摘要：
Lithium tetraborate [(4.000 0±0.000 1) g] was weighted in a platinum alloy crucible and melted at 950 °C to form a waxy protective film on the inner wall of the crucible.Then 1.000 0 g of anhydrous lithium tetraborate,0.500 0 g of barium peroxide,0.500 0 g of lithium carbonate and 0.100 0 g of ferrotitanium were added into the treated platinum alloy crucible and mixed well.2.000 0 g of anhydrous lithium tetraborate was added to cover the surface,and 0.35 mL of 1 000 g · L-1 lithium bromide solution was added along the reagent,and then sample preparation was carried our by melt method.The calibration curves were established using 5 CRMs of ferrotitanium and 2 calibration samples prepared with high purity iron powder and CRMs,to determine the contents of titanium,silicon,manganese,aluminum and phosphorus in ferrotitanium.Ti Kα was selected as analysis spectral line,and Ba was used as an internal standard for calibration of titanium.Empirical coefficient method and theoretical α-factor method were used to correct the matrix interferrence and spectral line interferrence to silicon,aluminum and phosphorus.The proposed method was applied to the analysis of ferrotitanium samples,giving results in consistency with the results obtianed by the wet-chemical method,and RSDs (n=11) ranged from 0.24 ％ to 4.7 ％.%在铂合金坩埚中称取四硼酸锂(4.000 0±0.000 1)g,在950°C下进行熔融,使得坩埚内壁形成一层蜡状的保护膜.在经处理的铂合金坩埚中加入无水四硼酸锂1.000 0 g、过氧化钡0.500 0 g、碳酸锂0.500 0 g、钛铁样品0.100 0 g,混匀,将2.000 0 g无水四硼酸锂覆盖在表面,沿试剂周边加入1 000 g·L-1溴化锂溶液0.35mL,然后进行熔融制样.用5个标准样品和2个由高纯铁粉和标准样品配制的校准样品建立校准曲线,同时测定钛铁中钛、硅、锰、铝和磷的含量.选用Ti Kα为分析谱线,以钡为内标对钛进行校正.采用经验系数法和理论α系数法对硅、铝和磷进行基体校正和谱线干扰校正.采用此方法分析钛铁样品,所得结果和湿法化学法的结果一致,测定值的相对标准偏差(n=11)在0.24％～4.7％之间.
