水质丁基黄原酸测定难点探讨
|
摘要
丁基黄原酸是水质监测的重要项目之一。水中丁基黄原酸的测定,在样品采集保存、前处理及仪器分析各阶段都存在一定的技术难点。实际分析时很容易出现测定结果不理想,甚至定性定量错误等问题。结合实验对丁基黄原酸测定中容易出现的问题及注意事项进行探讨,正确区分丁基黄原酸及其盐,有效保存样品,采用低损失的前处理方法以及选择性好的分析仪器,有利于提高丁基黄原酸测定的准确性。众多丁基黄原酸测定方法中,液相色谱质谱法、离子色谱法以及液相色谱法在选择性和灵敏度方面更具优势,也可用于其他方法检出丁基黄原酸时对测定进行确认。
Butylxanthic acid is one of the important indexes in water quality monitoring. There are some difficulties existed in sample collection and preservation, pretreatment and instrumental analysis of butylxanthic acid in water. Unsatisfactory results even qualitative and quantitative errors are likely to appear in actual analytical works. In order to provide references for accurate determination, easily arise problems and points for attention in determination of butylxanthic acid are reviewed in this paper. Distinguish between butylxanthic acid and butylxanthate correctly, efficient sample preservation, low loss pretreatment method, and adopt analysis method with good selectivity are beneficial for accurate determination of butylxanthic acid in water. Among the methods for detection of butylxanthic acid, liquid chromatography-mass spectrometry, ion chromatography and liquid chromatography have advantages of high selectivity and sensitivity. The three methods mentioned above can also be used to verify the existence of butylxanthic acid when it is checked out by the other methods.
Butylxanthic acid is one of the important indexes in water quality monitoring. There are some difficulties existed in sample collection and preservation, pretreatment and instrumental analysis of butylxanthic acid in water. Unsatisfactory results even qualitative and quantitative errors are likely to appear in actual analytical works. In order to provide references for accurate determination, easily arise problems and points for attention in determination of butylxanthic acid are reviewed in this paper. Distinguish between butylxanthic acid and butylxanthate correctly, efficient sample preservation, low loss pretreatment method, and adopt analysis method with good selectivity are beneficial for accurate determination of butylxanthic acid in water. Among the methods for detection of butylxanthic acid, liquid chromatography-mass spectrometry, ion chromatography and liquid chromatography have advantages of high selectivity and sensitivity. The three methods mentioned above can also be used to verify the existence of butylxanthic acid when it is checked out by the other methods.
引文
[1] 化工百科全书编委会.化工百科全书(第7卷)[M].北京:化学工业出版社,1994:637-642.
[2] 李辛夫.浮选剂黄药对蛙类胚胎的致畸毒性[J].环境科学学报,1990,10(2):212-216.LI Xinfu.Teratogenic Toxicity of Butyl Xanthate to Frog Embryos[J].Acta Scientiae Circumstantiae,1990,10(2):212-216.
[3] 张甫英.浮选剂丁基黄原酸钠对草鱼早期发育阶段的毒性效应[J].水生生物学报,1995,19(2):104-109.ZHANG Fuying.The Toxic Effects of Butyl Sodium Xanthate on the Early Development of Grass Carp,Ctenopharyngodon Idellus[J].Acta Hydrobiologica Sinica,1995,19(2):104-109.
[4] BOENING D W.Aquatic Toxicity and Environmental Fate of Xanthates[J].Mining Engineering,1998,50(9):65-68.
[5] 赵玉娥.黄药、黑药、二号油在水体中的降解试验研究[J].黄金,1995,16(7):47-51.ZHAO Yu’e.Experimental Study on Degradation of Xanthate,Aerofloat and Turpentine in Water Body[J].Gold,1995,16(7):47-51.
