某些硫（-Ⅱ）化合物及氧化中间物的氧化反应动力学与机理
摘要
运用高效液相色谱（HPLC）、毛细管电泳（CE）和紫外可见光分光光度法（UV-Vis）等多种分析方法，结合色质联用技术，对硫(-II)化合物（硫氰酸盐SCN-、硫脲Tu）及其氧化中间物的氧化反应动力学进行了系统研究，以揭示其详细反应机理，推进硫(-II)化合物氧化反应非线性机理和硫物种病理机制的研究进展。
建立了针对H2O2-SCN-氧化反应体系动力学测定的毛细管电泳间接紫外法和高效液相色谱测定方法。可在pH8.86-10.03范围内实现所有物种的基线分离，满足定性和定量分析要求。通过HPLC和CE可分别获得SCN-、H2O2和SCN-、SO42-、OCN-浓度-时间曲线。修正了Christy和Egeberg的研究关键结论：动力学分析证明弱碱性介质中，OxSCN-(x=1,2,3)为短寿命中间物，而不是CE可测定的稳定中间物；通过初始速率法计算获得反应对SCN-为一级，而不是零级。发现缓冲溶液性质影响总反应速率，按铵盐、磷酸盐、碳酸盐和硼酸盐的顺序，反应速率加快，总反应级数不受影响。由于形成过硼酸，硼酸盐对反应具有催化作用；碳酸根与H2O2形成活性过碳酸根而促进过氧化氢分解为氧气，碳酸盐则使化学反应计量比(H2O2/SCN-)明显增大。提出了基于不同缓冲溶液的动力学机理，较好的解释实验现象，并成功拟合动力学曲线（5个pH值、4种物种，共4800个数据点），误差均控制在5%以内。
二氧化硫脲（TuO2）和三氧化硫脲（TuO3）作为硫脲氧化过程中间物，其稳定性和反应性将对硫脲氧化过程产生影响。采用HPLC研究了pH4.0-11.0范围内TuO2和TuO3的水解反应动力学。高pH值（>8）大大降低了两者稳定性，水解均呈现一级动力学行为，其表观速率常数与pH值无线性依赖关系。HPLC-MS联用定性分析了TuO2和TuO3的含硫分解产物分别为次硫酸根（SO22-）和SO32-，剩余基团则分别形成尿素和氨基腈。在各物种定量的基础上确定了水解反应化学计量方程。
在TuO2稳定性研究基础上，使用UV-Vis监测360nm处ClO2的吸光度，探索了Tu氧化反应子体系ClO2-TuO2的反应动力学。pH1.5-3.0范围内存在ClO2自催化和TuO2的陈化效应。在陈化过程中，TuO2缓慢异构重排为高活性的甲脒亚磺酸，从而对ClO2自催化行为造成影响。实验证明了产物Cl-和中间物HOCl均能促进自催化现象的产生。基于实验提出可行性反应机理，很好的解释了自催化和陈化效应。ClO2-TuO2氧化反应涉及了TuO2的陈化异构、短寿命自催化物种及各价态含氯氧化剂之间的相互子反应。这种反应复杂性造成了速率方程无法进行简单表述，使得初始速率法计算得到ClO2、TuO2和OH-的级数均非整数。
利用液质联用，分离检测H2O2-Tu反应体系中各种含硫中间物。质谱测定表明氧化过程中相对分子质量92.10的未知中间物种为甲脒次磺酸。研究了H2O2-Tu氧化体系中pH值对甲脒次磺酸稳定性的影响及其动力学性质。甲脒次磺酸的存在证实了几十年来硫脲氧化机理中涉及的零价硫的存在，对硫脲氧化体系机理的研究有重大意义。在物种检测和实验现象基础上优化了动力学机理。以H2O2-Tu氧化研究为基础，初步探索了ClO2-氧化Tu反应动力学。pH值越小反应速率越大；硫脲的表观级数遵循零级反应，并计算获得了不同反应条件时的表观速率常数。同时采用UV-Vis检测到反应中间物ClO2的生成。在高酸度和过量ClO2-存在时，二氧化氯的生成具有时钟现象，且时钟现象的诱导期与硫脲的消耗时间相符合，诱导期随着Tu/ClO2-的初始浓度比增大而加长。
Combined with mass spectrometry (MS), high-performance liquidchromatography-mass spectrometry (HPLC), capillary electrophoresis (CE) andultraviolet spectrophotometer (UV-Vis) have been used to investigate the oxidation ofsulfur (-II)-containning compounds (thiocyanate SCN-and thiourea Tu) and the relatedoxides. It is to reveal the detail reaction mechanism and provide evidence for betterexplanation of non-linear phenomena and pathologic role of related reactions onthiocyanate and thiourea.
