熔融制样-X射线荧光光谱法测定碳化钛渣中碳化钛  

Determination of titanium carbide in titanium carbide slag by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：冯宗平 杨新能 FENG Zongping;YANG Xinneng(Testing Measuring Center of Pangang Group Panzhihua Steel&Vanadium Co.,Ltd.,Panzhihua 617000,China)

机构地区：[1]攀钢集团攀枝花钢钒有限公司检测计量中心,四川攀枝花617000

出　　处：《冶金分析》2025年第3期64-69,共6页Metallurgical Analysis

摘　　要：准确测定碳化钛渣(以下简称碳化渣)中碳化钛的含量对于碳化工艺生产过程的指导具有关键性作用。采用盐酸-硫酸-氢氟酸体系选择性溶解钛氧化物,实现了碳化渣中钛氧化物、碳化钛物相的快速分离;分离后残渣连同滤纸经600~700℃灰化灼烧20 min后,再于1100℃灼烧2~3 min。以四硼酸锂-碳酸锂为熔剂,溴化锂为脱模剂,在1100℃熔融20 min,制得透明的熔片,实现了熔融制样-X射线荧光光谱法对碳化渣中碳化钛的测定。用盐酸-硫酸-氢氟酸体系分离碳化渣样品后,通过高温灼烧,残渣中碳化钛会转化为二氧化钛,因此取5.0~80.0 mg的光谱纯二氧化钛共9份绘制校准曲线,线性相关系数r=0.99998,二氧化钛测量范围为1.25%~20.0%。按照实验方法测定2个碳化渣样品中碳化钛,测定结果的相对标准偏差(RSD,n=6)不大于0.5%;选择3个碳化渣样品,按照实验方法进行测定再分别加入高纯碳化钛进行加标回收试验,加标回收率在97%~102%之间。分别按照实验方法和分光光度法测定碳化渣实际样品中碳化钛,测定结果一致。The accurate determination of titanium carbide content in titanium carbide slag(titanium carbide)plays a key role in the guidance of carbonization production process.In this study,the hydrochloric acid-sulfuric acid-hydrofluoric acid system was used to selectively dissolve titanium oxide,realizing the rapid separation of titanium oxide and titanium carbide phases in titanium carbide slag.After separation,the residue and filter paper were ashed and burned at 600-700℃for 20 min,and then burned at 1100℃for 2-3 min.Lithium tetraborate-lithium carbonate was selected as the flux,and lithium bromide was selected as the release agent.The sample was fused at 1100℃for 20 min to prepare the transparent bead.A method for the determination of titanium carbide in titanium carbide slag by X-ray fluorescence spectrometry with fusion sample preparation was established.After the titanium carbide slag sample was separated using the hydrochloric acid-sulfuric acid-hydrofluoric acid system,titanium carbide in the residue could be converted to titanium dioxide through burning at high temperature.Therefore,nine samples of spectrally pure titanium dioxide(5.0-80.0 mg)were used to draw the calibration curve.The linear correlation coefficient was r=0.99998,and the determination range of titanium dioxide was 1.25%-20.0%.The contents of titanium carbide in two titanium carbide slag samples were determined according to the experimental method,and the relative standard deviations(RSD,n=6)of the determination results were not more than 0.5%.Three titanium carbide slag samples were selected and determined according to the experimental method.Then the high-purity titanium carbide was added for the spiked recovery test.The recoveries were between 97%and 102%.The contents of titanium carbide in titanium carbide slag samples were determined by the experimental method and spectrophotometry respectively,and the results were consistent.

关 键 词：熔融制样 X射线荧光光谱法(XRF) 碳化钛渣 碳化钛 二氧化钛 

分 类 号：O657.34[理学—分析化学] TF524[理学—化学]