碱熔-碘化物萃取-苯基荧光酮光度法测定铁矿石中锡
|
摘要
锡作为钢铁中的有害元素通常要严格控制其含量,因此需要准确测定其来源铁矿石中锡的含量。实验建立了碱熔-碘化物萃取-苯基荧光酮光度法测定铁矿石中锡含量的方法。样品以无水碳酸钠-硼酸(m∶m=3∶1)混合熔剂高温熔融,盐酸(1+5)浸取熔融物,硫酸冒烟,冷却后定容。分取合适体积,加入碘化钾,以苯萃取碘化物,然后用0.8mol/L硫酸反萃取,水相放入50mL容量瓶中,依次加入苯基荧光酮、溴化十六烷基三甲基铵显色,于分光光度计波长535nm处测量其吸光度,测定范围0.000 5%～0.20%,加标回收率99%～104%。方法应用于铁矿石样品中锡的测定,结果的相对标准偏差(RSD,n=8)小于4%。
Tin was a kind of harmful element in iron and steel and its content must be strictly controlled.Therefore,the content of tin in iron ore should be accurately measured.The determination method of tin in iron ore by alkali fusion-iodide extraction-phenylfluorone spectrophotometry was established.The sample was fused with anhydrous sodium carbonate-boric acid(m∶m=3∶1)as mixed flux at high temperature.The molten substance was then leached with hydrochloric acid(1+5).After sulfuric acid fuming and cooling,the sample solution was diluted to certain volume.Appropriate volume of prepared solution was sampled.The potassium iodide was added and benzene was used to extract the iodide,which was then re-extracted with 0.8 mol/L sulfuric acid.The water phase was transferred into 50 mL volumetric flask.After adding phenylfluorescein and cetyl trimethylammonium bromide for coloring,the absorbance was measured using spectrophotometer at the wavelength of 535 nm.The determination range was 0.000 5%-0.20%.The spiked recoveries were between 99%and 104%.The proposed method was applied for the determination of tin in iron ore samples.The relative standard deviation(RSD,n=8)of the results was less than 4%.
Tin was a kind of harmful element in iron and steel and its content must be strictly controlled.Therefore,the content of tin in iron ore should be accurately measured.The determination method of tin in iron ore by alkali fusion-iodide extraction-phenylfluorone spectrophotometry was established.The sample was fused with anhydrous sodium carbonate-boric acid(m∶m=3∶1)as mixed flux at high temperature.The molten substance was then leached with hydrochloric acid(1+5).After sulfuric acid fuming and cooling,the sample solution was diluted to certain volume.Appropriate volume of prepared solution was sampled.The potassium iodide was added and benzene was used to extract the iodide,which was then re-extracted with 0.8 mol/L sulfuric acid.The water phase was transferred into 50 mL volumetric flask.After adding phenylfluorescein and cetyl trimethylammonium bromide for coloring,the absorbance was measured using spectrophotometer at the wavelength of 535 nm.The determination range was 0.000 5%-0.20%.The spiked recoveries were between 99%and 104%.The proposed method was applied for the determination of tin in iron ore samples.The relative standard deviation(RSD,n=8)of the results was less than 4%.
引文
[1]刘伟,李超,滕晓雯,等.ICP-AES法测定钢铁中锡[J].山东冶金,2002,24(6):52-54.LIU Wei,LI Chao,TENG Xiao-wen,et al.Determination of stannum content in iron and steel with ICP-AESmethod[J].Shandong Metallurgy,2002,24(6):52-54.
[2]中华人民共和国国家质量检验检疫总局,中国国家标准化管理委员会.GB/T 6730.55-2004(ISO 11534:1998,MOD)铁矿石锡含量的测定火焰原子吸收光谱法[S].北京:中国标准出版社,2004.
[3]李海明,杨少斌.氢化物发生-原子荧光光谱法测定铁矿石中微量锡[J].光谱实验室,2005,22(2):373-375.LI Hai-ming,YANG Shao-bin.Determination of Sn in iron ore by hydride generation-atomic fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2005,22(2):373-375.
[4]蔡颖,卢艳蓉.氢化物发生原子荧光光谱法测定铁矿石中砷、锑、铋、铅、锡工作条件的确定[J].内蒙古石油化工,2014(9):8-11.CAI Ying,LU Yan-rong.Operating conditions in the determination of As,Sb,Bi,Pb and Sn in iron ores by hydridegeneration atomic fluorescence spectrometry[J].Inner Mongolia Petrochemical Industry,2014(9):8-11.
[5]中华人民共和国国家质量检验检疫总局,中国国家标准化管理委员会.GB/T 6730.34-2017铁矿石锡含量的测定邻苯二酚紫-溴化十六烷基三甲胺分光光度法[S].北京:中国标准出版社,2017.
