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作 者:赵坤 王源瑞 刘静静 卢昌祥 赵和存 ZHAO Kun;WANG Yuan-rui;LIU Jing-jing;LU Chang-xiang;ZHAO He-cun(Northwest Research Institute of Mining and Metallurgy,Baiyin 730900,China)
出 处:《甘肃冶金》2020年第5期117-119,122,共4页Gansu Metallurgy
摘 要:工业氢氟酸中氟硅酸的测定,通常以硅酸钠与钼酸铵反应生成黄色的硅钼杂多酸,然后经过无水亚硫酸钠-1-氨基-2-萘酚-4-磺酸-焦亚硫酸钠还原成钼蓝,但这种还原剂结构复杂,对钼黄还原生成稳定钼蓝的时间较长,且该溶液配置繁琐。因此,本实验提出了一种以抗坏血酸为还原剂,在适宜的pH下对钼黄进行还原,快速形成稳定的钼蓝,在波长810 nm处测定硅的吸光度值,该方法测定的氟硅酸结果的相对标准偏差均小于0.022%(n=6),加标回收率为96%~98%。因此,该方法快速、准确,适用于实际生产中氢氟酸样品中氟硅酸的批量检测。Determination of fluorosilicaic acid in industrial hydrofluoric acid,usually with sodium silicate and ammonium pyridoxine reaction to produce yellow silicate polysacnic acid,and then reduced to molybdenum blue by anhydrous sodium sulfite-1-amino-2-naphthol-4-sulfonic acid-sodium pyrosulfite,however,the structure of the reducing agent is complex,the reduction of molybdenum yellow to stable molybdenum blue takes a long time,and the solution configuration is cumbersome.Therefore,in this study,an ascorbic acid was used as a reducing agent to reduce molybdenum yellow at an appropriate pH and rapidly form a stable molybdenum blue.The absorbance of silicon was determined at 810 nm.The relative standard deviation of the method was less than 0.022%(n=6),and the standard recovery was 96%~98%.Therefore,this method is fast and accurate,and is suitable for the batch detection of fluorosilicic acid in hydrofluoric acid samples in actual production.
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