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时间:2018-07-27
《电感耦合等离子体原子发射光谱法测定纯银中镉_铋_铁_铅_锑_钯_硒_碲》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
1、电感耦合等离子体原子发射光谱法测定纯银中镉、铋、铁、铅、锑、钯、硒、碲张光华(北方铜业股份有限公司计量检验部中心化验室山西垣曲043700)摘要样品用硝酸溶解,加入过量盐酸沉淀分离银,过滤后利用电感耦合等离子体原子发射光谱法测定镉、铋、铁、铅、锑、钯、硒、碲,方法检出限分别为:0.0028,0.0075,0.0036,0.011,0.010,0.021,0.0075,0.0039μg/mL;加标回收率为98.1%~114.3%;RSD小于4.2%,方法能同时准确测定镉、铋、铁、铅、锑、钯、硒、碲,满足日常分析要求。关键词纯银;电感耦合等离子体原子发射光
2、谱法;镉;铋;铁;铅;锑;钯;硒;碲中图分类号:O657.31;TH744.11文献标志码:A文章编号: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镧富集杂质元素与基体分离,原子吸收光谱法[2],以上方法或需要基体匹配或检出限太高。近年来,电感耦合等离子体原子发射光谱法因其检出限低、测定范围宽广、灵敏度高、能同时测多种元素[3],已广泛应用于环境、冶金、地质、生物等样品分析[4-6]。前言镉、铋、铁、铅、锑、钯、硒、碲是纯银中主要杂质元素,对于纯银中的镉、铋、铁、铅等杂质元素的测定有直读光谱法[1],还有利用氯化银沉淀分离、氢氧化0收稿日期:2013-02-07修回日期
7、:2013-03-15作者简介:张光华,男,高级工程师,主要从事计量检验研究工作。E-mail:mlj721106032@sina.com中国无机分析化学2013年64采用盐酸沉淀分离银,电感耦合等离子体原子发射光谱法测定纯银中镉、铋、铁、铅、锑、钯、硒、碲,能够同时测定且检出限很低,满足纯银中杂质元素的分析。热电公司)。硝酸、盐酸为优级纯,镉、铋、铁、铅、锑、钯、硒、碲标准储备溶液(1mg/mL,国家标准物质研究中心)。混合标准溶液(0.1mg/mL):分别移取上述标准溶液10mL于100mL容量瓶中,加5mL盐酸用蒸馏水定容,混匀。经过分别改变仪器
8、的各参数进行实验,确定了仪器的工作条件,见表1。实验部分仪器与试剂ICP-6300电感耦合等离
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