[6] 宋小霞,朱静,张承屏,等.黄药的研制、应用和水污染处理研究进展[J].贵州化工,2012,37(3):19-22,25.SONG Xiaoxia,ZHU Jing,ZHANG Chengping,et al.Advance in Research of Production,Application and Treatment Process of Xanthate in Dressing Wastewater[J].Guizhou Chemical Industry,2012,37(3):19-22,25.
[7] 环境保护部科技标准司.水质丁基黄原酸的测定紫外分光光度法:HJ 756—2015[S].北京:中国环境科学出版社,2015.
[8] 环境保护部科技标准司.水质丁基黄原酸的测定吹扫捕集/气相色谱-质谱法:HJ 896—2017[S].北京:中国环境科学出版社,2017.
[9] 生态环境部科技标准司.水质丁基黄原酸的测定液相色谱-三重四极杆串联质谱法:HJ 1002—2018[S].北京:中国环境科学出版社,2018.
[10] 方黎,黄洪波,吴杰,等.离子色谱法检测地表水中丁基黄原酸[J].现代科学仪器,2011(2):72-73.FANG Li,HUANG Hongbo,WU Jie,et al.Determination of Butyl Xanthate in Surface Water by Ion Chromatography[J].Modern Scientific Instruments,2011(2):72-73.
[11] 王海燕,夏勇.超高效液相色谱-串联质谱同时测定水中的敌百虫和敌敌畏[J].中国环境监测,2014,30(6):153-158.WANG Haiyan,XIA Yong.Simultaneous Determination of Trichlorfon and Dichlorvos in Water by Ultra-Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry[J].Environmental Monitoring in China,2014,30(6):153-158.
[12] 王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报,2013,32(1):32-37.WANG Chao,LYU Yibing,TENG Enjiang,et al.Determination of Trace Aniline and Benzidine in Environmental Water by Ultra High-Pressure Liquid Chromatography with Fluorescence Detection[J].Journal of Instrumental Analysis,2013,32(1):32-37.
[13] 朱红霞,刀婿,彭涛.离子色谱法测定丁基黄原酸[J].中国测试,2015,41(4):36-38.ZHU Hongxia,DAO Xu,PENG Tao.Determination of Butyl Xanthate by Ion Chromatography[J].China Measurement & Test,2015,41(4):36-38.
[14] BARNES D E,POHLANDT-WATSON C.Separation and Determination of the Sulph-Hydryl Flotation Collectors Using Ion-Interaction Chromatography[J].Fresenius’ Journal of Analytical Chemistry,1993,345(1):36-42.
[15] 贺心然,曹雷,展卫红,等.紫外分光光度法测定水中丁基黄原酸[J].环境污染与防治,2007,29(7):552-554.HE Xinran,CAO Lei,ZHAN Weihong,et al.UV Spectrophotometric Measurement of Butyl Xanthate in Water[J].Environmental Pollution & Control,2007,29(7):552-554.
[16] 栗颖明,陈雪莉.水中超痕量黄药的顶部空间气相色谱法[J].有色金属(选矿部分),1989(3):40-42.LI Yingming,CHEN Xueli.Determination of Ultra Trace Amounts of Xanthate in Water by Head-Space Gas Chromatography[J].Nonferrous Metals(Mineral Processing Section),1989(3):40-42.
[17] 杨丽莉,王美飞,李娟,等.顶空-气相色谱-质谱法测定水中痕量丁基黄原酸[J].中国环境监测,2012,28(5):64-66.YANG Lili,WANG Meifei,LI Juan,et al.Determination of Butylxanthic Acid in Water by Head-Space Gas Chromatography-Mass Spectrometry[J].Environmental Monitoring in China,2012,28(5):64-66.
[18] 王美飞,胡恩宇,杨丽莉.吹扫捕集-气相色谱-质谱法测定水中痕量丁基黄原酸[J].中国环境监测,2011,27(增刊):12-14.WANG Meifei,HU Enyu,YANG Lili,et al.Determination for Butylxanthic Acid in Water by Purge and Trap-Gas Chromatography-Mass Spectrometry[J].Environmental Monitoring in China,2011,27(Suppl):12-14.
