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惰气熔融-热导法测定炼钢促进剂中氮

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氮含量是衡量炼钢促进剂性能的重要参数之一,测定炼钢促进剂中氮含量十分必要.称取0.10 g样品于锡箔中,包裹住样品,将其压紧封口后装入镍篮中,投入石墨套坩埚内进行测定,以能覆盖炼钢促进剂中氮含量范围且氮含量呈一定阶梯水平的铁屑粉、氮化锰铁、高氮铬铁和钒氮合金粉末状标准物质绘制校准曲线,建立了惰气熔融-热导法测定炼钢促进剂中氮含量的方法.在优化的实验条件下,样品中氮含量与其对应的峰面积呈良好的线性关系,校准曲线的相关系数为0.999 3,方法检出限为0.003%,方法定量限为0.010%.分别采用实验方法对4个炼钢促进剂样品中氮含量平行测定7次,测定结果的相对标准偏差(RSD)在0.91%~1.7%之间.分别称取2个0.05 g炼钢促进剂样品,加入约0.05 g铁屑粉标准物质或高氮铬铁标准物质进行加标回收试验,加标回收率为95%~102%.
Determination of nitrogen in steel slag accelerant by inert gas fusion-thermal conductivity method
Nitrogen content is one of the important parameters to measure the performance of steel slag ac-celerant,so it is necessary to determine the content of nitrogen in steel slag accelerant.0.10 g of sample was weighed and transferred into tin foil.After packing the sample,the tin foil was pressed and sealed and then put into nickel basket.The nickel basket was transferred into graphite duplex crucible for determina-tion.The calibration curve was drawn with powdered reference materials of iron dust,nitride ferromanga-nese,high nitrogen ferrochrome and vanadium nitrogen alloy powder,which could cover the range of ni-trogen content in steel slag accelerant.Meanwhile,the nitrogen content was at a certain gradient.Conse-quently,a method for determination of nitrogen content in steel slag accelerant was established by inert gas fusion-thermal conductivity.Under the optimized experimental conditions,the nitrogen content in the sample showed a good linear relationship with its corresponding peak area.The correlation coefficient of calibration curve was 0.999 3.The limit of detection was 0.003%,and the limit of quantification was 0.010%.The contents of nitrogen in 4 steel slag accelerant samples was determined according to the pro-posed method in parallel for 7 times,and the relative standard deviations(RSD)of determination results ranged from 0.91%to 1.7%.2 steel slag accelerant samples(0.05 g)were used for recovery test by adding about 0.05 g of reference material of iron dust or nitride ferromanganese.The recoveries were be-tween 95%and 102%.

steel slag accelerantinert gas fusionthermal conductivity methodnitrogen

王虹、魏秉炎、李异

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天津海关化矿金属材料检测中心,天津 300457

炼钢促进剂 惰气熔融 热导法

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(3)
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