CE and HPLC optimized separation methods have been developed for thedetermination of the species in H2O2-SCN-reaction system. With the optimizedconditions the species in the reaction were all baseline-separated with outstandingqualitative and quantitative analyzed within the pH8.86–10.08. Concentration-timeseries of SCN-, SO42-and OCN-have been followed by CE as well as that of H2O2andSCN-by HPLC. The crucial conclusions obtained by Christy and Egeberg have beenmodified: It has been clearly demonstrated that OxSCN-(where x=1,2and3) are short-lived intermediates but undetectable with CE in weak alkaline solution; the rate law isfirst-order with respect to SCN-by initial rate method rather than zero order. In addition,it is also enlightened that the quality of the buffer strongly affect the rate of the overallreaction that increases in the order of application of ammonia, phosphate, carbonate andborate respectively, but no any effect on the reaction order. Borate reacts with hydrogenperoxide to produce peroxoborate and monoperoxoborate (or diperoxoborate) whichcould greatly accelerate the H2O2-SCN-reaction. A relatively huge shift could beobserved in the consumed H2O2/SCN-ratio in the presence of carbonate buffer due tothe higher decomposition rate of hydrogen peroxide to oxygen which cause by theformation of peroxymonocarbonate ion from the hydrogen peroxide-bicarbonatereaction. A kinetic mechanism based on different buffer solution was proposed to fitmore than4800data point of four species simultaneously at five different pH values.The average deviation was found to be less than5%.
TuO2and TuO3, as the intermediates during thiourea oxidation, have effect on theoxidation of thiourea. The hydrolysis was studied by the means of HPLC in pH4.0-11.0. The decomposition rates increased rapidly wirh the pH value. Both displays firstorder and the dependence of pseudo-first-order rate constants (kobs, s-1) on theconcentration of OH-is not a simple linear relationship. In alkaline solution, SO22-, ureaand SO32-, urea were obtained as final hydrolysis products of TuO2and TuO3, respectively. The stoichiometric of the reactions was determined by the quantitativeanalysis of HPLC-MS.
The oxidation of TuO2by ClO2, a subsystem of Tu oxidation, was investigatedbased on the hydrolysis of TuO2, where UV-Vis spectrophotometer was employed formonitoring the maximum absorption of ClO2at360nm. Autocatalytic fashion of ClO2and aging effect of TuO2have been found in ClO2-TuO2reaction under pH1.5-3.0. Itseems that TuO2slowly rearranges into formamidine sulfinic acid which is high activityin acid solution. Both Cl-and HOCl are able to promote the emergence of theautocatalysis. A feasibility reaction path is proposed to describe the autocatalysis andaging effect. The reaction orders for ClO2, TuO2and OH-calculated from the initial ratemethods are non-integer number and it is difficult to express the rate equation in asimply way and because of the complexity of ClO2-TuO2reaction.
Several sulfur-containing intermediates in the H2O2-Tu reaction were seperatedand detected by HPLC successfully. Besides TuO2and TuO3, MS measurementindicates an unreported intermediate to be TuO with mass weights of92.10. The effectof pH value on stablity and reactivity of TuO in the H2O2-Tu reaction has been studied.The detection of TuO has gave evidence of the existence of S(0), and is of greatsignificance for the study of the mechanism of thiourea oxidation system for decades.Mechanism was optimized based on species detection and kinetic study. Meanwhile,the reaction of thiourea by chlorite was also studied on the basis of the research of H2O2-Tu reaction. The result indicated that the oxidation rate increases with the decreasing ofpH value and the consumption of thiourea with zero order as chlorite in access. Theapparent rate constants were obtained. The chlorite-thiourea reaction had also beenstudied by UV-Vis spectrophotometry to observe the generation of chlorine dioxide atthe same time. When pH<7and oxidant is exceed, the clock phenomenon of chlorinedioxide has been observed. Induction period of clock reaction equals to the timeconsumption of thiourea, and induction time was increased as initial concentrationincreasing.
