河口营养盐检测新方法应用研究
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摘要
本文的研究是针对现行的国标方法中营养盐分析方法相对落后,不能满足海洋环境管理中对监测数据快速、简单、准确的要求,建立流动注射分析测定河口水中营养盐的方法,解决流动注射技术在上海海域监测中的应用问题。上海海域位于我国最大的河口——长江口海域,是我国海洋赤潮高发和严重富营养化区域之一,是国家海洋局划定的典型河口海域赤潮监控区、绿潮监控区和生态监控区,因此营养盐是长江口海域最主要的监测项目之一。
但由于河口区处于地面水和海水的过渡性区域,盐度变化范围巨大,兼有地面水和海水的特点,而又物理化学性质复杂,借鉴流动注射测定海水中营养盐的分析方法应用于河口水营养盐监测,需要解决由于盐度变化范围大,而对分析造成的干扰的问题。
本文研究了流动注射法测定河口水中营养盐的盐效应的干扰与校正办法,和紫外光还原代替镉铜还原测定水中的硝酸盐的方法。
试验发现,流动注射测定河口水中的磷酸盐、氨氮、硅酸盐和硝酸盐,均会受到由于盐度变化大,样品折光率不同引起的纹影效应,可以通过修正样品峰的积分面积和位置,避开假峰的干扰,同时增加样品进样量体积和延长反应时间,提高方法灵敏度来克服。
研究表明,流动注射测定河口水中氨氮和硅酸盐受到较强烈动力学盐效应的干扰。氨氮的干扰主要由于镁离子浓度和离子强度变化引起,并在低盐区域(盐度0-9)和高盐区域(盐度12-30)表现不同。硅酸盐的盐效应主要由于离子强度不同引起反应速率变化。本文给出了氨氮和硅酸盐测定动力学盐效应校正系数表,样品实测浓度乘以相应的系数,为样品的真实浓度。
本文建立了紫外光还原代替镉铜还原测定河口水中的硝酸盐的方法,解决了常用的镉柱法中还原柱填装困难、使用时间短和环境污染严重的问题。
本文还对仪器和试剂条件进行了优化,应用所建立的方法分析天然水样品和国际互校样品,并与国标法进行比对验证,两种方法分析结果之间无显著性差异。
This paper research is for the flowing injection analysis technology application in the Shanghai sea area monitoring. The Shanghai sea area is located in the biggest river mouth in China- Changjiang estuary and sea area, it is one of the most red tides and serious eutrophication regions, and typical estuary sea area in China, it is selected as red tide monitoring and control area, green tide monitoring and control area, also ecology monitoring and control area by the State Ocean Administration, the nutrients salt is one of the most main monitoring parameters in the Changjiang estuary.
But because the river mouth area is the transitional region between the ground water and the sea water, the variation of salinity range is huge, the water body of the estuary has all the ground water and the sea water characteristics, and the physico-chemical properties are very complex. Use the determination method of nutrient salt in the seawater with flowing injection analyzer for reference to the estuary water, we need to solve the problems come from the variation of salinity.
This paper has studied salt effect disturbance in the FIA the nutrient salt determination method and correction of the effects. This paper also studied the nitrate determination method with ultraviolet reduction replaces the cadmium-copper column reduction.
It is found that, the analysis of phosphate, the ammonia, the silicate and the nitrate in the estuary with FIA are all disturbed by the schlieren effect, which is happened because the salinity changes in a big way, the samples’index of refraction are different. We can correct the effects from these ways: move the windows of the sample peak, escapes the position of refraction influences, simultaneously increases the sample specimen handling volume and extends reaction time, enhances the method sensitivity, so we can overcome the effect.
The research indicated that, the methods of determination ammonia and the silicate with FIA are influenced by the kinetic salt effect. The magnesium ion concentration and the ion intensity variety cause the effect when ammonia is determined. The disturbance is different between the low salinity (salinity is 0-9) and the high salinity (salinity is 12-30). The salt effect of silicate method is mainly caused by the ion intensity difference, which can affect the reaction speed.
This article has given the correction factors of kinetic salt effect in ammonia and the silicate determination methods, the samples’results need to multiply the corresponding factors.
