Determination of trace antimony by catalytic kinetic spectrophotometrywith antimony-potassium bromate-azocarmine B
SONG Xue-sheng1, CUI Yu-li2
1. School of Material Science and Engineering, University of Linyi, Linyi 276005, China; 2. School of Architecture,University of Linyi, Linyi 276005, China
Abstract：Antimony and its compounds can easily cause environmental pollution and belong to global priority pollutants. However, the catalytic activity of antimony is poor and there are few reports on the catalytic kinetic spectrophotometric determination of antimony. It was found that trace antimony (III) had catalytic effect on the fading reaction of azocarmine B oxidized by potassium bromate in phosphoric acid medium. Thus a novel determination method of antimony by kinetic spectrophotometry was established. Appropriate amount of antimony (III) sample solution (catalytic reaction, absorbance A) and same amount of water (non-catalytic reaction, absorbance A0) was added into colorimetric tube, respectively. Then, 0.7mL of 4.0×10-3 mol/L potassium bromated solution, 1.8mL of 1.0mol/L phosphoric acid and 2.2mL of 0.5g/L azocarmine B solution were added in sequence. After heating in water bath at 90℃ for 15min, the absorbance (A and A0) of two systems was measured at wavelength of 515nm. The experimental results indicated that the apparent activation energy was Ea=33.6kJ/mol. lg(A0/A) exhibited good linearity to the mass concentration of antimony in range of 0.02-0.26μg/mL and the limit of detection was 8.79×10-9 g/mL. For the measurement of complex sample (i.e., river mud), the extraction method was firstly used to avoid the interference of coexisting ions. Then the content of antimony was determined according to the experimental method. The relative standard deviations (RSD, n=6) of results were between 3.3% and 3.5%. The spiked recoveries were between 96% and 98%. The measured results were consistent with those obtained by atomic fluorescence spectrometry.
鲁丹,钱燕儿.石墨炉原子吸收光谱法快速测定塑料饮水管浸出液中的痕量锑[J].光谱学与光谱分析,2004,24(2):242-244.LU Dan,Q1AN Yan-er.Rapid determination of trace Sb in plastic pipes for bringing water by GFAAS[J].Spectroscopy and Spectral Analysis,2004,24(2):242-244.
[2]
何飞顶,李华昌,袁玉霞.氢化物发生-原子荧光光谱法同时测定红土镍矿中砷锑铋[J].冶金分析,2011,31(4):44-47.HE Fei-ding,LI Hua-chang,YUAN Yu-xia.Determination of arsenic, antimony and bismulth in laterite nickel ore by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2011,31(4):44-47.
[3]
白延涛,高楼军,柴红梅,等.桑色素荧光猝灭法测定水中微量锑[J].分析试验室,2014(4):452-454.BAI Yau-tao,GAO Lou-jun,CHAI Hong-mei,et al.Determination of antimony in water by fluorescence quenching method with morin[J].Chaiese Journal of Analysis Laboratory,2014(4):452-454.
[4]
李海.微波消解-电感耦合等离子体原子发射光谱法测定锌精矿中锑[J].冶金分析,2019,39(6):29-33.LI Hai.Determination of antimony in zinc concentrate by inductively coupled plasma with atomic emission spectrometry microwave digestion[J].Metallurgical Analysis,2019,39(6):29-33.
[5]
陈国树.催化褪色光度法测定微量锑的研究[J].江西大学学报:自然科学版,1985,9(3):74-75.CHEN Guo-shu.Studies of spectrophotometric determination of trace antimony by catalytic decolorization reaction[J].Jiangxi University:Natural Science Edition,1985,9(3):74-75.
[6]
高芝,刘利萍,高楼军,等.阻抑褪色光度法测定微量锑(III)[J].延安大学学报:自然科学版,2009,28(3):74-75.GAO Zhi,LIU li-ping,GAO Lou-jun,et al.Determination of antimony (III) by inhibition discoloring spectrophotometry[J].Journal of Yanan University:Natural Science Edition,2009,28(3):74-75.
[7]
朱复红,邱凤仙.水中锑的阻抑动力学光度测定法[J].环境与健康杂志,2006,23(6):549-551.ZHU Fu-hong,QIU Feng-xian.Determination of trace antimony (III) in water by inhibitory kinetic spectrophotometry[J].Journal of Environment and Health,2006,23(6):549-551.
[8]
柴红梅,高楼军,孙雪花,等.反相流动注射催化动力学光度法测定微量锑(III)[J].冶金分析,2008,28(7):42-45.CHAI Hong-mei,GAO Lou-jun,SUN Xue-hua,et al.Determination of micro antimony by reverse flow injection catalytic kinetic spectrophotometry[J].Metallurgical Analysis,2008,28(7):42-45.
[9]
杨迎春,张丽,吉爱军,等.H2O2氧化偶氮胂I褪色反应阻抑动力学光度法测定水样中痕量锑[J].冶金分析,2008,28(8):66-69.YANG Ying-chun,ZHANG Li,JI Ai-jun,et al.Inhibitory kinetic spectrophotometric determination of trace antimony in water samples based on oxidation of H2O2 on arsenazo I[J].Metallurgical Analysis,2008,28(8):66-69.
周之荣,熊艳,王群,等.高碘酸钾氧化中性红褪色催化动力学光度法测定痕量硒(IV)[J].分析试验室,2010,29(4):68-72.ZHOU Zhi-rong,XIONG Yan,WANG Qun,et al.Study on the kinetic spectrophotometric determination of selenium (IV) based on oxidation of neutral red with potassium periodate and its application[J].Chinese Journal of Analysis Laboratory,2010,29(4):68-72.
[12]
刘建国,菜翠青,彭涌涛.锑矿石分析[M]. 北京:地质出版社出版,1997:39-40.
[13]
林琳,张海燕,张军,等.微波消解试样-原子荧光光谱法测定土壤中砷和锑[J].理化检验:化学分册,2010,46(10):1155-1157.LIN Lin,ZHANG Hai-yan,ZHANG Jun,et al.AFS determination of arsenic and antimony in soil with microwave assisted sample digestion[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2010,46(10):1155-1157.
