多组分体系中比光谱导数分析方法的研究
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摘要
本论文对国内外分光光度法测定多组分的研究，特别是对比光谱导数分光光度法测定多组分研究进行了综述，并根据其原理开发研制了多组份比光谱导数分光光度法处理软件。在此基础上应用此软件对无机混合体系中Ca、Mg二组分，Ca、Mg、Sr三组分和有机混合体系中苯酚、对甲基酚、对硝基酚三组分的分析方法进行了研究，得到的主要成果有以下几点：
1．我们根据比光谱导数法同时测定混合体系多组份的原理，采用Visual Basic语言自行编写了分别适用于同时测定二组分或三组分的数据处理软件。该软件界面友好，清晰明了，操作简单，使用方便，方便用户浏览和使用，避免了大量繁琐的人工计算过程。我们还建立了该软件的安装程序和辅助的帮助文件，通过光盘用户可自行安装使用。经过实验验证，应用该软件可以得到令人满意的结果。
2．本文建立了以偶氮胂Ⅲ为显色剂用比光谱导数法同时测定Ca、Mg二组分的新方法，确定了实验的最佳条件，使Ca、Mg的测定更加快捷方便。该方法测定混合物中钙、镁的相对标准偏差(精密度)分别是0.76％、0.63％，回收率Ca在97.8％—103％、Mg在98.4％—102％范围内波动，Ca-偶氮胂(Ⅲ)在浓度0—60μg／25ml内，Mg-偶氮胂(Ⅲ)在浓度0—50μg／25ml内符合比耳定律，检出限分别为0.16μg／25ml、0.13μg／25ml。将该方法应用于实际体系，得到了令人满意的结果。
3．本文用两种数据处理方法：即双除数因子比光谱导数处理方法和零交点比光谱导数处理方法对三组分混合溶液分析结果进行处理和比较，结果表明：(1)从数学解析原理上来看，双除数因子法和零交点法各有优点；(2)在分析处理过程中，后者要比前者相对简单一些；(3)从数据处理结果上来看，前者好于后者。经过综合比较，实验中我们选择双除数因子比光谱导数法用于同时测定三组分混
多组分体系中比光谱导数分析方法的研究
合体系。
4.本文首次用分光光度法对Ca、Mg、Sr三组分混合溶液同时测定进行了
研究，采用双除数因子比光谱导数法进行数据处理，确定了实验的最佳条件，取
得了令人满意的结果。本方法中钙、镁、银络合物的最大吸收波长分别是652nm、
619nm、646tun，显色剂用量sml，缓冲溶液用量3ml，显色时间大于15mins，计
算波长分别为652nrn、638nm、657lun。本方法测定混合物中钙、镁、铭的相对
标准偏差(精密度)分别是0.85%、0.82%、0.82%，Ca-偶氮肿(m)在浓度0--
60夕g/25ml内，Mg一偶氮肿(111)在浓度任一50夕叭sml内，Sr-偶氮肿(111)在浓
度0一60夕创25ml内符合比耳定律，测定的相对偏差分别在0.3%一2.4%、0.05%
一2.3%、0.4%一3.4%范围内波动，检出限分别为0.16夕留25ml、0.16夕g/25ml、0.16
夕g/25ml。
5.本文首次应用双除数因子比光谱导数法同时测定了苯酚、对甲基酚、对
硝基酚三组分有机混合体系，并确定了实验的最佳条件，取得了令人满意的结果。
本方法中，苯酚、对甲基酚、对硝基酚的最大吸收波长分别是Znrun、220nm、
227nm，计算波长分别为202nm、1 99nm、245nln。苯酚在O~33.6m叭、对甲基
酚在O一33.6m留L、对硝基酚在o一38.4m留L内符合比尔定律，检出限分别为
0.018mg/L、0.O22mg/L、0.O22mg/L。本方法测定混合溶液中苯酚、对甲基酚、对
硝基酚的相对标准偏差(精密度)分别是0.79%、0.89%、0.93%相对偏差分别
在0.4%一1 .7%、0.7%一3.7%、0.1%一3.3%范围内波动。
6.本文应用所建立的方法测定了2002年下半年山东利津站黄河水Ca、Mg含量
的月变化和青岛5条河流及4个河口区Ca、Mg的含量以及海水中Ca、Mg的含
量。测定结果与络合滴定法进行了比较，取得一致的结果，并且在低含量时，本
方法的结果要好于络合滴定法。
This thesis reviewed the researches about spectrophotometric method, especially simultaneous multicomponent determine method such as ratio spectrum and derivative spectrophotometric method. According to the theory of ratio spectrum and derivative spectrophotometric method , we developed "multicomponent ratio spectrum and derivative spectrophotometric method analysis software". On this basis , we applied this software to research the analysis method of inorganic binary mixtures-Ca2+, Mg2+,ternary mixtures-Ca2+, Mg2+, Sr2+and organic ternary mixtures-phenol, p-methylphenol , p-nitrophenol, and mainly obtained following several results:
1. According to ratio spectrum derivative method, we programmed the data processing software using Visual Basic. This software can be used to process both binary component and ternary component and it is easy to use. With the help of the software, we can avoid much computing work and can accelerate data processing. We made a setup program for the other users to use. We can got a satisfactory result with the software which has been validated by experiment.