The new method of nitrate measurement is established in this paper, which uses the ultraviolet reduction, replaces the cadmium-copper reduction. Compared to the cadmium-copper method, this new one is more excellence: operation is very simple, for cadmium-copper column must be refixed after several days, now this step is omitted, this system can run for a long time. and the most important , it does not produce pollution like cadmium .
This article also does the optimization of the instrument and the reagent conditions, applies these methods to analyse natural water sample and international intercalibration samples, the results is satisfied.
但由于河口区处于地面水和海水的过渡性区域,盐度变化范围巨大,兼有地面水和海水的特点,而又物理化学性质复杂,借鉴流动注射测定海水中营养盐的分析方法应用于河口水营养盐监测,需要解决由于盐度变化范围大,而对分析造成的干扰的问题。
本文研究了流动注射法测定河口水中营养盐的盐效应的干扰与校正办法,和紫外光还原代替镉铜还原测定水中的硝酸盐的方法。
试验发现,流动注射测定河口水中的磷酸盐、氨氮、硅酸盐和硝酸盐,均会受到由于盐度变化大,样品折光率不同引起的纹影效应,可以通过修正样品峰的积分面积和位置,避开假峰的干扰,同时增加样品进样量体积和延长反应时间,提高方法灵敏度来克服。
研究表明,流动注射测定河口水中氨氮和硅酸盐受到较强烈动力学盐效应的干扰。氨氮的干扰主要由于镁离子浓度和离子强度变化引起,并在低盐区域(盐度0-9)和高盐区域(盐度12-30)表现不同。硅酸盐的盐效应主要由于离子强度不同引起反应速率变化。本文给出了氨氮和硅酸盐测定动力学盐效应校正系数表,样品实测浓度乘以相应的系数,为样品的真实浓度。
本文建立了紫外光还原代替镉铜还原测定河口水中的硝酸盐的方法,解决了常用的镉柱法中还原柱填装困难、使用时间短和环境污染严重的问题。
本文还对仪器和试剂条件进行了优化,应用所建立的方法分析天然水样品和国际互校样品,并与国标法进行比对验证,两种方法分析结果之间无显著性差异。
This paper research is for the flowing injection analysis technology application in the Shanghai sea area monitoring. The Shanghai sea area is located in the biggest river mouth in China- Changjiang estuary and sea area, it is one of the most red tides and serious eutrophication regions, and typical estuary sea area in China, it is selected as red tide monitoring and control area, green tide monitoring and control area, also ecology monitoring and control area by the State Ocean Administration, the nutrients salt is one of the most main monitoring parameters in the Changjiang estuary.
But because the river mouth area is the transitional region between the ground water and the sea water, the variation of salinity range is huge, the water body of the estuary has all the ground water and the sea water characteristics, and the physico-chemical properties are very complex. Use the determination method of nutrient salt in the seawater with flowing injection analyzer for reference to the estuary water, we need to solve the problems come from the variation of salinity.
This paper has studied salt effect disturbance in the FIA the nutrient salt determination method and correction of the effects. This paper also studied the nitrate determination method with ultraviolet reduction replaces the cadmium-copper column reduction.
It is found that, the analysis of phosphate, the ammonia, the silicate and the nitrate in the estuary with FIA are all disturbed by the schlieren effect, which is happened because the salinity changes in a big way, the samples’index of refraction are different. We can correct the effects from these ways: move the windows of the sample peak, escapes the position of refraction influences, simultaneously increases the sample specimen handling volume and extends reaction time, enhances the method sensitivity, so we can overcome the effect.
The research indicated that, the methods of determination ammonia and the silicate with FIA are influenced by the kinetic salt effect. The magnesium ion concentration and the ion intensity variety cause the effect when ammonia is determined. The disturbance is different between the low salinity (salinity is 0-9) and the high salinity (salinity is 12-30). The salt effect of silicate method is mainly caused by the ion intensity difference, which can affect the reaction speed.
This article has given the correction factors of kinetic salt effect in ammonia and the silicate determination methods, the samples’results need to multiply the corresponding factors.
