首页|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

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 Micro wave Digestion and Inductively Coupled Plasma Emission Spectrometry

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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HC1+H2O2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 diges-tion system,digestion temperature and digestion time on sample digestion in the super-microwave digestion instru-ment.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+H2O2,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 di-gestion 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.

super microwave digesterinductively coupled plasma emission spectroscopypalladiumrhodiumdiscarded on-board catalyst

孙洪飞、许博、吴鉴、易云虎、杨柒梅、伍秋云、唐飞龙、刘琪

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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

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

昆明理工大学真空冶金国家工程研究中心,云南 昆明 650093

昆明理工大学冶金与能源工程学院,云南 昆明 650093

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超级微波消解仪 电感耦合等离子体发射光谱 车载催化剂

2024

昆明理工大学学报(自然科学版)
昆明理工大学

昆明理工大学学报(自然科学版)

CSTPCD北大核心
影响因子:0.516
ISSN:1007-855X
年,卷(期):2024.49(6)