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《電感耦合等離子體原子發(fā)射光譜法測(cè)定純銀中鎘_鉍_鐵_鉛_銻_鈀_硒_碲》由會(huì)員上傳分享,免費(fèi)在線閱讀,更多相關(guān)內(nèi)容在行業(yè)資料-天天文庫(kù)。
1、電感耦合等離子體原子發(fā)射光譜法測(cè)定純銀中鎘、鉍、鐵、鉛、銻、鈀、硒、碲張光華(北方銅業(yè)股份有限公司計(jì)量檢驗(yàn)部中心化驗(yàn)室山西垣曲043700)摘要樣品用硝酸溶解,加入過(guò)量鹽酸沉淀分離銀,過(guò)濾后利用電感耦合等離子體原子發(fā)射光譜法測(cè)定鎘、鉍、鐵、鉛、銻、鈀、硒、碲,方法檢出限分別為:0.0028,0.0075,0.0036,0.011,0.010,0.021,0.0075,0.0039μg/mL;加標(biāo)回收率為98.1%~114.3%;RSD小于4.2%,方法能同時(shí)準(zhǔn)確測(cè)定鎘、鉍、鐵、鉛、銻、鈀、硒、碲,滿足日常分析要求。關(guān)鍵詞純銀;電感耦合等離子體原子發(fā)射光
2、譜法;鎘;鉍;鐵;鉛;銻;鈀;硒;碲中圖分類號(hào):O657.31;TH744.11文獻(xiàn)標(biāo)志碼:A文章編號(hào):2095-1035(2013)02-0063-03DeterminationofCd,Bi,Fe,Pb,Sb,Pd,Se,TeinSilverbyInductivelyCoupledPlasma-AtomicEmissionSpectrometryZHANGGuanghua(TheCentralTestingLaboratory,MetrologyandInspectionDepartmentofNorthernCopperIndustrialCo.
3、,Ltd.,Yuanqu,Shanxi043700,China)AbstractThesamplewasdissolvedbynitricacid.Thensilverinthesolutionwasprecipatedduetotheadditionofexcessivehydrochloricacidandthusseparatedfromthesolution.Afterfiltrationthecontentsofcadmium,bismuth,iron,lead,antimony,selenium,telluriumpalladiumwere
4、determinedbyinductivelycoupledplasmaatomicemissionspectroscopy(ICP-AES).Thedetectionlimitofthemethodforcadmium,bismuth,iron,lead,antimony,selenium,telluriumandpalladiumwere0.0028,0.0075,0.0036,0.011,0.010,0.021,0.0075,0.0039μg/mL,respectively.Therecoveriesrangefrom98.1%to114.3%;
5、Therelativestandarddeviation(RSD)islessthan4.2%.Themethodcanbeusedtosimultaneouslyandaccuratelydeterminecadmium,bismuth,iron,lead,antimony,selenium,telluriumandpalladium,thusmeetthedailyanalysisrequirement.sterlingsilver;inductivelycoupledplasma-atomicemissionspectrometry;cadmiu
6、m;bismuth;iron;lead;antimony;palladium;selenium;telluriumKeywords鑭富集雜質(zhì)元素與基體分離,原子吸收光譜法[2],以上方法或需要基體匹配或檢出限太高。近年來(lái),電感耦合等離子體原子發(fā)射光譜法因其檢出限低、測(cè)定范圍寬廣、靈敏度高、能同時(shí)測(cè)多種元素[3],已廣泛應(yīng)用于環(huán)境、冶金、地質(zhì)、生物等樣品分析[4-6]。前言鎘、鉍、鐵、鉛、銻、鈀、硒、碲是純銀中主要雜質(zhì)元素,對(duì)于純銀中的鎘、鉍、鐵、鉛等雜質(zhì)元素的測(cè)定有直讀光譜法[1],還有利用氯化銀沉淀分離、氫氧化0收稿日期:2013-02-07修回日期
7、:2013-03-15作者簡(jiǎn)介:張光華,男,高級(jí)工程師,主要從事計(jì)量檢驗(yàn)研究工作。E-mail:mlj721106032@sina.com中國(guó)無(wú)機(jī)分析化學(xué)2013年64采用鹽酸沉淀分離銀,電感耦合等離子體原子發(fā)射光譜法測(cè)定純銀中鎘、鉍、鐵、鉛、銻、鈀、硒、碲,能夠同時(shí)測(cè)定且檢出限很低,滿足純銀中雜質(zhì)元素的分析。熱電公司)。硝酸、鹽酸為優(yōu)級(jí)純,鎘、鉍、鐵、鉛、銻、鈀、硒、碲標(biāo)準(zhǔn)儲(chǔ)備溶液(1mg/mL,國(guó)家標(biāo)準(zhǔn)物質(zhì)研究中心)。混合標(biāo)準(zhǔn)溶液(0.1mg/mL):分別移取上述標(biāo)準(zhǔn)溶液10mL于100mL容量瓶中,加5mL鹽酸用蒸餾水定容,混勻。經(jīng)過(guò)分別改變儀器
8、的各參數(shù)進(jìn)行實(shí)驗(yàn),確定了儀器的工作條件,見(jiàn)表1。實(shí)驗(yàn)部分儀器與試劑ICP-6300電感耦合等離