The new method of nitrate measurement is established in this paper, which uses the ultraviolet reduction, replaces the cadmium-copper reduction. Compared to the cadmium-copper method, this new one is more excellence: operation is very simple, for cadmium-copper column must be refixed after several days, now this step is omitted, this system can run for a long time. and the most important , it does not produce pollution like cadmium .
This article also does the optimization of the instrument and the reagent conditions, applies these methods to analyse natural water sample and international intercalibration samples, the results is satisfied.
引文
[1] 2007年中国海洋环境质量公报
[2] 2008年中国海洋环境质量公报
[3]海洋调查规范[M]海洋出版社,北京,2007
[4]海洋监测规范[M]海洋出版社,北京,2007
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[8]张永生,邹晓春,张曼平,等.流动注射分析( FIA)气体扩散法测定海水中的NH4-N [J].海洋环境科学,2002,21 (2):57-59.
[9]王锋,李玉环.靛酚蓝光度法测定海水中的氨型氮[J].海洋技术,2002,21(3):631-633.
[10]王萍,张新申.反相流动注射法测定海水中磷酸盐[J].环境监测管理与技术,2006, (02):26-28.
[11]王萍,张新申,吴金苗.海水磷酸盐现场自动分析化学工艺的优化[J].皮革科学与工程,2005, (01):18-21
[12]李俊,刘芳,华桂珍.流动注射光度法测定水中磷[J].环境监测管理与技术,2004,16(5):27-28
[13]王庆霞,苏苓.孔雀绿体系流动注射光度法测定水中正磷酸盐[J].环境监测管理与技术,2006,(06):28-30
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[15]高甲友.流动注射荧光猝灭法测定环境水样中痕量磷[J].环境污染与防治2003, (02):125-128
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[17]顾范博,吴士良.结晶紫-杂多酸分光光度法测定地表水中痕量磷酸盐和硅酸盐[J].江苏大学学报(医学版) 2005,15(6):.514-515
[18]李永生,高秀峰.同时测定磷酸盐/硅酸盐流动注射分析系统的研究[J].四川大学学报(工程科学版) 2008,(04):62-65
[19]赵萍,陈金辉,肖靖泽,在线镉柱还原-流动注射分析法测定水中硝酸盐/亚硝酸盐氮,《生命科学仪器》[J],2007,(6):19-22
[20]王萍,海水中PO43-、NO3-和SiO32-自动分析方法的研究,四川大学硕士学位论文,2005.6
[21]王智丽韩永辉杜振辉等,海水营养盐自动分析系统的研究[J],现代仪器,2004(2):32-34
[22] Alain Aminot , Roger Kérouel(2006), The determination of total dissolved free primary amines in seawater:Critical factors, optimized procedure and artefact correction. Mar. Chem. 98:223-240
[23]Aminot & Kerouel, Stability and preservation of primary calibration solutions of nutrients,Marine Chemistry,April 1996,Vol 52(2): 173-181
[24]高玉安,靛蓝法测氨之盐度效应的剖析和pH校正及试剂配方改良之研究,国立台湾海洋大学水产养殖研究所硕士学位论文,1999
[25]白书祯、郭廷瑜、锺仕伟、苏宗德,迭氮修正希巴辣光度测氧法及其在环境监测上的应用,化学(中国化学会志), 1998,56(3):173-185.
[26]林恒毅,自然水体中靛蓝氨氮分析法之探讨与兰阳溪氮磷物种之分布,国立台湾大学海洋研究所硕士学位论文,1999。
[27]A. Aminot, D.S. Kirkwood and R.Kerouel, Determination of ammonia in seawater by the indopgenol—blue method: Evaluation of the ICES NUTS I/C 5 questionaire[J], Mar. Chem., 1997,56, 59-75.
[28]A. Aminot and R. Kerouel, Reference material for nutrients in seawater: stability of nitrate, nitrite, ammonia and phosphate in autoclaved samples[J], Mar. Chem., 1995,49, 221-232.
[29]A. J. Kempers and C. J. Kok, Re-examination of the determination of ammonium as the indophenol blue complex using salicylate[J], Anal. Chem. Acta, 1989,221, 147-155.
