熔融制样-X射线荧光光谱法测定铁水预处理脱硅消泡剂中主次成分  

Determination of major and minor components in defoamer for desilicication of pretreatment of hot metal by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：郭云涛[1] 刘伟[1] 戴学谦[1] 

机构地区：[1]山西太钢不锈钢股份有限公司技术中心,山西太原030003

出　　处：《冶金分析》2015年第1期50-54,共5页Metallurgical Analysis

摘　　要：消泡剂采用四硼酸锂和偏硼酸锂混合熔剂[m(Li2B4O7)∶m(LiBO2)=67∶33],稀释比为1∶10,滴加5滴200g/L溴化铵溶液做脱模剂,在950℃下熔融18min制备熔片。采用石灰石标准样品中添加基准碳酸钠的合成校准样品来绘制校准曲线,建立了X射线荧光光谱法(XRF)对铁水预处理脱硅消泡剂中二氧化硅、三氧化二铝、氧化钙、氧化镁、三氧化二铁和氧化钠等主次成分进行同时测定的方法。将烧失量作为消去组分处理,使用COLA模式校正,校正后的曲线能够准确测定未灼烧样品中主次成分的含量,大大缩短了分析时间。经验证,各组分测定结果的相对标准偏差(n=11)都在2%以内,消泡剂实际样品的分析结果与化学法分析结果吻合较好。With lithium tetraborate and lithium metaborate mixture [m（Li2B4O7）∶m（LiBO2）=67∶33] as flux, the defoamer sample was made into fused bead at the dilution ratio of 1 ： 10 through fusion at 950 ℃ for 18 min using five drops of 200 g/L ammonium bromide as release agent. The calibration curve was established with synthetic calibration sample that was prepared by adding standard sodium carbonate into limestone standard sample. Thus, a method for simultaneous determination of major and minor components of SiO2, Al2O3 , CaO, MgO, Fe2O3, Na2O, etc. in defoamer for desilicication of preparation of hot metal was established by X-ray fluorescence spectrometry （XRF）. The loss on ignition（LOI） was treated as elimination component. After correction by COLA mode, the content of major and minor component in the sample without ignition could be accurately determined with the calibrated curve, which greatly short ened the analysis period. Through validation, the relative standard deviations （RSD, n= 11） of each com ponent were all within 2 %, and the analytical results of actual defoamer sample were consistent with those of chemistry method.

关 键 词：消泡剂 X射线荧光光谱法 熔融制样 烧失量校正 主次成分 

分 类 号：O657.3[理学—分析化学]