熔融制样-X射线荧光光谱法测定钛铁中钛硅锰磷铝

熔融制样-X射线荧光光谱法测定钛铁合金中化学成分,核心技术是合金试样氧化技术,以有效避免样品熔融过程中铂-金坩埚受到侵蚀。在石墨垫底的瓷坩埚内以专用助熔剂将钛铁样品氧化成钛铁熔球,以四硼酸锂与碳酸锂混合熔剂熔融制备成玻璃片,建立X射线荧光光谱法(XRF)测定钛铁中钛、硅、锰、磷、铝含量的方法。试验探讨了熔剂选择、助熔剂用量、氧化条件、稀释比、脱模剂、熔融时间等条件对玻璃片质量及检测结果的影响,确定了最佳氧化、熔融实验条件。熔融制得的玻璃片强度高、质地均匀、检测面光洁,满足XRF测定要求。使用有证标准物质建立校准曲线,钛、硅、锰、磷、铝校准曲线相关系数介于0.999 6～1.000 0之间,校准曲线相关性满足XRF要求。方法应用于钛铁合金样品检测,各元素测定结果的相对标准偏差(RSD)介于0.25%～6.5%之间;准确度实验表明,钛铁标准样品测定结果与认定值相符。实验方法解决了钛铁熔融制样过程腐蚀铂-金坩埚问题,实现了钛铁合金中钛、硅、锰、磷、铝含量的同时快速分析,能够满足钛铁合金质量控制及作为炼钢生产指导的日常检测需求。

Determination of titanium,silicon, manganese,phosphorus andaluminum in ferrotitanium by X-ray fluorescence spectrometry with fusion sample preparation

During the determination of chemical compositions in ferrotitanium by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the core technology is the oxidization of alloy sample to effectively avoid the corrosion of platinum-gold crucible by sample in fusion process. The ferrotitanium sample was oxidized to titanium-iron molten globule in graphite backed porcelain crucible with a special oxidant. The sample was prepared to glass bead with mixed flux of lithium tetraborate and lithium carbonate. The determination method of titanium, silicon, manganese, phosphorus and aluminum in ferrotitanium by X-ray fluorescence spectrometry was established. The effects of flux selection, dosage of special oxidant, oxidation conditions, dilution ratio, mold release agent and melting time on the quality of glass bead and testing results were further discussed. The optimal oxidation and melting conditions were obtained. The prepared glass bead had uniform and smooth surface with good strength, which could meet the requirements of XRF determination. The calibration curves were established using the certified reference materials. The correlation coefficients of calibration curves for titanium, silicon, manganese, phosphorus and aluminum were between 0.999 6 and 1.000 0, which could meet the requirements of XRF. The proposed method was applied to the determination of ferrotitanium samples, and the relative standard deviations (RSD) of measurement results of elements were between 0.25% and 6.5%. The accuracy test results showed that the measured values of ferrotitanium standard samples were consistent with the certified values. The experimental method solved the corrosion problem of platinum-gold crucible during the fusion sample preparation of ferrotitanium. It realized the rapid and simultaneous analysis of titanium, silicon, manganese, phosphorus and aluminum contents in ferrotitanium, and could meet the quality control and daily determination requirements of ferrotitanium to guide the steelmaking production.