氟硅酸钾-滴定法及苦杏仁酸-重量法测定硅锆合金中硅和锆  

Determination of silicon and zirconium in silico-zirconium alloys by potassium fluosilicate titration and amygdalic acid gravimetric method

作　　者：秦建 赵希文 朱春要 张继明 QIN Jian;ZHAO Xiwen;ZHU Chunyao;ZHANG Jiming(Institute of Research of Iron and Steel,Jiangsu Province/Sha-Steel,Zhangjiagang 215625,China)

机构地区：[1]江苏省(沙钢)钢铁研究院,江苏张家港215625

出　　处：《中国有色冶金》2024年第3期81-87,共7页China Nonferrous Metallurgy

摘　　要：快速准确检测硅锆合金中硅、锆含量对于生产具有重要意义,参考行业标准《出口硅铁中硅含量测定氟硅酸钾容量法》(SN/T 1014.1—2001)对硅含量进行测定,对于锆含量较高的硅锆合金,较难完全反应,测定结果偏低;采用电感耦合等离子体原子发射光谱法测定锆时,较适用于测定微量或痕量锆,而硅锆合金中锆质量分数大于10%,且含量范围宽,不适用于此方法,其他方法也均存在各种问题。本研究以硫酸、硝酸、盐酸、氢氟酸溶解硅锆合金,将硅转化为氟硅酸,然后与饱和硝酸钾溶液生成氟硅酸钾沉淀,用热水溶解沉淀,以氢氧化钠标准溶液滴定水解析出的氢氟酸,从而间接测得硅的含量;硅锆合金在酸液溶解下,在盐酸介质中,锆与苦杏仁酸生成苦杏仁酸锆沉淀,过滤,灼烧成二氧化锆,称重,通过氧化锆的含量间接换算出锆含量。6次平行测定试验表明硅和锆含量结果的相对标准偏差(n=6)为0.13%~1.39%,准确度试验中加标回收率为96.20%~104.60%,结果表明该方法具有较好的精密度和准确度,能够满足硅锆合金中硅和锆的测定要求。Rapid and accurate detection of silicon and zirconium content in silicon-zirconium alloy is of great significance for production.The silicon content was determined by referring to the industry standard“Method for determination of potassium fluosilicate Content in export ferrosilicon”(SN/T 1014.1-2001),For silicon-zirconium alloys with high zirconium content,it is difficult to react completely,and the measured results are low.The inductively coupled plasma atomic emission spectrometry is more suitable for the determination of trace or trace zirconium.However,the mass fraction of zirconium in silicon zirconium alloy is greater than 10%and the content range is wide,which is not suitable for this method.In this study,the silicon-zirconium alloy was dissolved with sulfuric acid,nitric acid,hydrochloric acid and hydrofluoric acid,and then the silicon was converted into fluorosilicate,and then the potassium fluorosilicate was precipitated with saturated potassium nitrate solution,and dissolved and precipitated with hot water.The hydrofluoric acid was titrated with sodium hydroxide standard solution,so as to measure the silicon content indirectly.Zircon alloy is dissolved in acid solution,zirconium and amygdalic acid form zirconium amygdalic acid precipitation,filtration,burning into zirconia,weighing,indirect conversion of zirconia content by zirconia content.The relative standard deviation(n=6)of silicon and zirconium content was 0.13%~1.39%,and the standard recovery of accuracy test was 96.20%~104.60%.The results show that the method has good precision and accuracy,and can meet the determination requirements of silicon and zirconium in silicon-zirconium alloy.

关 键 词：硅锆合金 硅测定 锆测定 氟硅酸钾-滴定法 苦杏仁酸-重量法 

分 类 号：TF125.2[冶金工程—粉末冶金] O655[冶金工程—冶金物理化学]