2. We set up a new method using ratio spectrum and derivative simultaneous determineation Ca2+ and Mg2+ using ArsenazoIII as color reagent. We also got the optimum experimental conditions and made the determination easier than the traditional method. The precision for Ca2+ and Mg2+ is 0.76% and 0.63% respectively. The recovery rate is 97.8%-103% for calcium and 98.4%-102% for magnesium. The Beer's law is obeyed in the range of 0-60 g/25ml for calcium and 0-50 g/25ml for magnesium. The detection limitation for Ca2+and Mg2+ is 0.16 g/25ml and 0.13 g/25ml respectively, we applied this method for the analysis of natural water samples and got satisfactory
results.
3. The double divisor-ration spectra derivative method and the ratio spectra-zero crossing method are both used to analyze ternary mixtures. The result indicates that the double divisor-ration spectra derivative method is better than the ratio spectra-zero crossing method in the aspects of mathymatics theory and data results. So we chose the double divisor-ration spectra derivative method as our analysis method.
4. we studied simultaneous determination of Ca2+, Mg2+ and Sr2+ mixtures using spectrophotometric method for the first time and got satisfactory results. We determined the optimum experimental conditions followed here. The maximum wavelength is 625nm for Ca2+ , 619nm for Mg2+ and 646nm for Sr2+. The volume of color reagent is 5ml and reaction time is ISmins. The buffer solution volume is 3ml. The computation wavelength is 652nm for Ca2+, 638nm for Mg2+and 657nm for Sr2+. The precision for Ca2+,Mg2, Sr^is 0.72% , 0.68% and 2.10% respectively. The relative deviation is 0.3% -2.4% for Ca2+, 0.05%-2.3% for Mg2+ and 0.4%-3.4% for Sr2+. The Beer' s law is obeyed in the range of 0-60ug/25ml for Ca2+> 0-50ug/25ml for Mg2+and 0-60ug/25ml for Sr2+.The detection limitation for Ca2+ ,Mg2, Sr2+ is 0.16ug/25mK 0.16???g/25ml and 0.16 g/25ml respectively.
5. We applied double divisor-ration spectra derivative method to determine simultaneously ternary mixtures-phenol, p-methylphenol ,p-nitrophenol for the first time. The optimum experimental conditions and satisfactory results were obtained. The maximum wavelength is 211 nm for phenol, 220nm for p-methylphenol and 227nm for p-nitrophenol.. The Beer' s law is obeyed in the range of 0-33.6mg/L for phenol, 0-33.6mg/L for p-methylphenol and 0-38.4mg/L for p-nitrophenol. The detection limitation is 0.018mg/L, 0.022mg/L and 0.022mg/L. The precision for phenol, p-methylphenol ,p-nitrophenol is 0.79%> 0.89% and 0.93% respectively. The relative deviation is 0.4%-1.7%, 0.7%-3.7% and 0.1%-3.3% respectively.
