7、st.ThemethodwasappliedtomeasureOsandRuinNationalPGEgeochemistrystandardsubstance.Therelativeerror(RE)was-18.0%~+4.40%,andtherelativestandarddeviation(RSD)of12-timesresultswaslessthan20.1%.Themethodcouldmeettheanalysisqualityrequirementsofgeochemicalsu
8、rveysample.Keywords:analyticalchemistry;distillationseparation;catalyticspectrophotometricmethod;ultratrace;osmium;ruthenium收稿日期:2013-07-15基金项目:国土资源部公益性行业科研专项经费项目(201211081-03-34)。第一作者:来新泽,男,工程师,研究方向:贵金属分析方法研究。E-mail:laixinze@126.com*通讯作者:王琳,女