碱熔-碲共沉淀富集-电感耦合等离子体原子发射光谱法测定石油化工废催化剂不溶渣中铂钯  

Determination of platinum and palladium in insoluble slag of waste catalyst for petrochemical industry by inductively coupled plasma atomic emission spectrometry after alkali fusion-tellurium coprecipitation enrichment

作　　者：谭文进 郑允 贺小塘 肖雄 林波 马王蕊 

机构地区：[1]贵研资源(易门)有限公司、稀贵金属综合利用新技术国家重点实验室,云南昆明650106

出　　处：《冶金分析》2016年第2期43-48,共6页Metallurgical Analysis

基　　金：国家高技术研究发展计划基金资助(863计划)(2012AA063203,2012AA063207);云南省科技创新强省计划基金资助(2011AA004);云南省地方标准制(修)订基金资助(DBZD069-2014);云南省标准化研究与建设项目基金资助(2015BZHXM05)

摘　　要：采用过氧化钠高温熔解样品，3．0～4．5mol／L盐酸介质中二氯化锡还原、碲共沉淀富集铂、钯，选择Pt265．945nm、Pd340．458nm作为分析谱线，建立了电感耦合等离子体原子发射光谱法（ICP-AES）测定石油化工废催化剂不溶渣中铂、钯的方法。样品中铂的质量浓度在2～27μg／mL、钯的质量浓度在O．7～20μg／mL范围内，校准曲线线性方程分别为IPt=3624×ρPt-180．4和Ipd=9869×ρPd-220．9，线性相关系数R2均为0．99998。方法中铂、钯的检出限分别为0．017μg／mL和0．0042μg／mL。测定石油化工废催化剂不溶渣样品中109～1342g／t铂和37～977g／t钯，结果的相对标准偏差（RSD，n=5～11）分别为1．1％～1．9％和1．1％～3．6％，测定结果与火试金富集-电感耦合等离子体原子发射光谱法的测定结果一致，铂、钯的回收率分别为99％～100％和1OO％。The sample was fused with sodium peroxide at high temperature.Then,the platinum and palladium were enriched by stannous chloride reduction and tellurium coprecipitation in 3.0-4.5mol/L hydrochloric acid medium.Pt 265.945 nm and Pd 340.458 nm were selected as the analytical lines.The determination method of platinum and palladium in insoluble slag of waste catalyst for petrochemical industry by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.When the mass concentration of platinum and palladium in sample was in range of 2-27μg/mL and 0.7-20μg/mL,the linear equation of calibration curves was I_(Pt)=3 624×ρ_(Pt)-180.4and I_(Pd)=9 869×ρPd-220.9,respectively.The linear correlation coefficients(R2)were both 0.999 98.The detection limit of platinum and palladium in this method was 0.017μg/mL and 0.004 2μg/mL,respectively.The content of platinum(109-1 342g/t)and palladium(37-977g/t)in insoluble slag of waste catalyst for petrochemical industry was determined according to the experimental method.The relative standard deviation(RSD,n=5-11)was 1.1%-1.9%and 1.1%-3.6%,respectively.The determination results were consistent with those obtained by fire assaying enrichment-inductively coupled plasma atomic emission spectrometry.The recoveries of platinum and palladium were 99%-100% and 100%,respectively.

关 键 词：碱熔 碲富集 电感耦合等离子体原子发射光谱法 石油化工废催化剂不溶渣 铂 钯 

分 类 号：X833[环境科学与工程—环境工程] O657.3[理学—分析化学]