Determination of K2O in High Potassium Aluminosilicate by Tetraphenylborate Gravimetry
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摘要: 为了精确测定分解反应过程中钾的挥发量, 结合GB8574-2002, 在样品高钾铝硅酸盐物料(钾长石、碳酸钾焙烧熟料, K2O含量大于15%)处理中采用聚环氧乙烷絮凝沉淀Si, 新制Ca(OH)2溶液除去Mg2+、Fe2+、Fe3+、Mn2+等其他阳离子, 加入碳酸铵稳定溶液pH值以除去Ca2+和Al3+.采用四苯硼钾重量法测定钾含量, 测定结果与表样对照, 相对误差在0.5%以内.实验表明: 利用Ca(OH)2除杂, 溶液pH值须控制在10~ 12;碳酸铵双水解反应后, 溶液pH值须控制在7.35左右以除尽Ca2+和Al3+; 低温(T < 473 K)蒸发溶液除去NH4+, 消除了因生成四苯硼铵沉淀而带来的分析误差.结果表明该方法可以精确测定高钾铝硅酸盐物料的K2O含量, 具有成本低、方便快捷、无需大型仪器之优点.Abstract: A convenient and rapid method was established to determine K2O content in high potassium aluminosilicate(K2O content> 15%), which was obtained by calcining K-feldspar and K2CO3. Combined with the GB8574-2002 potassium tetraphenylborate gravimetry method, silicon was deposited by polyethylene oxide in an acid environment. Other cations such as Mg2+, Fe3+, Fe2+, Mn2+ were removed by the intrusion of newly formed calcium hydroxide solution by controlling pH at 10-12. The remaining Al3+ and Ca2+ were eliminated by salvolatile hydrolyzation which stabilized the solution at about pH = 7.35. Before the potassium tetraphenylborate gravimetry method, the introduced ammonia was removed by low temperature(T < 473 K)calcining to avert ammonium tetraphenylborate precipitation. The relative error in this experiment was less than 0.5% by comparison with standard specimen.
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图 1 25 ℃离子形态分布随pH值的变化
Fig. 1. Distribution of aqueous species as a function of pH in 25 ℃
表 1 溶液pH值对测定结果的影响
Table 1. pH value influence on test
表 2 样品的化学全分析结果
Table 2. Chemical composition of samples
表 3 本文测试结果Ⅰ与标准试样Ⅱ比较
Table 3. Analysis result and comparison with standard sample
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