[30]C. E. Bower, Ionizations of ammonia in seawater: effects of temperature, pH, and salinity[J], J. Fish. Res. Can., 1978,(35):1012-1015.
[31]C. J. Patton and S. R. Crouch, Spectrophotometric and kinetics investigation of berthelot reaction for the determination of ammonia[J], Anal. Chem., 1977,49(3), 464-469.
[32]I. Ivan & eacute; ié and Danilo Degobbis, An optimal manual procedure for ammonia analysis in natural waters by the indophenol blue method. Water Res. 1983,18(9), 1143-1147.
[33]J. Kanda, Determination of ammonium in seawater based on the indophenol reaction with O-phenylphenol (OPP) [J], Water. Res. 1995,29(12):2746-2750.
[34] J. A. Dean, ed. In Lange’s Hansbook of Chemistry, 14th ed. Mcgraw-Hill Inc. New York, 1992, p 8.91 K. Sasaki and Y. Sawada, Determination of ammonia in estuary [J],Bull. Jap. Soc. Sci. Fisheries. 1980,46(3), 319-321.
[35]L.Solórzano, Determination of ammonia in natural waters by the phenolhypochlorite method [J], Limnol. Oceanogr. 1969,5, 799-801.
[36]M. I. Liddicoat, S. Tibbets and E. L. Butler, The determination of ammonia in seawater. Limnol. Oceanogr., 1975,20, 131-132.
[37]S. C. Pai, Y. J. Tsau and T. I. Yang, pH and buffering capacity problems involved in the determination of ammonia in saline water using the indophenol blue spectrophotometric method. [J] Anal. Chim. Acta 2001,434(2), 209-216.
[38]W. T. Bolleter, C. J. Bushman, and P. W. Tidwell, Spectrophotometric determination of ammonia as indophenol[J], Anal. Chem., 1961,33(4), 592-594
[39]Y. Nimura, Adirect estimation of microgram amounts of ammonia in water without salt-error[J],Bull. Jap. Soc. Sci. 1973,39(12):1315-1324.
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[41]姚庆祯,范燕,谭加强等.超声波锌(卷)-镉法测定天然水中的硝酸盐,海洋科学[J], 1999,(6):11-13.
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[43]锺仕伟、温良硕、庄佳颖、苏宗德,盐度效应对营养盐测定之影响[J],The Chinese Chem. SOC. Taipei, 2001,59(3):311-316.
[44]Iwaji Iwasaki and Toshikazu Tarutani,Silica in Water. V. Salt Effect on the Colorimetric Determination of Silica in Concentrated Salt Solution[J],Bulletin of the Chemical Society of Japan, 1959, 32 (1):32-36
[1]海洋监测规范[M]海洋出版社,北京,2007
[2]李俊,刘芳,华桂珍.流动注射光度法测定水中磷[J].环境监测管理与技术2004,(05): 29-30
[3]王庆霞,苏苓.孔雀绿体系流动注射光度法测定水中正磷酸盐[J].环境监测管理与技术2006,(06):28-30
[4]赵卫红,焦念志,赵增霞.海水中总氮和总磷的同时测定[J].海洋科学,1999,(5):64-66
[5]王萍,张新申.反相流动注射法测定海水中磷酸盐[J].环境监测管理与技术2006,(2):26-28.
[6]王萍,张新申,吴金苗.海水磷酸盐现场自动分析化学工艺的优化[J].皮革科学与工程2005,(01):18-21
[7]王萍,海水中PO43-、NO3-和SiO32-自动分析方法的研究,四川大学硕士学位论文,2005.6
[8]高甲友.流动注射荧光猝灭法测定环境水样中痕量磷[J].环境污染与防治2003, (02):125-128
[9]顾范博,吴士良.结晶紫-杂多酸分光光度法测定地表水中痕量磷酸盐和硅酸盐[J].江苏大学学报(医学版)2005,15(6):.514-515
[10]李永生,高秀峰.同时测定磷酸盐/硅酸盐流动注射分析系统的研究[J].四川大学学报(工程科学版)2008,(04):63-35
[11] J. P. Riley and R. Chester, Introduction to Marine Chesmistry, Academic Press, London, New York, San Francisco, 1971, p 465
[12]B. M. Stewart and P. A. W. Elliott,Systematic salt effects in the automated determination of nutrients in seawater[J],Water Research,April 1996,30(4): 869-874
[13]锺仕伟、温良硕、庄佳颖、苏宗德,盐度效应对营养盐测定之影响[J],The Chinese Chem. SOC. Taipei, 2001,59(3):311-316.
