摘要
钒钛渣富含钒、钛等有益元素,具有较高综合利用价值,其化学成分的测定一般采用化学分析法,操作步骤繁琐、化学试剂用量大、分析周期长。实验以四硼酸锂-碳酸锂为熔剂,稀释比1∶20,碘化钾为脱模剂,在700℃预氧化20min,在1 100℃熔融22min,制得透明的熔片。使用钒渣、钒钛高炉渣、转炉渣等标准样品及钒尾渣、钒铁炉渣、铁矿石等湿法定值的生产样品,组成测定样品浓度和梯度相匹配的系列校准样品,拓展了校准曲线含量范围,建立了熔融制样-X射线荧光光谱法(XRF)测定钒渣、钒钛高炉渣、钒铁炉渣、钒尾渣中TFe、SiO2、Al2O3、CaO、MgO、MnO、V2O5、TiO2、Cr2O3、P的快速检测方法,解决了每种钒钛渣都要建立一套分析方法,不能同时测定多种类型钒钛渣的问题。对钒钛渣样品进行精密度考察,测定结果的相对标准偏差(RSD,n=10)均小于7%;采用实验方法对钒钛渣标准样品进行分析,测定结果与认定值相符,能满足钒钛渣中各成分的检测要求。
The vanadium-titanium slag contains rich beneficial elements including vanadium and titanium,and it has high comprehensive utilization value.The determination of composition in vanadium-titanium slag usually adopts chemical analysis method,which has some disadvantages such as complicated operation procedures,large consumption of chemical reagents and long analysis period.The transparent fuse piece of sample was prepared under the following conditions：the flux was lithium tetraborate-lithium carbonate,the dilution ratio was 1∶20,the release agent was potassium iodide,and the sample was pre-oxidized at700℃for 20 min followed by fusion at 1 100℃for 22 min.The standard samples（vanadium slag,vanadium-titanium blast furnace slag,converter slag,etc）and production samples（vanadium tailings,ferrovanadium slag and iron ore,which had been determined by wet method）were used to prepare series calibration samples with matched concentration and gradient to the test samples.The content range of calibration curve was expanded.The rapid determination method of TFe,SiO2,Al2 O3,CaO,MgO,MnO,V2 O5,TiO2,Cr2 O3 and P in vanadium slag,vanadium-titanium blast furnace slag,ferrovanadium slag and vanadium tailings by X-ray fluorescence spectrometry（XRF）with fusion sample preparation was established.The problem that one set of analysis method should be established for each type of vanadium-titanium slag and it could not be used for the simultaneous determination of several types of vanadium-titanium slag was solved.The precision test of vanadium-titanium slag sample was conducted.The relative standard deviations（RSD,n=10）of determination results were less than 7%.The experimental method was applied for the analysis of vanadium-titanium slag standard sample,and the found results were consistent with the certified values.The detection requirements of each component in vanadium-titanium slag could be satisfied.
作者
杨新能
冯宗平
YANG Xin-neng;FENG Zong-ping(Manufacturing Department of Panzhihua Steel ＆ Vanadium Co.,Ltd.,Panzhihua 617000,China)
出处
《冶金分析》
CAS
CSCD
北大核心
2018年第7期57-62,共6页
Metallurgical Analysis
关键词
X射线荧光光谱法
熔融制样
钒钛高炉渣
钒渣
钒尾渣
钒铁炉渣
X-ray fluorescence spectrometry （XRF）
fusion sample preparation
vanadium-titanium blast furnace slag
vanadium slag
vanadium tailings
ferrovanadium slag
