熔融制样-X射线荧光光谱法测定锰渣中8种组分  

Determination of 8 components in manganese slag by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：邓军华 亢德华 胡忠新 高品 王一凌 杨洁 DENG Junhua;KANG Dehua;HU Zhongxin;GAO Pin;WANG Yiling;YANG Jie(State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009,China;Iron&Steel Research Institute of Ansteel Group,Anshan 114009,China)

机构地区：[1]海洋装备用金属材料及其应用国家重点实验室,辽宁鞍山114009 [2]鞍钢集团钢铁研究院,辽宁鞍山114009

出　　处：《冶金分析》2023年第7期96-101,共6页Metallurgical Analysis

摘　　要：锰渣中各组分通常采用化学湿法进行测定,操作繁琐。实验以四硼酸锂为熔剂,选用炉渣、富锰渣、锰矿等标准物质以及用这些标准物质按照不同质量比混合配制而成的校准样品,组成各组分含量呈一定梯度和含量范围足够宽的标准样品/校准样品系列绘制校准曲线,克服了基体效应的影响,以经验系数法(MC)校正锰渣中各组分之间的光谱增强-吸收干扰,建立了X射线荧光光谱法(XRF)测定锰渣中SiO_(2)、Al_(2)O_(3)、CaO、MgO、TMn、P_(2)O_(5)、TiO_(2)、TFe共8种组分的方法。通过对稀释比、预氧化处理方式、熔融温度、熔融时间、脱膜剂量等条件进行优化,解决了四硼酸锂熔融锰渣时熔体黏度大、流动性弱导致的玻璃片成型不均匀、脱膜困难等问题。实验表明,各组分校准曲线线性相关系数均不小于0.9997,方法的检出限为11.2~90.2μg/g。实验方法应用于锰渣试样中各组分的测定,结果的相对标准偏差(RSD,n=6)为0.27%~3.7%。分别采用实验方法和标准方法对锰渣试样中各组分进行测定,结果基本一致。The determination of components in manganese slag usually adopts chemical wet method with complicated operation.Lithium tetraborate was used as flux.The certified reference materials of slag,manganese-rich slag and manganese ore were selected,and their synthetic calibration samples with different mass ratios were prepared.The calibration sample series with a certain gradient and a wide enough content range were used to draw calibration curves,which overcame the influence of matrix effect.The empirical coefficient method(MC)was used to correct the spectral enhancement-absorption interference among the components in manganese slag.The analysis method for the determination of 8 components in manganese slag,including SiO_(2),Al_(2)O_(3),CaO,MgO,TMn,P_(2)O_(5),TiO_(2)and TFe,by X-ray fluorescence spectrometry(XRF)was established.Through the optimization of dilution ratio,pre-oxidation method,fusion temperature,fusion time and the dosage of release agent,the problems of nonuniform forming and difficulty in demoulding caused by high viscosity and weak fluidity of molten manganese slag from lithium tetraborate were solved.The results showed that the linear correlation coefficients of calibration curves were higher than 0.9997,and the limit of detection was 11.2-90.2μg/g.The experimental method was applied to the determination of each component in manganese slag samples,and the relative standard deviations(RSDs,n=6)of the measured results were between 0.27%and 3.7%.The components in manganese slag samples were determined by the experimental method and standard method,respectively.The results of two methods were basically consistent.

关 键 词：X射线荧光光谱法(XRF) 锰渣 经验系数法校正(MC) 四硼酸锂 熔融制样 

分 类 号：O657.34[理学—分析化学] TF524[理学—化学]