摘要
冶炼钒钛磁铁矿时加入一种作为示踪剂的碳酸钡以标定出铁过程中铁水所夹带的高炉渣.为准确测定钡的含量,在试验的基础上,建立了用电感耦合等离子体原子发射光谱法（ICP-AES）测定钒钛高炉渣中钡含量的方法.以氢氟酸、盐酸、硝酸混合试剂消解样品,冒高氯酸烟驱赶残余氢氟酸等试剂,盐酸溶解盐类后直接采用ICP-AES测定钡的含量.系统考察了钒钛高炉渣复杂共存体系所导致的基体效应、光谱干扰、背景噪音等干扰因素的影响,优选了灵敏度适宜的钡分析谱线（Ba 230.424 nm、233.527 nm、413.066 nm、455.403 nm、493.409nm）、检测积分与背景校正区域以及ICP光谱仪工作参数.试验结果表明,在分析线扫描窗口内,钒、钛、铁、钙、镁、铝等主要共存基体元素均不产生谱峰,并且与试剂空白信号基线重叠一致,表明钒钛高渣炉中基体组分对测定钡不产生基体效应、光谱干扰等影响,因此实验方法未采用基体匹配校正措施,直接以钡元素标准溶液绘制校准曲线.对于Ba 230.424 nm、233.527 nm、413.066 nm、455.403 nm、493.409 nm分析线,方法的测定下限在0.000 2％～0.001 0％范围,背景等效浓度在0.000 3％～0.000 5％范围,相对标准偏差（RSD）小于2.5％,加标回收率在93％～102％之间.方法适用于质量分数为0.005％～2.50％钡的测定.
Barium carbonate is used as a kind of tracer in smelting of vanadium-titanium magnetite to calibrate the blast {urnace slag carried in molten iron during tapping process. In order to accurately determine the content of barium, the inductively coupled plasma atomic emission spectrometry （ICPAES） for the determination of barium in vanadium-titanium blast furnace slag was established based on several experiments. The sample was digested using mixed hydrofluoric acid, hydrochloric acid and nitric acid. The residual hydrofluoric acid was removed by evolution of perchloric acid fumes. After dissolving the salts using hydrochloric acid, the content of barium was directly determined by ICPAES. The influence of matrix effect, spectral interference and background noise caused by vanadium- titanium blast furnace slag complex coexistence system was investigated in detail. The analysis line of barium with proper sensitivity （Ba 230. 424 nm, 233. 527 nm, 413. 066 nm, 455. 403 nm and 493. 409 nm）, detection integration, background correction area and the working parameters of ICP spectrometer were optimized and selected. The testing results showed that the main coexisting matrix elements （vanadium, titanium, iron, calcium, magnesium and aluminum） had no spectral peaks in scanning window of analysis line. In addition, they were consistent with the signal baseline of regent blank, indicating that the matrix components in vanadium-titanium blast furnace slag had no matrix effect and spectral interference in the determination of barium. Therefore, the correction measures of matrix matching were not adopted in this method. The calibration curve was directly plotted using the stand- ard solution of barium. For the analysis lines of Ba 230. 424 nm, 233. 527 nm, 413. 066 nm, 455. 403 nm and 493. 409 nm, the limit of quantitation for the method was in range of 0. 000 2%-0. 0010%, the background equivalent concentration was in range of 0. 000 3%-0. 000 5%, the relative standard deviation （RSD） was less than 2.5%, and the recoveries of standard addition were between 93O/oo and 102%. The proposed method was applicable for the determination of barium with mass fraction of 0. 005 2.50%.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第11期18-23,共6页
Metallurgical Analysis
关键词
电感耦合等离子体原子发射光谱
钡
钒钛高炉渣
常量分析
基体效应
inductively coupled plasma atomic emission spectrometry
barium
vanadium-titaniumblast furnace slag
macro-analysis
matrix effect
作者简介
作者简介：成勇（1968-），男，高级工程师，主要研究方向：ICP-AES，ICP-MS和GC-MS分析方法的研究及应用；E-mail：luck2005_1@sina．com
