1,2-萘醌-4-磺酸钠共振散射法测定痕量银
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摘要
以1,2-萘醌-4-磺酸钠为光谱探针,利用其与Ag(I)络合作用建立了一种共振散射法测定银含量的分析方法。在pH=5.0的Walpole(HCl-NaAc)缓冲溶液中,1,2-萘醌-4-磺酸钠溶液无明显的散射峰。当加入Ag+后,由于Ag+与1,2-萘醌-4-磺酸钠之间发生络合作用形成银络合物,使得体系在294nm处产生一个较强的共振射射峰。在最优的实验条件下,Ag+质量浓度在0.005 0～4.0μg/mL范围内与共振散射强度(ΔI)之间呈较好的线性关系;检出限为18.2ng/L。并且常见的金属离子和非金属离子不干扰Ag+的测定。该方法用于测定废胶片中痕量银,结果的相对标准偏差(RSD,n=5)为2.1%～4.8%,回收率为99%～101%,并与原子吸收光谱法(AAS)测定结果相吻合。
An analysis method of silver content by resonance scattering was established using sodium 1,2-naphthoquinone-4-sulfonate as spectral probe based on its complexation action with silver.There was no obvious scattering peak for sodium 1,2-naphthoquinone-4-sulfonate solution in Walpole(HCl-NaAc)buffer solution at pH 5.0.After adding Ag+,a complex was formed due to the complexation between Ag+and 1,2-naphthoquinone-4-sulfonate,thus generating a strong resonance scattering peak at 294 nm.Under the optimal experimental conditions,there was a good linear relationship between the resonance scattering intensity(ΔI294 nm)and the mass concentration of Ag+in range of 0.005 0-4.0μg/mL.The limit of detection was 18.2 ng/L.Moreover,the common metal ions and nonmetal ions had no interference with the determination of Ag+.The proposed method was applied for the determination of trace silver in waste film.The relative standard deviation(RSD,n=5)of results was 2.1%-4.8%.The recoveries were between99%and 101%.The determination results of this method were consistent with those obtained by atomic absorption spectrometry(AAS).
An analysis method of silver content by resonance scattering was established using sodium 1,2-naphthoquinone-4-sulfonate as spectral probe based on its complexation action with silver.There was no obvious scattering peak for sodium 1,2-naphthoquinone-4-sulfonate solution in Walpole(HCl-NaAc)buffer solution at pH 5.0.After adding Ag+,a complex was formed due to the complexation between Ag+and 1,2-naphthoquinone-4-sulfonate,thus generating a strong resonance scattering peak at 294 nm.Under the optimal experimental conditions,there was a good linear relationship between the resonance scattering intensity(ΔI294 nm)and the mass concentration of Ag+in range of 0.005 0-4.0μg/mL.The limit of detection was 18.2 ng/L.Moreover,the common metal ions and nonmetal ions had no interference with the determination of Ag+.The proposed method was applied for the determination of trace silver in waste film.The relative standard deviation(RSD,n=5)of results was 2.1%-4.8%.The recoveries were between99%and 101%.The determination results of this method were consistent with those obtained by atomic absorption spectrometry(AAS).
引文
[1]墙蔷,倪红卫,幸伟,等.银的抗菌作用机理[J].武汉科技大学学报:自然科学版,2007,30(2):121-124.QIANG Qiang,NI Hong-wei,XING Wei,et al.Antibacterial mechanism of silver[J].Journal of Wuhan University of Science and Technology:Natural Science Edition,2007,30(2):121-124.
[2]韩志辉,高寿泉,肖锡林.银-邻菲罗啉-茜素红体系共振瑞利散射法测定痕量银[J].中国卫生检查杂志,2005,15(12):1424-1426.HAN Zhi-hui,GAO Shao-quan,XIAO Xi-lin.Determ ination of silver with Ag(I)-phenanthroline-alizarin system by resonance rayleight scattering method[J].Chinese Journal of Health Aboratory Technology,2005,15(12):1424-1426.
[3]于洁玫,王西奎,国伟林,等.二苯基碳酰二肼分光光度法测定显影废液中银离子[J].冶金分析,2007,27(2):60-62.YU Jie-mei,WANG Xi-kui,GUO Wei-lin.Spectrohotometric determination of silver ion developing waste liquor with diphenylcarbazide[J].Metallurgical Analysis,2007,27(2):60-62.
[4]辛文芳.交流电弧原子发射光谱法测定锶矿石中银[J].冶金分析,2016,36(8):56-59.XIN Wen-fang.Determination of silver in strontium ore by alternating current arc atomic emission spectrometry[J].Metallurgical Analysis,2016,36(8):56-59.
