顺序注射—分光光度法测定水中挥发酚的研究
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摘要
挥发酚是一类对人体和环境都有害的有机污染物,是欧共体国家和我国饮水中的必测项目,因此,建立灵敏、简单、快速的挥发酚分析方法用于分析环境水中的挥发酚具有极其重要的意义。
论文的第一部分介绍了水质监测的发展状况、挥发酚的分析现状及顺序注射技术在水质监测中的应用。
论文的第二部分结合顺序注射技术方便快速、重现性好、样品消耗量少以及样品交叉污染少、自动化程度高的特点,建立了在线蒸馏-顺序注射与分光光度法联用的技术,用于测定水中的挥发酚。实验中采用2.5 mL的样品进行在线蒸馏,馏出液在碱性条件和铁氰化钾存在的条件下,用4-氨基安替比林进行显色,显色后溶液的吸光度与挥发酚溶液的浓度在0.05-8.0 mg/L范围内呈线性关系,该方法的检出限为0.01 mg/L,对2.0 mg/L的挥发酚标准溶液进行9次平行测定的相对标准偏差为1.5%,测定了实际水样并进行了加标回收实验,回收率在96%-106%之间。
论文的第三部分建立了顺序注射-固相萃取分离富集与分光光度法联用的技术,用于测定水样中低浓度的挥发酚。实验中选择Amberlite XAD-7树脂为吸附材料对显色后的挥发酚溶液进行吸附,并用乙醇溶液进行洗脱。在4 mL的进样体积下,方法的线性范围在0.004-0.3 mg/L之间,检出限为0.002 mg/L,对0.1 mg/L的挥发酚溶液进行9次平行测定,相对标准偏差为1.4%,对实际水样中的挥发酚进行了加标回收实验,回收率在96%-102%之间。
论文第四部分对实验内容进行了简单总结。
Volatile phenolic compounds are toxic organic substances to human health and the biotic environment, which are strictly regulated by both China and International commumities. Therefore, the development of sensitive, simple and fast methods for their determination is highly demanded, especially for environmental water quality monitoring.
The first section of the dissertation reviewed of the current situation for water quality monitoring and the analytical methods for the determination of volatile phenolic compounds. In addition, the application of sequential injection in water quality monitoring is also discussed.
The second part of the dissertation developed a sequential injection on-line distillation procedure for the determination of volatile phenolic compounds with detection by spectrophotometry, by taking the advantages of sequential injection system in terms of rapidness, repeatability, minimized sample consumption and cross contamination as well as automation. A 2.5mL sample solution was used for on-line distillation, and the distillate reacts with 4-aminoantipyrine and potassium ferricyanide to form a red substance in NH3-NH4Cl buffer solution. The absorbance of the reaction product is proportional to the concentration of phenol in the range 0.05-8.0 mg/L, giving rise to a detection of 0.01 mg/L. The relative standard deviation is 1.5% at the concentration level of 2.0 mg/L. The method was applied to the determination of volatile phenolic compounds in waste waters and the recoveries are within the range of 96%-106%.
The last part of the dissertation developed a procedure for per-concentration of low level of volatile phenolic compounds by employing solid-phase extraction in a sequential injection system with detection by spectrophotometry. The red substance which was formed by the reaction of phenol and 4-aminoantipyrine and potassium ferricyanide in NH3-NH4Cl buffer solution can be efficiently adsorbed by an Amberlite XAD-7 resin packed microcolumn, which can be afterwards effectly by a small amount of ethanol. With a sample loading volume of 4 mL, a linear range of 0.004-0.3 mg/L was obtained, with a detection limit is 0.002 mg/L, A relative standard deviation of 1.4% is achieved at 0.1 mg/L. The procedure was applied to the determination of low volatile phenolic compounds in water samples and spiking recoveries within 96%-102% were obtained.
In the last section, a summary for content of the experimentation was described.
论文的第一部分介绍了水质监测的发展状况、挥发酚的分析现状及顺序注射技术在水质监测中的应用。
论文的第二部分结合顺序注射技术方便快速、重现性好、样品消耗量少以及样品交叉污染少、自动化程度高的特点,建立了在线蒸馏-顺序注射与分光光度法联用的技术,用于测定水中的挥发酚。实验中采用2.5 mL的样品进行在线蒸馏,馏出液在碱性条件和铁氰化钾存在的条件下,用4-氨基安替比林进行显色,显色后溶液的吸光度与挥发酚溶液的浓度在0.05-8.0 mg/L范围内呈线性关系,该方法的检出限为0.01 mg/L,对2.0 mg/L的挥发酚标准溶液进行9次平行测定的相对标准偏差为1.5%,测定了实际水样并进行了加标回收实验,回收率在96%-106%之间。
论文的第三部分建立了顺序注射-固相萃取分离富集与分光光度法联用的技术,用于测定水样中低浓度的挥发酚。实验中选择Amberlite XAD-7树脂为吸附材料对显色后的挥发酚溶液进行吸附,并用乙醇溶液进行洗脱。在4 mL的进样体积下,方法的线性范围在0.004-0.3 mg/L之间,检出限为0.002 mg/L,对0.1 mg/L的挥发酚溶液进行9次平行测定,相对标准偏差为1.4%,对实际水样中的挥发酚进行了加标回收实验,回收率在96%-102%之间。
论文第四部分对实验内容进行了简单总结。
Volatile phenolic compounds are toxic organic substances to human health and the biotic environment, which are strictly regulated by both China and International commumities. Therefore, the development of sensitive, simple and fast methods for their determination is highly demanded, especially for environmental water quality monitoring.
The first section of the dissertation reviewed of the current situation for water quality monitoring and the analytical methods for the determination of volatile phenolic compounds. In addition, the application of sequential injection in water quality monitoring is also discussed.
The second part of the dissertation developed a sequential injection on-line distillation procedure for the determination of volatile phenolic compounds with detection by spectrophotometry, by taking the advantages of sequential injection system in terms of rapidness, repeatability, minimized sample consumption and cross contamination as well as automation. A 2.5mL sample solution was used for on-line distillation, and the distillate reacts with 4-aminoantipyrine and potassium ferricyanide to form a red substance in NH3-NH4Cl buffer solution. The absorbance of the reaction product is proportional to the concentration of phenol in the range 0.05-8.0 mg/L, giving rise to a detection of 0.01 mg/L. The relative standard deviation is 1.5% at the concentration level of 2.0 mg/L. The method was applied to the determination of volatile phenolic compounds in waste waters and the recoveries are within the range of 96%-106%.
The last part of the dissertation developed a procedure for per-concentration of low level of volatile phenolic compounds by employing solid-phase extraction in a sequential injection system with detection by spectrophotometry. The red substance which was formed by the reaction of phenol and 4-aminoantipyrine and potassium ferricyanide in NH3-NH4Cl buffer solution can be efficiently adsorbed by an Amberlite XAD-7 resin packed microcolumn, which can be afterwards effectly by a small amount of ethanol. With a sample loading volume of 4 mL, a linear range of 0.004-0.3 mg/L was obtained, with a detection limit is 0.002 mg/L, A relative standard deviation of 1.4% is achieved at 0.1 mg/L. The procedure was applied to the determination of low volatile phenolic compounds in water samples and spiking recoveries within 96%-102% were obtained.
In the last section, a summary for content of the experimentation was described.
引文
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