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1、第35卷第2期PreciousMetalsVol.35,No.2堿熔蒸餾分離-催化分光光度法測定超痕量鋨、釕來新澤1,王琳1*,牛娜2,王敏捷1,來克冰1(1.河南省巖石礦物測試中心國土資源部貴金屬分析與勘查技術(shù)重點實驗室,鄭州450012;2.遼寧省地質(zhì)礦產(chǎn)研究院,沈陽110032)摘要:研制了新型的鋨、釕混合氧化劑K2Cr2O7-NaBrO3和鋨稀釋劑As2O3-H2SO4,能夠降低堿熔蒸餾分離-催化分光光度法測定鋨、釕的全流程空白,提高了鋨、釕催化As3+-Ce4+體系的靈敏度。在35℃時,
2、通過延長反應時間,提高了方法的穩(wěn)定性和降低方法的檢測下線。使Os、Ru檢出限(3σ)分別達到0.010ng/g和0.012ng/g。改進后的蒸餾裝置使鋨、釕蒸餾的安全性和工作效率極大提高。方法操作簡便、效率高、成本低。測定國家鉑族元素地球化學一級標準物質(zhì)中的Os、Ru,相對誤差(RE)為-18.0%~+4.40%,12次測定的相對標準偏差(RSD)均小于20.1%,滿足地球化學調(diào)查樣品分析質(zhì)量要求。關(guān)鍵詞:分析化學;蒸餾分離;催化分光光度法;超痕量;鋨;釕中圖分類號:O657.32文獻標識碼:A文
3、章編號: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基金項目:國土資源部公益性行業(yè)科研專項經(jīng)費項目(201211081-03-34)。第一作者:來新澤,男,工程師,研究方向:貴金屬分析方法研究。E-mail:laixinze@126.com*通訊作者:王琳,女