电感耦合等离子体原子发射光谱(ICP-AES)法测定镧玻璃废粉中稀土元素总量及配分量

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定镧玻璃废粉中稀土元素总量和配分量的分析方法。样品经碱熔融后分离硅、铝等元素及钠盐,用硝酸和高氯酸破坏滤纸和溶解沉淀,用ICP-AES法测定稀土元素总量和配分量。讨论了溶解样品条件、共存元素干扰等影响测定的各种因素。实际样品的稀土总量与草酸盐重量法测定结果一致,配分量与X-射线荧光光谱(XRF)法、电感耦合等离子体质谱(ICP-MS)法测定结果一致。RSD(n=11)在0.15%~1.1%,加标回收率为97%~105%。测定范围为:La_2O_3/REO(80%~98%);CeO_2/REO(2%~20%);REO(16%~70%)。方法能快速准确地测定镧玻璃废粉中稀土元素总量及配分量。

Determination of Total Content and Component Contents of Rare Earth Complex in Waste Powder of Lanthanum Glass by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

A method was established for determination of total content and component contents of rare earth complex in waste powder of lanthanum glass by inductively coupled plasma atomic emission spectrometry. The samples were first melt by sodium hydroxide and sodium peroxide, and then the silicon, aluminum and sodium salt were separated. Nitric acid and perchloric acid were used to destroy the filter paper and dissolve the precipitate. The solution was analyzed for total content and component contents of rare earth complex by ICP-AES. The various factors that may influence the measurement were discussed, including dissolution conditions and interference by coexisting elements, etc. The total contents of rare earth were consistent with that by oxalate gravimetric method, and the component contents of rare earth complex were consistent with those by XRF and ICP-MS. RSDs (n=11) were between 0.15%~1.1%. Recoveries were in the range of 97%~105%. Measurement ranges: La2O3/REO (80%~98%); CeO2/REO(2%~20%); REO(16%~70%). This method can fast and accurately determine the total amount and components amount of the rare earth in the waste powder of lanthanum glass.