建立了针对H2O2-SCN-氧化反应体系动力学测定的毛细管电泳间接紫外法和高效液相色谱测定方法。可在pH8.86-10.03范围内实现所有物种的基线分离，满足定性和定量分析要求。通过HPLC和CE可分别获得SCN-、H2O2和SCN-、SO42-、OCN-浓度-时间曲线。修正了Christy和Egeberg的研究关键结论：动力学分析证明弱碱性介质中，OxSCN-(x=1,2,3)为短寿命中间物，而不是CE可测定的稳定中间物；通过初始速率法计算获得反应对SCN-为一级，而不是零级。发现缓冲溶液性质影响总反应速率，按铵盐、磷酸盐、碳酸盐和硼酸盐的顺序，反应速率加快，总反应级数不受影响。由于形成过硼酸，硼酸盐对反应具有催化作用；碳酸根与H2O2形成活性过碳酸根而促进过氧化氢分解为氧气，碳酸盐则使化学反应计量比(H2O2/SCN-)明显增大。提出了基于不同缓冲溶液的动力学机理，较好的解释实验现象，并成功拟合动力学曲线（5个pH值、4种物种，共4800个数据点），误差均控制在5%以内。
二氧化硫脲（TuO2）和三氧化硫脲（TuO3）作为硫脲氧化过程中间物，其稳定性和反应性将对硫脲氧化过程产生影响。采用HPLC研究了pH4.0-11.0范围内TuO2和TuO3的水解反应动力学。高pH值（>8）大大降低了两者稳定性，水解均呈现一级动力学行为，其表观速率常数与pH值无线性依赖关系。HPLC-MS联用定性分析了TuO2和TuO3的含硫分解产物分别为次硫酸根（SO22-）和SO32-，剩余基团则分别形成尿素和氨基腈。在各物种定量的基础上确定了水解反应化学计量方程。
在TuO2稳定性研究基础上，使用UV-Vis监测360nm处ClO2的吸光度，探索了Tu氧化反应子体系ClO2-TuO2的反应动力学。pH1.5-3.0范围内存在ClO2自催化和TuO2的陈化效应。在陈化过程中，TuO2缓慢异构重排为高活性的甲脒亚磺酸，从而对ClO2自催化行为造成影响。实验证明了产物Cl-和中间物HOCl均能促进自催化现象的产生。基于实验提出可行性反应机理，很好的解释了自催化和陈化效应。ClO2-TuO2氧化反应涉及了TuO2的陈化异构、短寿命自催化物种及各价态含氯氧化剂之间的相互子反应。这种反应复杂性造成了速率方程无法进行简单表述，使得初始速率法计算得到ClO2、TuO2和OH-的级数均非整数。
利用液质联用，分离检测H2O2-Tu反应体系中各种含硫中间物。质谱测定表明氧化过程中相对分子质量92.10的未知中间物种为甲脒次磺酸。研究了H2O2-Tu氧化体系中pH值对甲脒次磺酸稳定性的影响及其动力学性质。甲脒次磺酸的存在证实了几十年来硫脲氧化机理中涉及的零价硫的存在，对硫脲氧化体系机理的研究有重大意义。在物种检测和实验现象基础上优化了动力学机理。以H2O2-Tu氧化研究为基础，初步探索了ClO2-氧化Tu反应动力学。pH值越小反应速率越大；硫脲的表观级数遵循零级反应，并计算获得了不同反应条件时的表观速率常数。同时采用UV-Vis检测到反应中间物ClO2的生成。在高酸度和过量ClO2-存在时，二氧化氯的生成具有时钟现象，且时钟现象的诱导期与硫脲的消耗时间相符合，诱导期随着Tu/ClO2-的初始浓度比增大而加长。
Combined with mass spectrometry (MS), high-performance liquidchromatography-mass spectrometry (HPLC), capillary electrophoresis (CE) andultraviolet spectrophotometer (UV-Vis) have been used to investigate the oxidation ofsulfur (-II)-containning compounds (thiocyanate SCN-and thiourea Tu) and the relatedoxides. It is to reveal the detail reaction mechanism and provide evidence for betterexplanation of non-linear phenomena and pathologic role of related reactions onthiocyanate and thiourea.