[19] 李仁勇.离子色谱法串联紫外检测环境地表水样中的丁基黄原酸[J].环境化学,2017,36(3):688-690.Li Renyong.Determination of Butyl Xanthate in Surface Water Samples by Ion Chromatography with Ultraviolet Detection[J].Environmental Chemistry,2017,36(3):688-690.
[20] 朱红霞,白雪,黄影霞.离子色谱法测定水中的6种黄原酸盐[J].理化检验-化学分册,2016,52(9):1 065-1 067.ZHU Hongxia,BAI Xue,HUANG Yingxia.Determination of 6 Xanthates in Water by Ion Chromatography[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(9):1 065-1 067.
[21] ZHOU C S,BAHR A,SCHWEDT G.Studies on the HPLC Determination of Xanthates via Copper (I) Xanthates and Dixanthogens[J].Fresenius’ Journal of Analytical Chemistry,1989,334(6):527-533.
[22] 彭涛,王超,吕怡兵,等.超高效液相色谱法快速检测地表水中丁基黄原酸[J].中国环境监测,2013,29(2):65-68.PENG Tao,WANG Chao,LYU Yibing,et al.Rapid Analysis of Butylxanthic Acid in Surface Water by Ultra Performance Liquid Chromatography[J].Environmental Monitoring in China,2013,29(2):65-68.
[23] 张凌云.高效液相色谱法测定地表水中丁基黄原酸方法的探讨[C]//第十二次全国环境监测学术交流会论文集.北京:中国环境出版社,2015:22-26.
[24] 周岩,赵永刚,张蓓蓓,等.超高效液相色谱-三重四极杆/复合线性离子阱质谱测定水样中三苯甲烷类及代谢物[J].分析化学,2014,42(3):367-374.ZHOU Yan,ZHAO Yonggang,ZHANG Beibei,et al.Determination of Triphenylmethane Dye Residues in Water by Ultra Performance Liquid Chromatography-Triple Quadrupole Linear Ion Trap Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(3):367-374.
[25] 赵云芝,钱蜀,谢永洪,等.固相萃取-超高效液相色谱-串联质谱法测定水中6种雌激素[J].中国环境监测,2013,29(1):107-111.ZHAO Yunzhi,QIAN Shu,XIE Yonghong,et al.Determination of Six Estrogens in Water Using Solid Phase Extraction-Ulra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Environmental Monitoring in China,2013,29(1):107-111.
[26] 王静,刘铮铮,钟光剑.超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药[J].中国环境监测,2013,29(4):103-106.WANG Jing,LIU Zhengzheng,ZHONG Guangjian.Determination of Carbamates in Soil and Sediment Using UPLC-MS/MS[J].Environmental Monitoring in China,2013,29(4):103-106.
[27] 杨坪.环境样品分析新方法及其应用[M].北京:科学出版社,2010:149-151.
[28] 刘景泰,李振国.超高效液相色谱-质谱法测定地表水中丁基黄原酸[J].中国环境监测,2012,28(5):76-78.LIU Jingtai,LI Zhenguo.Determination of Butylxanthate in Ground Water by UPLC-MS[J].Environmental Monitoring in China,2012,28(5):76-78.
[2] 李辛夫.浮选剂黄药对蛙类胚胎的致畸毒性[J].环境科学学报,1990,10(2):212-216.LI Xinfu.Teratogenic Toxicity of Butyl Xanthate to Frog Embryos[J].Acta Scientiae Circumstantiae,1990,10(2):212-216.
[3] 张甫英.浮选剂丁基黄原酸钠对草鱼早期发育阶段的毒性效应[J].水生生物学报,1995,19(2):104-109.ZHANG Fuying.The Toxic Effects of Butyl Sodium Xanthate on the Early Development of Grass Carp,Ctenopharyngodon Idellus[J].Acta Hydrobiologica Sinica,1995,19(2):104-109.