[6]郭春山,陈凯.邻苯二酚紫(PV)-溴化十六烷基三甲铵(CTMAB)分光光度法测定铁矿石中微量锡[J].冶金分析,1982,1(11):27-28.GUO Chun-shan,CHEN Kai.Spectrophotometric determination of trace tin in iron ore by pyrocatechol violet(PV)-cetyl trimethylammonium bromide(CTMAB)[J].Metallurgical Analysis,1982,1(11):27-28.
[7]孙佩士,王振宁.CTAB-苯芴酮光度法快速测定铁矿石中微量锡[J].安阳工学院学报,2008(6):30-31.SUN Pei-shi,WANG Zhen-ning.Rapid spectrophotometric determination of trace tin in iron ore by cetyl trimethylammonium bromide(CTAB)[J].Journal of Anyang Institute of Technology,2008(6):30-31.
[8]陈小迪,于阗.过氧化氢-CTMAB-苯芴酮体系分光光度法测定矿样中的锡含量[J].化学工程与装备,2011(7):176-177.CHEN Xiao-di,YU Tian.Determination of tin in ore by hydrogen peroxide-CTMAB-benzene fluoren ketone spectrophotometry[J].Chemical Engineering&Equipment,2011(7):176-177.
[9]李伟枢,佘小芳.铁矿石中锡的X荧光光谱测定[J].冶金丛刊,1998(1):23-25.LI Wei-shu,SHE Xiao-fang.Determination of tin in iron ore by X-fluorescence spectrometry[J].Metallurgical Collections,1998(1):23-25.
[10]常玉文.X射线荧光光谱法测定铁矿石中锡[J].金属矿山,2003(5):39-40.CHANG Yu-wen.Determination of tin in iron ore by X-ray fluorescence spectrometry[J].Metal Mine,2003(5):39-40.
[2]中华人民共和国国家质量检验检疫总局,中国国家标准化管理委员会.GB/T 6730.55-2004(ISO 11534:1998,MOD)铁矿石锡含量的测定火焰原子吸收光谱法[S].北京:中国标准出版社,2004.
[3]李海明,杨少斌.氢化物发生-原子荧光光谱法测定铁矿石中微量锡[J].光谱实验室,2005,22(2):373-375.LI Hai-ming,YANG Shao-bin.Determination of Sn in iron ore by hydride generation-atomic fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2005,22(2):373-375.
[4]蔡颖,卢艳蓉.氢化物发生原子荧光光谱法测定铁矿石中砷、锑、铋、铅、锡工作条件的确定[J].内蒙古石油化工,2014(9):8-11.CAI Ying,LU Yan-rong.Operating conditions in the determination of As,Sb,Bi,Pb and Sn in iron ores by hydridegeneration atomic fluorescence spectrometry[J].Inner Mongolia Petrochemical Industry,2014(9):8-11.
[5]中华人民共和国国家质量检验检疫总局,中国国家标准化管理委员会.GB/T 6730.34-2017铁矿石锡含量的测定邻苯二酚紫-溴化十六烷基三甲胺分光光度法[S].北京:中国标准出版社,2017.
[6]郭春山,陈凯.邻苯二酚紫(PV)-溴化十六烷基三甲铵(CTMAB)分光光度法测定铁矿石中微量锡[J].冶金分析,1982,1(11):27-28.GUO Chun-shan,CHEN Kai.Spectrophotometric determination of trace tin in iron ore by pyrocatechol violet(PV)-cetyl trimethylammonium bromide(CTMAB)[J].Metallurgical Analysis,1982,1(11):27-28.
[7]孙佩士,王振宁.CTAB-苯芴酮光度法快速测定铁矿石中微量锡[J].安阳工学院学报,2008(6):30-31.SUN Pei-shi,WANG Zhen-ning.Rapid spectrophotometric determination of trace tin in iron ore by cetyl trimethylammonium bromide(CTAB)[J].Journal of Anyang Institute of Technology,2008(6):30-31.
[8]陈小迪,于阗.过氧化氢-CTMAB-苯芴酮体系分光光度法测定矿样中的锡含量[J].化学工程与装备,2011(7):176-177.CHEN Xiao-di,YU Tian.Determination of tin in ore by hydrogen peroxide-CTMAB-benzene fluoren ketone spectrophotometry[J].Chemical Engineering&Equipment,2011(7):176-177.
[9]李伟枢,佘小芳.铁矿石中锡的X荧光光谱测定[J].冶金丛刊,1998(1):23-25.LI Wei-shu,SHE Xiao-fang.Determination of tin in iron ore by X-fluorescence spectrometry[J].Metallurgical Collections,1998(1):23-25.
[10]常玉文.X射线荧光光谱法测定铁矿石中锡[J].金属矿山,2003(5):39-40.CHANG Yu-wen.Determination of tin in iron ore by X-ray fluorescence spectrometry[J].Metal Mine,2003(5):39-40.