超级微波消解-电感耦合等离子体发射光谱法测定车载催化剂中的钯、铑含量  

Determination of Palladium and Rhodium in Catalysts on Board Vehicles by Super Microwave Digestion and Inductively Coupled Plasma Emission Spectrometry

作　　者：孙洪飞 许博 吴鉴[1,2,3,4] 易云虎 杨柒梅 伍秋云 唐飞龙 刘琪 SUN Hongfei;XU Bo;WU Jian;YI Yunhu;YANG Qimei;WU Qiuyun;TANG Feilong;LIU Qi(Key Laboratory for Nonferrous Vacuum Metallurgy of Yunnan Province,Kunming University of Science and Technology,Kunming 650093,China;State Key Laboratory of Complex Non-ferrous Metal Resources Clean Utilization,Kunming University of Science and Technology,Kunming 650093,China;National Engineering Research Center of Vacuum Metallurgy,Kunming University of Science and Technology,Kunming 650093,China;Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming 650093,China)

机构地区：[1]昆明理工大学云南省有色金属真空冶金重点实验室,云南昆明650093 [2]昆明理工大学省部共建复杂有色金属资源清洁利用国家重点实验室,云南昆明650093 [3]昆明理工大学真空冶金国家工程研究中心,云南昆明650093 [4]昆明理工大学冶金与能源工程学院,云南昆明650093

出　　处：《昆明理工大学学报（自然科学版）》2024年第6期8-18,共11页Journal of Kunming University of Science and Technology(Natural Science)

基　　金：云南省科技厅重大科技专项(202302AB080002).

摘　　要：为了准确、快速分析车载催化剂中Pd、Rh的含量,结合超级微波消解和ICP-AES测定,针对车载催化剂消解难、消解不充分、消解效率低等问题,探究了在超级微波消解仪中消解体系、消解温度以及消解时间对样品消解的影响,在此基础上考察了消解液在ICP-AES测定中共存元素的干扰情况,建立了一种高效、快速消解车载催化剂并直接进行ICP-AES测定的方法.研究结果表明:在HCl+H_(2)O_(2)的消解体系中,以250℃的加热条件高速搅拌消解45 min,样品中的Pd、Rh元素能够完全消解,同时有效控制共存元素的溶出,削弱对待测元素的ICP-AES测定干扰,测定方法的RSD分别为Pd 1.50%和Rh 1.60%,加标回收率分别为Pd 98.93%和Rh 101.85%,测定结果与标准样品的认定值一致,满足可靠性评估标准.该方法相较于碱熔融、常压酸溶、密闭消解、微波消解结合碲共沉淀等常用测定方法,极大缩短了消解时间,同时削减了碲共沉淀分离富集贵金属的过程,提高了车载催化剂的测定效率.该方法的建立,实现了对车载催化剂更高效、快速地消解,并通过ICP-AES准确测定和评估Pd、Rh含量,为车载催化剂及相关样品中Pd、Rh的评估提供参考.To optimize the accurate and rapid analysis of Pd and Rh content in on-board catalysts,this study combined with the determination of super microwave digestion and ICP-AES,aiming at the problems of difficult digestion,insufficient digestion and low digestion efficiency of on-board catalysts,explored the influence of digestion system,digestion temperature and digestion time on sample digestion in the super-microwave digestion instrument.On this basis,the interference of co-existing elements in ICP-AES was investigated,and an efficient and fast method was established to dissolve the on-board catalyst and directly determine ICP-AES.The results show that:In the digestion system of HCl+H_(2)O_(2),the Pd and Rh elements in the sample can be completely dissolved by high-speed stirring digestion at 250℃for 45 min,and the dissolution of co-existing elements can be effectively controlled,thus reducing the interference of ICP-AES determination of the tested elements.The RSD of the method were Pd 1.50%and Rh 1.60%,and the recoveries were Pd 98.93%and Rh 101.85%,respectively.The results were consistent with the confirmed values of standard samples and met the reliability evaluation criteria.Compared with the common methods such as alkali melting,atmospheric acid dissolution,closed digestion,and microwave digestion combined with tellurium co-precipitation,this method greatly reduces the digestion time,reduces the process of tellurium co-precipitation separation and enrichment of precious metals,and improves the determination efficiency of on-board catalysts.The establishment of this method can realize more efficient and rapid digestion of on-board catalysts,and accurately determine and evaluate Pd and Rh contents by ICP-AES,which provides a reference for the evaluation of Pd and Rh in on-board catalysts and related samples.

关 键 词：超级微波消解仪 电感耦合等离子体发射光谱 钯 铑 车载催化剂 

分 类 号：O657.31[理学—分析化学] O643.36[理学—化学]