6. We applied the proposed method to determine concentrations of calcium and magnesium of nature water samples collected from Yellow river at Lijin station, Shandong province. We also analyzed samples from 5 rivers and 4 bayous of Qingdao. The result was similar with that d
1．我们根据比光谱导数法同时测定混合体系多组份的原理，采用Visual Basic语言自行编写了分别适用于同时测定二组分或三组分的数据处理软件。该软件界面友好，清晰明了，操作简单，使用方便，方便用户浏览和使用，避免了大量繁琐的人工计算过程。我们还建立了该软件的安装程序和辅助的帮助文件，通过光盘用户可自行安装使用。经过实验验证，应用该软件可以得到令人满意的结果。
2．本文建立了以偶氮胂Ⅲ为显色剂用比光谱导数法同时测定Ca、Mg二组分的新方法，确定了实验的最佳条件，使Ca、Mg的测定更加快捷方便。该方法测定混合物中钙、镁的相对标准偏差(精密度)分别是0.76％、0.63％，回收率Ca在97.8％—103％、Mg在98.4％—102％范围内波动，Ca-偶氮胂(Ⅲ)在浓度0—60μg／25ml内，Mg-偶氮胂(Ⅲ)在浓度0—50μg／25ml内符合比耳定律，检出限分别为0.16μg／25ml、0.13μg／25ml。将该方法应用于实际体系，得到了令人满意的结果。
3．本文用两种数据处理方法：即双除数因子比光谱导数处理方法和零交点比光谱导数处理方法对三组分混合溶液分析结果进行处理和比较，结果表明：(1)从数学解析原理上来看，双除数因子法和零交点法各有优点；(2)在分析处理过程中，后者要比前者相对简单一些；(3)从数据处理结果上来看，前者好于后者。经过综合比较，实验中我们选择双除数因子比光谱导数法用于同时测定三组分混
多组分体系中比光谱导数分析方法的研究
合体系。
4.本文首次用分光光度法对Ca、Mg、Sr三组分混合溶液同时测定进行了
研究，采用双除数因子比光谱导数法进行数据处理，确定了实验的最佳条件，取
得了令人满意的结果。本方法中钙、镁、银络合物的最大吸收波长分别是652nm、
619nm、646tun，显色剂用量sml，缓冲溶液用量3ml，显色时间大于15mins，计
算波长分别为652nrn、638nm、657lun。本方法测定混合物中钙、镁、铭的相对
标准偏差(精密度)分别是0.85%、0.82%、0.82%，Ca-偶氮肿(m)在浓度0--
60夕g/25ml内，Mg一偶氮肿(111)在浓度任一50夕叭sml内，Sr-偶氮肿(111)在浓
度0一60夕创25ml内符合比耳定律，测定的相对偏差分别在0.3%一2.4%、0.05%
一2.3%、0.4%一3.4%范围内波动，检出限分别为0.16夕留25ml、0.16夕g/25ml、0.16
夕g/25ml。
5.本文首次应用双除数因子比光谱导数法同时测定了苯酚、对甲基酚、对
硝基酚三组分有机混合体系，并确定了实验的最佳条件，取得了令人满意的结果。
本方法中，苯酚、对甲基酚、对硝基酚的最大吸收波长分别是Znrun、220nm、
227nm，计算波长分别为202nm、1 99nm、245nln。苯酚在O~33.6m叭、对甲基
酚在O一33.6m留L、对硝基酚在o一38.4m留L内符合比尔定律，检出限分别为
0.018mg/L、0.O22mg/L、0.O22mg/L。本方法测定混合溶液中苯酚、对甲基酚、对
硝基酚的相对标准偏差(精密度)分别是0.79%、0.89%、0.93%相对偏差分别
在0.4%一1 .7%、0.7%一3.7%、0.1%一3.3%范围内波动。
6.本文应用所建立的方法测定了2002年下半年山东利津站黄河水Ca、Mg含量
的月变化和青岛5条河流及4个河口区Ca、Mg的含量以及海水中Ca、Mg的含
量。测定结果与络合滴定法进行了比较，取得一致的结果，并且在低含量时，本
方法的结果要好于络合滴定法。
This thesis reviewed the researches about spectrophotometric method, especially simultaneous multicomponent determine method such as ratio spectrum and derivative spectrophotometric method. According to the theory of ratio spectrum and derivative spectrophotometric method , we developed "multicomponent ratio spectrum and derivative spectrophotometric method analysis software". On this basis , we applied this software to research the analysis method of inorganic binary mixtures-Ca2+, Mg2+,ternary mixtures-Ca2+, Mg2+, Sr2+and organic ternary mixtures-phenol, p-methylphenol , p-nitrophenol, and mainly obtained following several results:
1. According to ratio spectrum derivative method, we programmed the data processing software using Visual Basic. This software can be used to process both binary component and ternary component and it is easy to use. With the help of the software, we can avoid much computing work and can accelerate data processing. We made a setup program for the other users to use. We can got a satisfactory result with the software which has been validated by experiment.
