分光光度计的改装及在锑测定中的应用
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摘要
试样以硫酸分解,在硫酸(1+4)中加入碘化钾,Sb3+与碘化钾形成[SbI4]-黄色络合物,在改装后分光光度计上测量吸光度,建立快速测定锑的方法。Sb3+质量在0~250μg范围内符合朗伯比尔定律,回归方程为y=0.945 6 x+0.002 3,线性相关系数r=0.999 7。方法适用于样品中1.00%以下锑的测定。按照实验方法测定地质样等不同样品中锑,结果的相对标准偏差(RSD,n=6)为2.1%~6.8%。并与国标法GB/T 15925-2010及改进前分光光度计和目视比色法的测定结果相吻合。
The sample was decomposed with sulfuric acid.After adding potassium iodide into sulfuric acid(1+4),Sb3+would react with potassium iodide to form yellow [SbI4]-complex.The absorbance was measured on a modified spectrophotometer,and the rapid determination method of antimony was established.Beer's law was obeyed for Sb3+in range of 0-250μg.The regression equation was y=0.945 6 x+0.002 3with correlation coefficient of r=0.999 7.The proposed method was applicable for the determination of antimony in sample with content lower than 1.00%.The content of antimony in different geological samples was determined according to the experimental method.The relative standard deviations(RSD,n=6)were between 2.1% and 6.8%.The found results were consistent with those obtained by national standard method(GB/T 15925-2010)as well as unmodified spectrophotometer and visual colorimetry.
The sample was decomposed with sulfuric acid.After adding potassium iodide into sulfuric acid(1+4),Sb3+would react with potassium iodide to form yellow [SbI4]-complex.The absorbance was measured on a modified spectrophotometer,and the rapid determination method of antimony was established.Beer's law was obeyed for Sb3+in range of 0-250μg.The regression equation was y=0.945 6 x+0.002 3with correlation coefficient of r=0.999 7.The proposed method was applicable for the determination of antimony in sample with content lower than 1.00%.The content of antimony in different geological samples was determined according to the experimental method.The relative standard deviations(RSD,n=6)were between 2.1% and 6.8%.The found results were consistent with those obtained by national standard method(GB/T 15925-2010)as well as unmodified spectrophotometer and visual colorimetry.
引文
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[10]张炜炜.碘化钾分光光度法测定ZL101A中锑的含量[J].科技信息,2010(21):454.ZHANG Wei-wei.KI Spectrophotometric method to determine the size of antimony in the level of ZL101A[J].Science&Technology Information,2010(21):454.
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[12]王金峰,邢晓明.7522自动进样器与722分光光度计配套使用时出现的问题和解决方法[J].中国医疗器械杂志(Chinese Journal of Medical Instrumentation),1997(6):363-364.
[13]贺国庆,李晓慧.分光光度计比色装置的改进[J].分析仪器,2001(1):22-23.HE Guo-qing,LI Xiao-hui.Improvement of colorimetric device of spectrophotometer[J].Analytical Instrumentation,2001(1):22-23.
[14]毕明文.722型光栅分光光度计的应用现状及改进[J].中国计量(China Metrology),2003(3):46.
[2]韩宗才,关弘弢.原子荧光光谱法测定合金钢中锑[J].光谱实验室,2014,31(2):281-283.HAN Zong-cai,GUAN Hong-tao.Determination of antimony in steel alloys by AFS[J].Chinese Journal of Spectroscopy Laboratory,2014,31(2):281-283.
[3]袁永海,尹昌慧,元志红,等.氢化物发生-原子荧光光谱法同时测定锡矿石中砷和锑[J].冶金分析,2016,36(3):39-43.YUAN Yong-hai,YIN Chang-hui,YUAN Zhi-hong,et al.Determination of arsenic and antimony in tinore by hydridegeneration-atomic fluorescence spectrometry[J].Metallurgical Analysis,2016,36(3):39-43.
[4]马新荣,马生凤,王蕾,等.王水溶矿-等离子体光谱法测定砷矿石和锑矿石中砷锑硫铜铅锌[J].岩矿测试,2011,30(2):190-194.MA Xin-rong,MA Sheng-feng,WANG Lei,et al.Determination of As,Sb,S,Cu,Pb,Zn in arsenic ore and stibium ore by inductively coupled plasma-atomic emission spectrometry with aqua regia digestion[J].Rock and Mineral Analysis,2011,30(2):190-194.
[5]魏灵巧,付胜波,罗磊,等.电感耦合等离子体发射光谱法多向观测同时测定锑矿石中锑砷铜铅锌[J].岩矿测试,2012,31(6):967-970.WEI Ling-qiao,FU Sheng-bo,LUO Lei,et al.Simultaneous determination of Sb,As,Cu,Pb and Zn in antimony oresby inductively coupled plasma-atomic emission spectrometry with a multi-directional observation mode[J].Rock and Mineral Analysis,2012,31(6):967-970.
[6]张光华.电感耦合等离子体原子发射光谱法测定纯银中镉铋铁铅锑钯[J].中国无机分析化学,2013,3(2):63-65.ZHANG Guang-hua.Determination of Cd,Bi,Fe,Pb,Sb,Pd,Se,Te in silver by inductively coupled plasmaatomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(2):63-65.
[7]任志海,牟思名,程功,等.王水密闭溶矿电感耦合等离子体原子发射光谱法测定锑矿石中的锑[J].中国无机分析化学,2014,4(1):53-55.REN ZHi-hai,MU Si-ming,CHENG Gong,et al.Determination of Sb in stibium ore by inductively coupied plasma-atomic emission spectrometry with ciosed digestion using aqua regia[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(1):53-55.
[8]陈丽梅,谢明丽,罗正波,等.ICP-AES直接测定粗铅中锑、铜、铋[J].湖南有色金属,2016,32(2):74-76.CHEN Li-mei,XIE Ming-li,LUO Zheng-bo,et al.Determination method of antimony,copper and bismuth in crude lead by ICP-AES[J].Hunan Nonferrous Metals,2016,32(2):74-76.
[9]张志喜,黄惠琴.电感耦合等离子体质谱法测定地球化学样品中的银砷锑铋[J].中国无机分析化学,2014,4(4):46-49.ZHANG Zhi-xi,HUANG Hui-qin.Determination of silver,arsenic,antimony and bismuth in geochemical samples using inductively coupled plasma mass spectrometry together with aqua regia decomposition[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(4):46-49.
[10]张炜炜.碘化钾分光光度法测定ZL101A中锑的含量[J].科技信息,2010(21):454.ZHANG Wei-wei.KI Spectrophotometric method to determine the size of antimony in the level of ZL101A[J].Science&Technology Information,2010(21):454.
[11]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 15925—2010锑矿石化学分析方法锑量测定[S].北京:中国标准出版社出版,2010.
[12]王金峰,邢晓明.7522自动进样器与722分光光度计配套使用时出现的问题和解决方法[J].中国医疗器械杂志(Chinese Journal of Medical Instrumentation),1997(6):363-364.
[13]贺国庆,李晓慧.分光光度计比色装置的改进[J].分析仪器,2001(1):22-23.HE Guo-qing,LI Xiao-hui.Improvement of colorimetric device of spectrophotometer[J].Analytical Instrumentation,2001(1):22-23.
[14]毕明文.722型光栅分光光度计的应用现状及改进[J].中国计量(China Metrology),2003(3):46.