[4] BOENING D W.Aquatic Toxicity and Environmental Fate of Xanthates[J].Mining Engineering,1998,50(9):65-68.
[5] 赵玉娥.黄药、黑药、二号油在水体中的降解试验研究[J].黄金,1995,16(7):47-51.ZHAO Yu’e.Experimental Study on Degradation of Xanthate,Aerofloat and Turpentine in Water Body[J].Gold,1995,16(7):47-51.
[6] 宋小霞,朱静,张承屏,等.黄药的研制、应用和水污染处理研究进展[J].贵州化工,2012,37(3):19-22,25.SONG Xiaoxia,ZHU Jing,ZHANG Chengping,et al.Advance in Research of Production,Application and Treatment Process of Xanthate in Dressing Wastewater[J].Guizhou Chemical Industry,2012,37(3):19-22,25.
[7] 环境保护部科技标准司.水质丁基黄原酸的测定紫外分光光度法:HJ 756—2015[S].北京:中国环境科学出版社,2015.
[8] 环境保护部科技标准司.水质丁基黄原酸的测定吹扫捕集/气相色谱-质谱法:HJ 896—2017[S].北京:中国环境科学出版社,2017.
[9] 生态环境部科技标准司.水质丁基黄原酸的测定液相色谱-三重四极杆串联质谱法:HJ 1002—2018[S].北京:中国环境科学出版社,2018.
[10] 方黎,黄洪波,吴杰,等.离子色谱法检测地表水中丁基黄原酸[J].现代科学仪器,2011(2):72-73.FANG Li,HUANG Hongbo,WU Jie,et al.Determination of Butyl Xanthate in Surface Water by Ion Chromatography[J].Modern Scientific Instruments,2011(2):72-73.
[11] 王海燕,夏勇.超高效液相色谱-串联质谱同时测定水中的敌百虫和敌敌畏[J].中国环境监测,2014,30(6):153-158.WANG Haiyan,XIA Yong.Simultaneous Determination of Trichlorfon and Dichlorvos in Water by Ultra-Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry[J].Environmental Monitoring in China,2014,30(6):153-158.
[12] 王超,吕怡兵,滕恩江,等.超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J].分析测试学报,2013,32(1):32-37.WANG Chao,LYU Yibing,TENG Enjiang,et al.Determination of Trace Aniline and Benzidine in Environmental Water by Ultra High-Pressure Liquid Chromatography with Fluorescence Detection[J].Journal of Instrumental Analysis,2013,32(1):32-37.
[13] 朱红霞,刀婿,彭涛.离子色谱法测定丁基黄原酸[J].中国测试,2015,41(4):36-38.ZHU Hongxia,DAO Xu,PENG Tao.Determination of Butyl Xanthate by Ion Chromatography[J].China Measurement & Test,2015,41(4):36-38.
[14] BARNES D E,POHLANDT-WATSON C.Separation and Determination of the Sulph-Hydryl Flotation Collectors Using Ion-Interaction Chromatography[J].Fresenius’ Journal of Analytical Chemistry,1993,345(1):36-42.
[15] 贺心然,曹雷,展卫红,等.紫外分光光度法测定水中丁基黄原酸[J].环境污染与防治,2007,29(7):552-554.HE Xinran,CAO Lei,ZHAN Weihong,et al.UV Spectrophotometric Measurement of Butyl Xanthate in Water[J].Environmental Pollution & Control,2007,29(7):552-554.
[16] 栗颖明,陈雪莉.水中超痕量黄药的顶部空间气相色谱法[J].有色金属(选矿部分),1989(3):40-42.LI Yingming,CHEN Xueli.Determination of Ultra Trace Amounts of Xanthate in Water by Head-Space Gas Chromatography[J].Nonferrous Metals(Mineral Processing Section),1989(3):40-42.