2. We set up a new method using ratio spectrum and derivative simultaneous determineation Ca2+ and Mg2+ using ArsenazoIII as color reagent. We also got the optimum experimental conditions and made the determination easier than the traditional method. The precision for Ca2+ and Mg2+ is 0.76% and 0.63% respectively. The recovery rate is 97.8%-103% for calcium and 98.4%-102% for magnesium. The Beer's law is obeyed in the range of 0-60 g/25ml for calcium and 0-50 g/25ml for magnesium. The detection limitation for Ca2+and Mg2+ is 0.16 g/25ml and 0.13 g/25ml respectively, we applied this method for the analysis of natural water samples and got satisfactory
results.
3. The double divisor-ration spectra derivative method and the ratio spectra-zero crossing method are both used to analyze ternary mixtures. The result indicates that the double divisor-ration spectra derivative method is better than the ratio spectra-zero crossing method in the aspects of mathymatics theory and data results. So we chose the double divisor-ration spectra derivative method as our analysis method.
4. we studied simultaneous determination of Ca2+, Mg2+ and Sr2+ mixtures using spectrophotometric method for the first time and got satisfactory results. We determined the optimum experimental conditions followed here. The maximum wavelength is 625nm for Ca2+ , 619nm for Mg2+ and 646nm for Sr2+. The volume of color reagent is 5ml and reaction time is ISmins. The buffer solution volume is 3ml. The computation wavelength is 652nm for Ca2+, 638nm for Mg2+and 657nm for Sr2+. The precision for Ca2+,Mg2, Sr^is 0.72% , 0.68% and 2.10% respectively. The relative deviation is 0.3% -2.4% for Ca2+, 0.05%-2.3% for Mg2+ and 0.4%-3.4% for Sr2+. The Beer' s law is obeyed in the range of 0-60ug/25ml for Ca2+> 0-50ug/25ml for Mg2+and 0-60ug/25ml for Sr2+.The detection limitation for Ca2+ ,Mg2, Sr2+ is 0.16ug/25mK 0.16???g/25ml and 0.16 g/25ml respectively.
5. We applied double divisor-ration spectra derivative method to determine simultaneously ternary mixtures-phenol, p-methylphenol ,p-nitrophenol for the first time. The optimum experimental conditions and satisfactory results were obtained. The maximum wavelength is 211 nm for phenol, 220nm for p-methylphenol and 227nm for p-nitrophenol.. The Beer' s law is obeyed in the range of 0-33.6mg/L for phenol, 0-33.6mg/L for p-methylphenol and 0-38.4mg/L for p-nitrophenol. The detection limitation is 0.018mg/L, 0.022mg/L and 0.022mg/L. The precision for phenol, p-methylphenol ,p-nitrophenol is 0.79%> 0.89% and 0.93% respectively. The relative deviation is 0.4%-1.7%, 0.7%-3.7% and 0.1%-3.3% respectively.
6. We applied the proposed method to determine concentrations of calcium and magnesium of nature water samples collected from Yellow river at Lijin station, Shandong province. We also analyzed samples from 5 rivers and 4 bayous of Qingdao. The result was similar with that d
引文
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