富锂固溶体正极材料中锰含量的测定

Determination of Manganese Content in Lithium-Enriched Solid Solution

为了制定富锂固溶体正极材料的生产工艺,需要对其前驱体中锰含量进行准确测定,以硝酸铵为氧化剂,采用磷酸固定锰的价态,用硫酸亚铁铵标准溶液滴定锰的容量法来测定锰含量,并对溶样方法及温度控制、磷酸的加入量、加入硝酸铵时的温度控制和硝酸铵的加入量等条件进行了优化实验,实验结果表明：称样量为0.300 0g,溶样消耗盐酸10mL,加入10mL H3PO4,溶液温度240℃时加入1.2g硝酸铵进行氧化,测定准确度最高,加标回收率为99.70%~100.5%,相对标准偏差小于0.24%,方法耗时短,不需要加入任何掩蔽剂,适合实际分析采用。

In order to formulate the production process of lithium-enriched solid anode material, it is necessary to accurately determine the content of manganese. Ammonium nitrate is employed as an oxidant and phosphoric acid is used to fix the valence of manganese. The content of Mn can be determined by titration of ferrous ammonium sulfate titration. In addition, an optimized experiment was conducted regarding the conditions of measurement process such as sample dissolution method, temperature control, phosphoric acid volume, the temperature control when adding NH4NO3 and NH4NO3 dosage. Experiment conditions were optimized as follows： 0. 300 0 g of the sample, 10 mL of hydrochloric acid for sample digestion solution , 10 mL of H3PO4 added, oxidation of ammonium nitrate（1.2 g） at 240 ℃ The recovery was 99.70%~100. 5%, and the relative standard deviation was less than 0.24%. The proposed method is simple, rapid, and it can be applied for practical analysis needing no masking agent.