[5]习霞,明亮,刘超.电化学还原石墨烯修饰玻碳电极测定痕量银[J].冶金分析,2014,34(8):7-10.XI Xia,MING Liang,LIU Chao.Determination of trace silver with electrochemically reduced-graphene modified glassy carbon electrode[J].Metallurgical Analysis,2014,34(8):7-10.
[6]冯振华,王可伟.火焰原子吸收光谱法直接测定锡阳极泥中的银[J].中国无机分析化学,2017,7(2):59-62.FENG Zhen-hua,WANG Ke-wei.Determination of silver in tin anode slime by flame atomic absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):59-62.
[7]翟好英,张学艳,阮尚全,等.曙红共振散射法测定痕量银[J].冶金分析,2009,29(12):17-20.ZHAI Hao-ying,ZHANG Xue-yan,RUAN Shang-quan,et al.Eosin resonance scattering method for the determination of trace silver[J].Metallurgical Analysis,2009,29(12):17-20.
[8]肖刘萍.灰吹富集-氯化钠电位滴定法测定贵铅中银[J].冶金分析,2018,38(3):56-60.XIAO Liu-ping.Determination of silver in noble lead by cupellation enrichment-sodium chloride potentiometric titration method[J].Metallurgical Analysis,2018,38(3):56-60.
[9]谢宇奇,凌绍明,莫秋萍,等.酚藏花红共振散射光谱法测定水中痕量亚氯酸根[J].工业水处理,2018,38(1):90-93.XIE Yu-qi,LING Shao-ming,MO Qiu-ping,et al.Determination of trace amount of chlorite by Phenosafranine resonance scattering spectrometry[J].Industrial Water Treatment,2018,38(1):90-93.
[10]陈永宁,张容珲,单展,等.锌试剂共振散射光谱新方法快速测定硫酸新霉素[J].桂林理工大学学报,2018,38(2):324-328.CHEN Yong-ning,ZHANG Rong-hui,SHAN Zhan,et al.Novel resonance light scattering method for rapid determination of neomycin sulfate by zincon[J].Journal of Guilin University of Technology,2018,38(2):324-328.
[11]范秉琳,张西军,张振轩,等.1,2-萘醌-4-磺酸钠体系分光光度法测定头孢他啶[J].分析实验室,2011,30(3):104-106.FAN Bing-lin,ZHANG Xi-jun,ZHANG Zhen-xuan,et al.Spectrophotom etric determination of ceftazidime by use sodium 1,2-naphquinone 4-sulfonate[J].Chinese Journal of Analysis Laboratory,2011,30(3):104-106.
[12]李全民,杨占军.1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑[J].分析化学,2006,34(1):83-86.LI Quan-min,YANG Zhan-jun.Spectrophotometric determination of sulfamethoxazole using sodium 1,2-naphthenquinone 4-sulfonate as the chemical derivative chromogrnic reagent[J].Chinese Journal of Analytical Chemistry,2006,34(1):83-86.
[13]王世雷,李晶,张欢欢,等.1,2-萘醌-4-磺酸钠分光光度法测定间苯二酚[J].分析试验室,2009,28(8):36-39.WANG Shi-lei,LI Jing,ZHANG Huan-huan,et al.Spectrophotometry determination of resorcinol by using sodium 1-2-naphquinone 4-sulfonate as chromogenic reagent[J].Chinese Journal of Analysis Laboratory,2009,28(8):36-39.
[14]翟好英,胡尧,张金洋.钛铁试剂共振散射法测定废胶片中的银含量[J].化学试剂,2016,38(9):875-877.ZHAI Hao-ying,HU Yao,ZHANG Jin-yang.Resonance scattering determination of silver content in waste film with tiron[J].Chemical Reagents,2016,38(9):875-877.
[15]史军,时岚.火焰原子吸收光谱法测定废水中金和银[J].理化检验:化学分册,2011,47(5):604,606.SHI Jun,SHI Lan.Determination of gold and silver in waste water by flame atomic absorption spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2011,47(5):604,606.
[2]韩志辉,高寿泉,肖锡林.银-邻菲罗啉-茜素红体系共振瑞利散射法测定痕量银[J].中国卫生检查杂志,2005,15(12):1424-1426.HAN Zhi-hui,GAO Shao-quan,XIAO Xi-lin.Determ ination of silver with Ag(I)-phenanthroline-alizarin system by resonance rayleight scattering method[J].Chinese Journal of Health Aboratory Technology,2005,15(12):1424-1426.