[14] Alain Aminot* and Roger Kérouel ,An automated photo-oxidation method for the determination of dissolved organic phosphorus in marine and fresh water[J] Marine Chemistry October 2001; 76 (1-2) : 113-126
[1]水质铵的测定纳氏试剂比色法,GB7479-97
[2]海洋调查规范[M]海洋出版社,北京,2007
[3]海洋监测规范[M]海洋出版社,北京,2007
[4]余翔翔,郭卫东海水中低含量氨氮的高灵敏度荧光法测定[J],海洋科学2007, 31(4) :37-41
[5]江伟武.河口水质氨氮的自动监测影响因素研究[J].中国环境监测,2004,20(3):12-13.
[6]王锋,李玉环.靛酚蓝光度法测定海水中的氨型氮[J].海洋技术,2002,21(3):631-633.
[7]Aminot & Kerouel, Stability and preservation of primary calibration solutions of nutrients,Marine Chemistry,April 1996, 52(20): 173-181.
[8]高玉安,靛蓝法测氨之盐度效应的剖析和pH校正及试剂配方改良之研究。国立台湾海洋大学水产养殖研究所硕士学位论文,1999
[9]白书祯、郭廷瑜、锺仕伟等迭氮修正希巴辣光度测氧法及其在环境监测上的应用,化学(中国化学会志), 1998,56(3):173-185.
[10]林恒毅,自然水体中靛蓝氨氮分析法之探讨与兰阳溪氮磷物种之分布,国立台湾大学海洋研究所硕士学位论文,1999.
[11]A. Aminot, D.S. Kirkwood and R.Kerouel, Determination of ammonia in seawater by the indopgenol—blue method: Evaluation of the ICES NUTS I/C 5 questionaire[J], Mar. Chem., 1997,56:59-75.
[12]A. Aminot and R. Kerouel, Reference material for nutrients in seawater: stability of nitrate, nitrite, ammonia and phosphate in autoclaved samples[J], Mar. Chem., 1995,49:221-232.
[13]A. J. Kempers and C. J. Kok, Re-examination of the determination of ammonium as the indophenol blue complex using salicylate[J], Anal. Chem. Acta, 1989,221: 147-155.
[14]C. E. Bower, Ionizations of ammonia in seawater: effects of temperature, pH, and salinity[J], J. Fish. Res. Can., 1978,35: 1012-1015.
[15]C. J. Patton and S. R. Crouch, Spectrophotometric and kinetics investigation of berthelot reaction for the determination of ammonia[J], Anal. Chem., 1977,49(3):464-469.
[16]I. Ivan & eacute; ié and Danilo Degobbis, An optimal manual procedure for ammonia analysis in natural waters by the indophenol blue method. Water Res. 1983,18(9): 1143-1147.
[17]J. Kanda, Determination of ammonium in seawater based on the indophenol reaction withO-phenylphenol (OPP) [J], Water. Res. , 1995,29(12):2746-2750.
[18] Sasaki and Y. Sawada, Determination of ammonia in estuary [J],Bull. Jap. Soc. Sci. Fisheries.1980,46(3):319-321.
[19]L.Solórzano, Determination of ammonia in natural waters by the phenolhypochlorite method [J], Limnol. Oceanogr. 1969,5:799-801.
[20]M. I. Liddicoat, S. Tibbets and E. L. Butler, The determination of ammonia in seawater. Limnol. Oceanogr., 1975,20:131-132.
[21]S. C. Pai, Y. J. Tsau and T. I. Yang, pH and buffering capacity problems involved in the determination of ammonia in saline water using the indophenol blue spectrophotometric method. [J],Anal. Chim. Acta 2001,434(2):209-216.
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