氟硅酸钾沉淀-酸碱滴定法测定超低碳碳化稻壳中二氧化硅-中国测试.pdfVIP

第41卷第8期 中国测试 Vol.41 No.8 2015年8月 CHINA MEASUREMENT TEST August，2015 doi院10.11857/j.issn.1674-5124.2015.08.011 氟硅酸钾沉淀-酸碱滴定法测定超低碳 碳化稻壳中二氧化硅 董礼男袁 朱春要袁 张良芬袁 年季强 （江苏省沙钢钢铁研究院分析测试中心，江苏 张家港 215625） 摘 要院该文基于氢氧化钾熔融法分解袁氟硅酸钾滴定检测超低碳稻壳样品中SiO 含量的方法研究遥试样在镍或银坩埚 2 中袁通过氢氧化钾熔融袁二氧化硅转化为硅酸钾袁在有过量氯化钾存在的强酸性溶液中加入氟化钾溶液袁生成氟硅酸钾 沉淀袁经抽滤尧洗涤后溶于沸水中袁以溴麝香草酚蓝与酚红混合物为指示剂袁氢氧化钠标准溶液滴定水解后生成氢氟酸袁 从而间接得出二氧化硅含量遥 对熔样方式尧干扰元素尧沉淀时间尧温度控制及指示剂的选择等条件进行试验及优化袁考察 检测方法的准确度和精密度袁精密度相对标准偏差渊RSD冤臆0.20%渊n=6冤袁与经典重量法进行比较袁结果一致遥 关键词院碳化稻壳曰氢氧化钾曰氟硅酸钾曰滴定法曰二氧化硅 文献标志码院A 文章编号院1674-5124渊2015冤08-0048-04 Determination of silicon dioxide in ultra-low carbon carbonised rice husk by potassium fluosilicate precipitation-acid-base titration method DONG Li’nan，ZHU Chunyao，ZHANG Liangfen，NIAN Jiqiang （Analysis and Characterization Center，Institute of Research of Iron and Steel，Zhangjiagang 215625，China） Abstract: A simple and accurate way was proposed to determine the content of silicon dioxide in ultra-low carbon samples based on potassium fluosilicate titration. The samples were molted in potassium hydroxide in a nickel or silver crucible to generate potassium silicate; the product was placed into a strong acid solution with excess potassium chloride or potassium oxalate and then added with potassium fluoride solution to obtain potassium siliofluoride precipitation. Afterwards， the content of silicon dioxide was acquired by performing the following steps: draw，filter，wash， and then dissolve into boiling water; use bromothymol blue and phenol red as a mixed i