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Microwave-assisted sample preparation of α-spodumene: A simple procedure for analysis of a complex sample
Minerals Engineering ( IF 4.9 ) Pub Date : 2022-08-30 , DOI: 10.1016/j.mineng.2022.107820
Matteo Volpi , Camillo Pirola , Gianpaolo Rota , Joaquim A. Nóbrega , Diego Carnaroglio

Lithium-ion industry requires high amounts of lithium in high purity and spodumene, together with brine, are the major sources. Spodumene has three polymorphic forms, the one occurring in nature is α-spodumene. This form is highly resistant to chemical attack due to its compact structure containing silicon and aluminium oxides. Chemical analysis of this material is usually performed by combining fusion followed by acid digestion. However, microwave radiation converts α-spodumene to β-spodumene and it is known that this latter form can be chemically attacked using less critical reaction conditions. Based on this behaviour, it was developed a microwave-assisted procedure for chemical analysis of α-spodumene aiming the determination of lithium and other metals of interest by using an acid mixture composed by sulphuric and phosphoric acids and diluted hydrofluoric acid solution. The feasibility of using ammonium fluoride, a less critical reagent, instead of HF was also demonstrated. The heating program was implemented in 60 min at a maximum temperature of 230 °C using closed vessels for digestion of α-spodumene. All elements were determined by inductively coupled plasma optical emission spectrometry.



中文翻译:

α-锂辉石的微波辅助样品制备:复杂样品分析的简单程序

锂离子工业需要高纯度的大量锂,锂辉石和盐水是主要来源。锂辉石具有三种多晶型,自然界中存在的一种是α-锂辉石。由于其含有硅和氧化铝的紧凑结构,这种形式对化学侵蚀具有很强的抵抗力。这种材料的化学分析通常通过结合熔融和酸消化来进行。然而,微波辐射将 α-锂辉石转化为 β-锂辉石,并且已知后一种形式可以使用不太关键的反应条件进行化学攻击。基于这种行为,它开发了一种用于 α-锂辉石化学分析的微波辅助程序,旨在通过使用由硫酸和磷酸以及稀氢氟酸溶液组成的酸混合物来测定锂和其他感兴趣的金属。还证明了使用不太重要的试剂氟化铵代替 HF 的可行性。加热程序在 60 分钟内实施,最高温度为 230 °C,使用封闭容器消化 α-锂辉石。所有元素均通过电感耦合等离子体发射光谱法测定。

更新日期:2022-08-31
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