[17] 杨丽莉,王美飞,李娟,等.顶空-气相色谱-质谱法测定水中痕量丁基黄原酸[J].中国环境监测,2012,28(5):64-66.YANG Lili,WANG Meifei,LI Juan,et al.Determination of Butylxanthic Acid in Water by Head-Space Gas Chromatography-Mass Spectrometry[J].Environmental Monitoring in China,2012,28(5):64-66.
[18] 王美飞,胡恩宇,杨丽莉.吹扫捕集-气相色谱-质谱法测定水中痕量丁基黄原酸[J].中国环境监测,2011,27(增刊):12-14.WANG Meifei,HU Enyu,YANG Lili,et al.Determination for Butylxanthic Acid in Water by Purge and Trap-Gas Chromatography-Mass Spectrometry[J].Environmental Monitoring in China,2011,27(Suppl):12-14.
[19] 李仁勇.离子色谱法串联紫外检测环境地表水样中的丁基黄原酸[J].环境化学,2017,36(3):688-690.Li Renyong.Determination of Butyl Xanthate in Surface Water Samples by Ion Chromatography with Ultraviolet Detection[J].Environmental Chemistry,2017,36(3):688-690.
[20] 朱红霞,白雪,黄影霞.离子色谱法测定水中的6种黄原酸盐[J].理化检验-化学分册,2016,52(9):1 065-1 067.ZHU Hongxia,BAI Xue,HUANG Yingxia.Determination of 6 Xanthates in Water by Ion Chromatography[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(9):1 065-1 067.
[21] ZHOU C S,BAHR A,SCHWEDT G.Studies on the HPLC Determination of Xanthates via Copper (I) Xanthates and Dixanthogens[J].Fresenius’ Journal of Analytical Chemistry,1989,334(6):527-533.
[22] 彭涛,王超,吕怡兵,等.超高效液相色谱法快速检测地表水中丁基黄原酸[J].中国环境监测,2013,29(2):65-68.PENG Tao,WANG Chao,LYU Yibing,et al.Rapid Analysis of Butylxanthic Acid in Surface Water by Ultra Performance Liquid Chromatography[J].Environmental Monitoring in China,2013,29(2):65-68.
[23] 张凌云.高效液相色谱法测定地表水中丁基黄原酸方法的探讨[C]//第十二次全国环境监测学术交流会论文集.北京:中国环境出版社,2015:22-26.
[24] 周岩,赵永刚,张蓓蓓,等.超高效液相色谱-三重四极杆/复合线性离子阱质谱测定水样中三苯甲烷类及代谢物[J].分析化学,2014,42(3):367-374.ZHOU Yan,ZHAO Yonggang,ZHANG Beibei,et al.Determination of Triphenylmethane Dye Residues in Water by Ultra Performance Liquid Chromatography-Triple Quadrupole Linear Ion Trap Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(3):367-374.
[25] 赵云芝,钱蜀,谢永洪,等.固相萃取-超高效液相色谱-串联质谱法测定水中6种雌激素[J].中国环境监测,2013,29(1):107-111.ZHAO Yunzhi,QIAN Shu,XIE Yonghong,et al.Determination of Six Estrogens in Water Using Solid Phase Extraction-Ulra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Environmental Monitoring in China,2013,29(1):107-111.
[26] 王静,刘铮铮,钟光剑.超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药[J].中国环境监测,2013,29(4):103-106.WANG Jing,LIU Zhengzheng,ZHONG Guangjian.Determination of Carbamates in Soil and Sediment Using UPLC-MS/MS[J].Environmental Monitoring in China,2013,29(4):103-106.
[27] 杨坪.环境样品分析新方法及其应用[M].北京:科学出版社,2010:149-151.
[28] 刘景泰,李振国.超高效液相色谱-质谱法测定地表水中丁基黄原酸[J].中国环境监测,2012,28(5):76-78.LIU Jingtai,LI Zhenguo.Determination of Butylxanthate in Ground Water by UPLC-MS[J].Environmental Monitoring in China,2012,28(5):76-78.
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |