基于流动注射光度法同时测定催化剂浸渍液中CoO/MoO3

doi:10.11949/j.issn.0438-1157.20170123

摘要/Abstract

摘要：

基于Mo（Ⅵ）-抗坏血酸、Co（Ⅱ）-KSCN反应体系和流动注射光度法，建立了一个全新的催化剂浸渍液中超高浓度CoO/MoO₃的同时测定系统。研究发现：Co（Ⅱ）与KSCN络合物是由K₂Co（SCN）₄和K₄Co（SCN）₆构成，利用后者可定量Co（Ⅱ）；Co（Ⅱ）对Mo（Ⅵ）-抗坏血酸反应有抑制作用，会干扰Mo（Ⅵ）测定；本研究利用Co（Ⅱ）的抑制作用，人为在测Mo（Ⅵ）的显色剂中加入一定量的硝酸钴，解决了该干扰问题。另外，对测定Co（Ⅱ）/Mo（Ⅵ）用的显色剂中的成分及浓度、进样体积、反应温度等相关影响因素进行了优选，得到的结果是：测定Mo（Ⅵ）的显色剂由15%（质量分数）抗坏血酸、10 g·L^-1硝酸钴（以CoO计）及0.1 mol·L^-1硫酸组成，测定Co（Ⅱ）的显色剂由37.5% KSCN、0.1 mol·L^-1 NaAc-HAc（pH 5.8）组成；MoO₃和CoO的测定范围分别为10~100 g·L^-1和5~50 g·L^-1，检出限分别为2.1 g·L^-1和1.3 g·L^-1，RSD<1.2%（n=11），回收率为98%~104%，分析速度为20样/小时。

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

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.

Key words: cobalt and molybdenum, simultaneous determination, flow injection, catalysts, impregnation solution, petroleum, chemical analysis

中图分类号:

O657.3

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.

ZENG Mingguo, LI Yongsheng, ZHAO Yang, DU Xin. Simultaneous determination of CoO and MoO₃ in catalyst impregnation solutions by flow injection spectrophotometry[J]. CIESC Journal, 2017, 68(8): 3056-3063.

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[8]	CHAPARRO L, FERRER L, LEAL L, et al. A multisyringe flow-based system for kinetic-catalytic determination of cobalt(Ⅱ) [J]. Talanta, 2015, 133: 94~99.
[9]	NAKANO S, KAMAGUCHI C, HIRAKAWA N. Flow-injection catalytic spectrophotometic determination of molybdenum (Ⅵ) in plants using bromate oxidative coupling of p-hydrazinobensene sulfonic acid with N-(1-naphthyl)ethylene diamine [J]. Talanta, 2010, 81(3): 786~791.
[10]	MANSOURI A I, MIRZAEI M, AFZALI D, et al. Catalytic spectrophotometric determination of Mo(Ⅵ) in water samples using 4-amino-3-hydroxy-naphthalene sulfonic acid[J]. Arabian Journal of Chemistry, 2016, 9(S2): 1105~1109.
[11]	TEMEL N K, GURKAN R. Catalytic spectrophotometric determination of trace Mo(Ⅵ) in milk-based beverages in the presence of bromophenol blue and H2O2 using SDS as a sensitizer[J]. Analytical Methods, 2016, 8(33): 6284~6292.
[12]	ZHANG X F, ZHOU Q, LV Y, et al. Ultrasensitive determination of cobalt in single hair by capillary electrophoresis using chemiluminescence detector [J]. Microchemical Joural, 2010, 95(1): 80~84.
[13]	CHEN J Q, YU Y, ZHANG Z W, et al. NBS-rCDs(OH-) chemiluminescence analysis system for the determination of cobalt ions[J]. Diamond and Related Materials, 2015, 58(none): 5~9.
[14]	SHELLEY R U, ZACHHUBER B, SEDWICK P N, et al. Determination of total dissolved cobalt in UV-irradiated seawater using flow injection with chemiluminescence detection [J]. Limnology and Oceanography-methods, 2010, 8(none): 352~362.
[15]	DU J X, LI J J, YANG L J, et al. Sensitive and selective determination of molybdenum by flow injection chemiluminescence method combined with controlled potential eletrolysis technique[J]. Analytica Chimica Acta, 2003, 481(none): 239~244.
[16]	杨玲娟, 谢天柱, 雷新有. 恒电位电解流动注射化学发光分析法测定钢铁中微量钼[J]. 冶金分析, 2011, 31(11): 24~28. YANG L J, XIE T Z, LEI X Y. Determination of micro molybdenum in steel by constant potential electrolysis - flow injection chemiluminescence analysis[J]. Metallurgical Analysis, 2011, 31(11): 24~28.
[17]	GAO X F, IKEBUKURO K, LI Y S, et al. A novel assay for determination of sulfated bile acids in urine by use of flow-injection chemiluminescence principle with immobilized enzymes[J]. Laboratory Robotics and Automation (Wiley & Sons), 1997, 9(2): 69~79.
[18]	ZACHARIADIS G A, THEMELIS D G, KOSSEOGLOU D J, et al. Flame AAS and UV-ⅥS determination of cobalt, nickel and palladium using the synergetic effect of 2-benzoylpyridine-2-pyridylhydrazone and thiocyanate ions [J]. Talanta, 1998, 47(1): 161~167.
[19]	SHEGEFTI S, MEHDINIA A, SHEMIRANI F. Preconcentration of cobalt(Ⅱ) using polythionine-coated Fe3O4 nanocomposite prior its determination by AAS[J]. Microchimica Acta, 2016. 183(6): 1963~1970.
[20]	SHAMSIPUR M, HASHEMI O R, SAFAⅥ A. Flotation-separation and ICP-AES determination of ultra trace amounts of copper, cadmium, nickel and cobalt using 2-aminocyclopentene-1-dithiocarboxylic acid[J]. Analytical Sciences, 2005, 21(9): 1063~1066.
[21]	邵从和. 电感耦合等离子体原子发射光谱法测定铜电积液中锑、铋、钴、镍和砷的含量[J]. 理化检验(化学分册), 2016, 52(6): 691~694. SHAO C H. ICP-AES Determination of Stibium, Bismuth, Cobalt,Nickel and Arsenic in Copper Electrowinning Solution[J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2016, 52(6): 691~694.
[22]	CANFRANC E, ABARCA A, SIERRA I. Determination of iron and molybdenum in a dietetic preparation by flame AAS after dry ashing [J]. Journal of Pharmaceutical and Biomedical Analysis, 2001, 25(none): 103~108.
[23]	BOSCHETTI W, BORGES A R, DUARTE A T, et al. Simultaneous determination of Mo and Ni in wine and soil amendments by HR-CS GF AAS[J]. Analytical Methods, 2014, 6(12): 4247~4256.
[24]	KAI X M, CHENG L, JIE W, et al. Determination of W, Mo and other 8 elements in powder metallurgical materials by ICP-AES [J]. Spectroscopy and Spectral Analysis, 2007, 27(12): 2578~2580.
[25]	张世龙, 黄启华, 胡小明, 等. 电感耦合等离子体原子发射光谱法测定钨矿石中硅、铁、铝、钛、钨、锡和钼的含量简[J]. 理化检验(化学分册), 2016, 52(10): 1237~1240. ZHANG S L, HUANG Q H, HU X M, et al. ICP-AES Determination of Si,Fe,Al,Ti,W,Sn and Mo in Tungsten Ores[J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2016, 52(10): 1237~1240.
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[27]	LI Y S, GAO X F. Flow injection analysis and application for chemistry analysis [M]. Jilin: The Jilin People's Publisher, 2002: 2~15.
[28]	LI Y S, XING C X, YANG L L. Determination of trace-level sodium ion in water-steam system of power plants using an FIA/ISE method with an automatic penetration and alkalization apparatus [J]. Analytical Science, 2005, 21(3), 273~279.
[29]	张红, 李永生, 李乔婧, 等. 流动注射-分光光度法测定钴钼催化剂浸渍液中高浓度钼离子[J]. 理化检验(化学分册), 2013, 49(6): 713~719.ZHANG H, LI Y S, LI Q J, et al. FI-spectrophotometric determination of molybdenum of high concentration in maceration extract of cobalt-molybdenum catalysts [J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2013, 49(6): 713~719.
[30]	杜鑫, 李永生. 基于磷钼蓝反应测定钴-钼催化剂浸渍液中钼离子含量[J]. 理化检验(化学分册), 2015, 51(3): 296~299.DU X, LI Y S. Determination of molybdenum ion in impregnation solution of Co-Mo catalysts based on the reaction of phosphorus molybdenum blue [J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2015, 51(3): 296~299.
[31]	孙宝莲, 李波, 王国栋, 等. 硫氰酸盐光度法测定氨浸渣中的钼[J]. 稀有金属材料与工程, 2009, 38(12): 2253~2255. SUN B L, LI B, WANG G D, et al. Spectrophotometric determination of molybdenum in the ammonia leaching residue using thiocyanate [J]. Rare Metal Materials and Engineering, 2009, 38(12): 2253~2255.
[32]	LI Y S, Muo Y, XIE H M, Simultaneous determination of silicate and phosphate in boiler water at power plants based on series flow cells by using flow injection spectrophotometry [J]. Analytica Chimica Acta, 2002, 455: 315-325.

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

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