CE and HPLC optimized separation methods have been developed for thedetermination of the species in H2O2-SCN-reaction system. With the optimizedconditions the species in the reaction were all baseline-separated with outstandingqualitative and quantitative analyzed within the pH8.86–10.08. Concentration-timeseries of SCN-, SO42-and OCN-have been followed by CE as well as that of H2O2andSCN-by HPLC. The crucial conclusions obtained by Christy and Egeberg have beenmodified: It has been clearly demonstrated that OxSCN-(where x=1,2and3) are short-lived intermediates but undetectable with CE in weak alkaline solution; the rate law isfirst-order with respect to SCN-by initial rate method rather than zero order. In addition,it is also enlightened that the quality of the buffer strongly affect the rate of the overallreaction that increases in the order of application of ammonia, phosphate, carbonate andborate respectively, but no any effect on the reaction order. Borate reacts with hydrogenperoxide to produce peroxoborate and monoperoxoborate (or diperoxoborate) whichcould greatly accelerate the H2O2-SCN-reaction. A relatively huge shift could beobserved in the consumed H2O2/SCN-ratio in the presence of carbonate buffer due tothe higher decomposition rate of hydrogen peroxide to oxygen which cause by theformation of peroxymonocarbonate ion from the hydrogen peroxide-bicarbonatereaction. A kinetic mechanism based on different buffer solution was proposed to fitmore than4800data point of four species simultaneously at five different pH values.The average deviation was found to be less than5%.
TuO2and TuO3, as the intermediates during thiourea oxidation, have effect on theoxidation of thiourea. The hydrolysis was studied by the means of HPLC in pH4.0-11.0. The decomposition rates increased rapidly wirh the pH value. Both displays firstorder and the dependence of pseudo-first-order rate constants (kobs, s-1) on theconcentration of OH-is not a simple linear relationship. In alkaline solution, SO22-, ureaand SO32-, urea were obtained as final hydrolysis products of TuO2and TuO3, respectively. The stoichiometric of the reactions was determined by the quantitativeanalysis of HPLC-MS.
The oxidation of TuO2by ClO2, a subsystem of Tu oxidation, was investigatedbased on the hydrolysis of TuO2, where UV-Vis spectrophotometer was employed formonitoring the maximum absorption of ClO2at360nm. Autocatalytic fashion of ClO2and aging effect of TuO2have been found in ClO2-TuO2reaction under pH1.5-3.0. Itseems that TuO2slowly rearranges into formamidine sulfinic acid which is high activityin acid solution. Both Cl-and HOCl are able to promote the emergence of theautocatalysis. A feasibility reaction path is proposed to describe the autocatalysis andaging effect. The reaction orders for ClO2, TuO2and OH-calculated from the initial ratemethods are non-integer number and it is difficult to express the rate equation in asimply way and because of the complexity of ClO2-TuO2reaction.
Several sulfur-containing intermediates in the H2O2-Tu reaction were seperatedand detected by HPLC successfully. Besides TuO2and TuO3, MS measurementindicates an unreported intermediate to be TuO with mass weights of92.10. The effectof pH value on stablity and reactivity of TuO in the H2O2-Tu reaction has been studied.The detection of TuO has gave evidence of the existence of S(0), and is of greatsignificance for the study of the mechanism of thiourea oxidation system for decades.Mechanism was optimized based on species detection and kinetic study. Meanwhile,the reaction of thiourea by chlorite was also studied on the basis of the research of H2O2-Tu reaction. The result indicated that the oxidation rate increases with the decreasing ofpH value and the consumption of thiourea with zero order as chlorite in access. Theapparent rate constants were obtained. The chlorite-thiourea reaction had also beenstudied by UV-Vis spectrophotometry to observe the generation of chlorine dioxide atthe same time. When pH<7and oxidant is exceed, the clock phenomenon of chlorinedioxide has been observed. Induction period of clock reaction equals to the timeconsumption of thiourea, and induction time was increased as initial concentrationincreasing.
引文
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