[3]于洁玫,王西奎,国伟林,等.二苯基碳酰二肼分光光度法测定显影废液中银离子[J].冶金分析,2007,27(2):60-62.YU Jie-mei,WANG Xi-kui,GUO Wei-lin.Spectrohotometric determination of silver ion developing waste liquor with diphenylcarbazide[J].Metallurgical Analysis,2007,27(2):60-62.
[4]辛文芳.交流电弧原子发射光谱法测定锶矿石中银[J].冶金分析,2016,36(8):56-59.XIN Wen-fang.Determination of silver in strontium ore by alternating current arc atomic emission spectrometry[J].Metallurgical Analysis,2016,36(8):56-59.
[5]习霞,明亮,刘超.电化学还原石墨烯修饰玻碳电极测定痕量银[J].冶金分析,2014,34(8):7-10.XI Xia,MING Liang,LIU Chao.Determination of trace silver with electrochemically reduced-graphene modified glassy carbon electrode[J].Metallurgical Analysis,2014,34(8):7-10.
[6]冯振华,王可伟.火焰原子吸收光谱法直接测定锡阳极泥中的银[J].中国无机分析化学,2017,7(2):59-62.FENG Zhen-hua,WANG Ke-wei.Determination of silver in tin anode slime by flame atomic absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):59-62.
[7]翟好英,张学艳,阮尚全,等.曙红共振散射法测定痕量银[J].冶金分析,2009,29(12):17-20.ZHAI Hao-ying,ZHANG Xue-yan,RUAN Shang-quan,et al.Eosin resonance scattering method for the determination of trace silver[J].Metallurgical Analysis,2009,29(12):17-20.
[8]肖刘萍.灰吹富集-氯化钠电位滴定法测定贵铅中银[J].冶金分析,2018,38(3):56-60.XIAO Liu-ping.Determination of silver in noble lead by cupellation enrichment-sodium chloride potentiometric titration method[J].Metallurgical Analysis,2018,38(3):56-60.
[9]谢宇奇,凌绍明,莫秋萍,等.酚藏花红共振散射光谱法测定水中痕量亚氯酸根[J].工业水处理,2018,38(1):90-93.XIE Yu-qi,LING Shao-ming,MO Qiu-ping,et al.Determination of trace amount of chlorite by Phenosafranine resonance scattering spectrometry[J].Industrial Water Treatment,2018,38(1):90-93.
[10]陈永宁,张容珲,单展,等.锌试剂共振散射光谱新方法快速测定硫酸新霉素[J].桂林理工大学学报,2018,38(2):324-328.CHEN Yong-ning,ZHANG Rong-hui,SHAN Zhan,et al.Novel resonance light scattering method for rapid determination of neomycin sulfate by zincon[J].Journal of Guilin University of Technology,2018,38(2):324-328.
[11]范秉琳,张西军,张振轩,等.1,2-萘醌-4-磺酸钠体系分光光度法测定头孢他啶[J].分析实验室,2011,30(3):104-106.FAN Bing-lin,ZHANG Xi-jun,ZHANG Zhen-xuan,et al.Spectrophotom etric determination of ceftazidime by use sodium 1,2-naphquinone 4-sulfonate[J].Chinese Journal of Analysis Laboratory,2011,30(3):104-106.
[12]李全民,杨占军.1,2-萘醌-4-磺酸钠体系分光光度法测定磺胺甲噁唑[J].分析化学,2006,34(1):83-86.LI Quan-min,YANG Zhan-jun.Spectrophotometric determination of sulfamethoxazole using sodium 1,2-naphthenquinone 4-sulfonate as the chemical derivative chromogrnic reagent[J].Chinese Journal of Analytical Chemistry,2006,34(1):83-86.
[13]王世雷,李晶,张欢欢,等.1,2-萘醌-4-磺酸钠分光光度法测定间苯二酚[J].分析试验室,2009,28(8):36-39.WANG Shi-lei,LI Jing,ZHANG Huan-huan,et al.Spectrophotometry determination of resorcinol by using sodium 1-2-naphquinone 4-sulfonate as chromogenic reagent[J].Chinese Journal of Analysis Laboratory,2009,28(8):36-39.
[14]翟好英,胡尧,张金洋.钛铁试剂共振散射法测定废胶片中的银含量[J].化学试剂,2016,38(9):875-877.ZHAI Hao-ying,HU Yao,ZHANG Jin-yang.Resonance scattering determination of silver content in waste film with tiron[J].Chemical Reagents,2016,38(9):875-877.
[15]史军,时岚.火焰原子吸收光谱法测定废水中金和银[J].理化检验:化学分册,2011,47(5):604,606.SHI Jun,SHI Lan.Determination of gold and silver in waste water by flame atomic absorption spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2011,47(5):604,606.