高氯酸脱水重量法测定氮化硅铁中硅含量.pdf

高氯酸脱水重量法测定氮化硅铁中硅含量
doi:10.3969/igs.10065-110X.,2015.06.017
高氯酸脱水重量法测定氮化硅铁中硅含量
许广凯
(天津天铁治金集团技术中心,河北涉县056404)
摘要果用高氯酸脱水重过法测定氯化硅铁中的硅含量。将氮化硅铁试样用过氧化钠一碳钠混合熔剂熔解,
经盐酸酸化,加高氯酸冒烟,硅酸脱水,沉淀于950℃马弗炉灼烧至恒重;加入硫酸、氢氟酸处理,使硅转化成四氟化
硅逸出,再灼烧至恒重,根椐酸处理前后两次的质量差计算硅的质量分数。实验结果表明,该测定方法简单易行,可
使试样溶解完全,测定糒密度和准确度都很高,能够满足使用要求。
[关键词]氩化硅;高氟酸;脱水;重量法;硅
Determination of Silicon Content in Nitrided Ferrosilicon with Perchloric
Acid Dehydration Gravimetric Method
XU Guang-hai
(Technology Center of Tianjin Tiantie Metallurgy Group, She County, Hebei Province 056404,China
Abstract Perchloric acid dehydration gravimetric method was adopted for the determination of silicon con-
tent in nitrided ferrosilicon. The sample of nitrided ferrosilicon melted with sodium dioxide - sodium carbon
ate mixed flux, was acidified by hydrochloric acid, smoked after perchloric acid was added, was dehydrated
with silicic acid, settled at 950 C and was burnt in muffle furnace to constant weight; then the sample was
further treated with the addition of sulfuric acid and hydrofluoric acid to transform silicon into silicon tetraflu-
oride to emit, and afterwards was rebut to constant weight. The mass fraction of silicon was calculated by
the mass difference before and after acid treatment. Test results showed this method was easy and feasible
With it, the sample could dissolve completely. Due to its high precision and accuracy in measurement, it i
could well meet the application requirement
Key words silicon nitride; perchloric acid; dehydration; gravimetric method; silicon
1引言
之差,即为二氧化硅的含量。该方法用镍坩埚2次
氮化硅铁是一种高级耐火材料,它具有热稳定灼烧试样和残渣,且灼烧温度过高,对镍坩埚消耗
生高、抗氧化能力强以及产晶精密度高的特点,在较大,操作过程较复杂。
冶金、机械、化学、电子、军事等行业有至关重要的
YB/4329-2010中试样用碳酸钠熔融分解,加
用途。氮化硅铁在治金中是生产冷轧单向硅钢片的盐酸溶解,蒸发干燥将硅酸脱水。可溶性盐类用盐
添加剂,具有良好的耐腐蚀性、热冲击和耐磨性能,酸溶解,沉淀高温蒸发脱水称重,加氢氟酸挥发硅
它与金属高温熔解后可获得良好的常温和低温强后再高温灼烧称重。过滤后的滤液用ICP-AES或制
度,适用于不锈钢、特种钢、耐火材料等铸造方面叫
光度法测定硅量,两次测定之和即为硅的总量,该
分析硅铁、氮化硅铁、耐火材料中硅的测定
方法用单一碳酸钠助熔,试样分解不完全,必须残
般采用重量法,CB/r6901.3-2004中第三部分四:氢渣回收处理之后硅总和,操作过程比较复杂。
氟酸重量法测定二氧化硅含量,试样经高温灼烧至
本文研究了高氯酸脱水重量法测定硅含量,试
恒重后,用氢氟酸、硝酸溶解,蒸发除硅,再以硝酸样用过氧化钠一碳酸钠混合嫆剂嫆解,经盐酸酸化,
除氟。于1000℃左右灼烧至恒重,测量两次质量加高氯酸冒烟,硅酸脱水。沉淀于950℃灼烧至恒
重。加硫酸、氢氟酸处理,使硅转化成四氟化硅逸
收稿日期:2015-08-23修回日期:2015-09-15
作者简介:徐广凯(1983-),男,本科,工程师,主要从事化验分析
出,再灼烧至恒重。加氢氟酸处理前后的质量之差
方面的研究工作。
计算硅的质量分数,该方法的特点是:试样一次熔
on〈(理化检测〉
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