摘要
目的本文旨在研究直接除碳重量法测定碳复合磷酸铁锂中总磷含量。方法采用高氯酸分解试样并同时除去样品中的碳后,在酸性介质中,正磷酸根与喹钼柠酮沉淀剂反应生成黄色磷钼酸喹啉沉淀,经过滤、洗涤、干燥、称量,即可求出磷含量。结果高氯酸消解除碳,样品消解完全且清亮,减少了过滤除碳步骤,通过优化条件试验、对该方法进行了精密度和准确度试验,其相对标准偏差(Relative Standard Deviation,RSD)小于0.2%,加标回收率为98.4%~101.1%。该方法最大的优点在于碳在消解过程中直接除去,消除了碳包裹对磷测定的影响,不需要过滤除碳,缩短了操作流程,分析时间短,高含量磷用经典重量法测定,其精密度和准确度高,能为生产提供快速准确的结果。结论本法适用于快速准确测定碳复合磷酸铁锂中总磷含量的。
Objective To study the determination of total phosphorus in carbon compound lithium iron phosphate by direct carbon removal gravimetric method.Methods After the sample was decomposed by perchloric acid and the carbon in the sample was removed at the same time,the yellow quinoline phosphomolybdate was precipitated by the reaction of orthophosphoric acid with the precipitant quinomolymonone in the acidic medium.The phosphorus content could be obtained by filtration,washing,drying and weighing.Results The carbon removal by perchloric acid was complete and clear,and the steps of filter and carbon removal were reduced.The precision and accuracy tests of the method were carried out by optimizing the conditions.The relative standard deviation(RSD)of the method was less than 0.2%,and the recovery rate of standard addition was 98.4%~101.1%.The biggest advantage of this method is that carbon is directly removed in the digestion process,eliminating the influence of carbon encapsulation on phosphorus determination,no need to filter carbon removal,shorten the operation process,short analysis time,high content of phosphorus is determined by classical gravimetric method,which has high precision and accuracy,and can provide rapid and accurate results for production.Conclusion This method is suitable for the rapid and accurate determination of total phosphorus in carbon complex lithium iron phosphate.
作者
邹小芬
ZOU Xiao-Fen(Fujian Zijin Mining&Metallurgy Test Technology Co.,Ltd.,Longyan 364204,China)
出处
《实验室检测》
2024年第5期14-17,共4页
Laboratory Testing
关键词
高氯酸
磷酸铁锂
总磷
perchloric acid
lithium iron phosphate
total phosphorus
作者简介
通信作者:邹小芬,工程师,主要研究方向为化学分析。E-mail:961908109@qq.com
