采取一次称样,先用高锰酸钾-草酸钠返滴定法测定了尖晶石型锰酸锂样品中高价锰的还原电子的物质的量,而后在磷酸介质中,用高氯酸-硫酸亚铁铵滴定法测定了溶液中的总锰量,减去加入高锰酸钾中的锰量即为样品中的锰量,结合还原电子的物质的量计算得到了尖晶石型锰酸锂中锰的平均价态.对测定锰平均价态的条件,如水浴温度,草酸钠、磷酸和高氯酸的用量进行了详细研究,并确定了最佳实验条件.将该方法应用于掺杂尖晶石型锰酸锂中锰平均价态的测定,所得结果在3.57~3.69之间,与掺杂锰酸锂中锰化合价高于3.5结果一致,相对标准偏差(RSD,n=6)在0.26%~0.30%之间.
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