化工学报2017，Vol.68Issue(8)：3056-3063,8.DOI:10.11949/j.issn.0438-1157.20170123
基于流动注射光度法同时测定催化剂浸渍液中CoO/MoO3
Simultaneous determination of CoO and MoO3 in catalyst impregnation solutions
by flow injection spectrophotometry
曾明国 1李永生 1赵炀 1杜鑫1
作者信息
- 1. 四川大学化学工程学院,四川成都 610065
- 折叠
摘要
Abstract
Based on flow-injection analysis (FIA) and reaction systems of Mo(Ⅵ)-ascorbic acid and Co(Ⅱ)-KSCN, a new FIA system was proposed for simultaneous determination of high-concentration CoO/MoO3 in impregnation solutions. It was found that reaction products of Co(Ⅱ) and KSCN were K2Co(SCN)4 and K4Co(SCN)6, which the latter can be used to quantitate Co(Ⅱ). Co(Ⅱ) inhibitory effect on reaction system of Mo(Ⅵ)-ascorbic acid interfered with the determination of Mo(Ⅵ). Such Co(Ⅱ) interference was resolved by adding cobalt nitrate in the chromogenic agent for Mo(Ⅵ) measurement. In addition, testing conditions were optimized for various factors such as constituents and concentrations in chromogenic reagents for determining Co(Ⅱ) or Mo(Ⅵ), sampling volume and reaction temperature. The chromogenic agents for testing Mo(Ⅵ) were consisted of 15% (mass) ascorbic acid, 10 g·L-1 cobalt nitrate (calculated by CoO) and 0.1 mol·L-1 sulfuric acid, whereas those for testing Co(Ⅱ) were consisted of 37.5% (mass) KSCN and 0.1 mol·L-1 NaAc-HAc (pH 5.8). The detection ranges of MoO3 and CoO were in 10—100 g·L-1 and 5—50 g·L-1, and the detection limits for MoO3 and CoO were 2.1 g·L-1 and 1.3 g·L-1, respectively. Relative standard deviation was less than 1.2% (n=11), recovery was in range 98%—104%, and the analysis rate was 20 samples per hour.关键词
钴钼离子/同时测定/流动注射/催化剂/浸渍液/石油/化学分析Key words
cobalt and molybdenum/simultaneous determination/flow injection/catalysts/impregnation solution/petroleum/chemical analysis分类
化学化工引用本文复制引用
曾明国,李永生,赵炀,杜鑫..基于流动注射光度法同时测定催化剂浸渍液中CoO/MoO3[J].化工学报,2017,68(8):3056-3063,8.
