CN1789219A - Method for initiating, capturing and measuring hydroxy radical under high temperature - Google Patents
Method for initiating, capturing and measuring hydroxy radical under high temperature Download PDFInfo
- Publication number
- CN1789219A CN1789219A CN 200510102197 CN200510102197A CN1789219A CN 1789219 A CN1789219 A CN 1789219A CN 200510102197 CN200510102197 CN 200510102197 CN 200510102197 A CN200510102197 A CN 200510102197A CN 1789219 A CN1789219 A CN 1789219A
- Authority
- CN
- China
- Prior art keywords
- solution
- hydrogen peroxide
- hydroxy radical
- sodium hydroxide
- radical qiao
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for initiating under high temperature, catching and detecting hydroxy free radical, mixing the hydrogen dioxide solution and sodium-hydroxide solution, then adding the mixture into dimethyl sulfoxide solution with the temperature being 70-130 Deg C; or mixing the hydrogen dioxide solution, sodium-hydroxide solution and dimethyl sulfoxide solution, heating the mixing solution to make the temperature be 70-130 Deg C. The adding amount of hydrogen dioxide, sodium-hydroxide and dimethyl sulfoxide is that the mole ratio between hydrogen dioxide and sodium-hydroxide is 140:1-1:1, the mole ratio between dimethyl sulfoxide and hydrogen dioxide is 20:1-0.5:1. The temperature and alkali condition for initiating and catching hydroxy free radical is similar to that of bleaching hydrogen dioxide under high temperature and paper pulp elignifying, which is suited to be applied in the field of chemical pulping. The invention is characterized by simple device for initiating and catching and easy and fast operation.
Description
Technical field
The present invention relates to the method that a kind of initiation hydroxy radical qiao (HO) produces, and simultaneously it is captured and further measure.Specifically be meant and utilize higher temperature and suitable alkaline condition to cause hydrogen peroxide decomposition, produce hydroxy radical qiao, under comparatively high temps, react as trapping agent and hydroxy radical qiao simultaneously with dimethyl sulfoxide (DMSO), the product methyl-sulfinic acid that generates generates colored diazonium sulfone derivatives by reacting with diazonium salt, thereby uses spectrophotometry diazonium sulfone derivatives indirect measurement hydroxy radical qiao again.
Background technology
Hydroxy radical qiao (OH) is extremely short and a material that moment exists of life-span, and hydroxy radical qiao produces morely in human body or animal body under certain conditions, causes disease to take place, phenomenons such as aging acceleration.In order to seek, develop, produce and develop the food and the medicine that can suppress or eliminate hydroxy radical qiao, often need artificially to cause hydroxy radical qiao and produce, then verification the verifying results.The method that the initiation hydroxy radical qiao of biological and medical field report produces mainly contains: (1) Fenton reaction method:
(2) the gamma-rays method of radiating of water:
(3) hydrogen peroxide UV-light decomposition method:
。These methods that cause the hydroxy radical qiao generation are adapted at using under the lower temperature (as room temperature), for example the activation energy of Fenton reaction is lower, the existence of ferrous ion finishes hydrogen peroxide with regard to decomposing in the short period of time at room temperature, do not need high temperature also to be not suitable for being applied to hot conditions so cause hydroxy radical qiao.Because initiation under the lesser temps and trap conditions and biological intravital temperature condition are close, so aforesaid method is applicable to biological and medical field.
Yet in some pyritous environment, also can produce hydroxy radical qiao, for example in the high temperature hydrogen peroxide bleaching and oxygen delignification process of paper pulp, the generation meeting of hydroxy radical qiao causes material impact to bleaching and delignification result, in order to obtain rationally to control and utilize the processing condition of hydroxy radical qiao to make it to help bleaching results, be necessary to obtain at high temperature to cause and capture the method for hydroxy radical qiao.But at high temperature artificially cause hydroxy radical qiao at present and it is captured method for measuring and yet there are no report.
For the hydroxy radical qiao that causes generation being separated and detecting, need in initiation reaction, catch the hydroxy radical qiao of generation with trapping agent, make it to generate more stable reaction product, then product is measured.Though to the existing several different methods of the capture of hydroxy radical qiao, as utilize dimethyl sulfoxide (DMSO), Whitfield's ointment, Virahol, phenylalanine, aldehydes matter etc. as trapping agent, these methods are all non-to capture under hot conditions.In known multiple trapping agent, the effect of dimethyl sulfoxide (DMSO) is better, people such as U.S. Steiner and Babbs use the trapping agent of dimethyl sulfoxide (DMSO) (DMSO) as hydroxy radical qiao at normal temperatures, (CharlesF.Babbs et al, Analytical Biochemistry, 1987,163:67～73; Melissa G.Steiner et al, Archives ofBiochemistry and Biophysics, 1990,278 (2): 478～481), the result shows that dimethyl sulfoxide (DMSO) can sensitive be effectively applied to the qualitative and detection by quantitative of hydroxy radical qiao.The reaction principle that dimethyl sulfoxide (DMSO) captures hydroxy radical qiao is as follows:
1. the hydroxy radical qiao that produces in the dimethyl sulfoxide (DMSO) seizure system generates the methyl-sulfinic acid:
(dimethyl sulfoxide (DMSO), DMSO) (methyl-sulfinic acid)
2. with aromatic series diazonium salt and the reaction of methyl-sulfinic acid, generate colored diazonium sulfone derivatives:
(diazonium salt) (diazonium sulfone derivatives)
Ar---represent aryl or substituted aryl
Product diazonium sulfone derivatives in the reaction formula (2) can utilize spectrophotometry.Babbs etc. filter out the best fast blue BB salt of effect (Fast Blue BB Salt) and are used for spectrophotometric analysis according to the comparative experiments to more than 20 kinds of diazonium salts, and its characteristic absorbance relevant with hydroxy radical qiao is near 420nm.With theoretical yield relatively, hydroxy radical qiao by dimethyl sulfoxide (DMSO) capture be converted into the methyl-sulfinic acid and then generate the diazonium sulfone derivatives with the fast blue BB salt reaction after, be 80.0%～90.8% with the detected efficient of spectrophotometry.In above-mentioned reaction, between the reactant and the mol ratio between reactant and the product be 1: 1 relation, therefore can judge the generation of hydroxy radical qiao according to the characteristic absorbance of diazonium sulfone derivatives, and can measure the concentration of diazonium sulfone derivatives, thereby calculate the concentration of the hydroxy radical qiao that produces according to its absorption intensity.
Summary of the invention
The objective of the invention is to overcome prior art deficiency at high temperature, provide a kind of suitable higher temperature conditions and alkaline condition of utilizing to cause the method that hydrogen peroxide decomposition produces hydroxy radical qiao, and under comparatively high temps, utilize dimethyl sulfoxide (DMSO) to capture hydroxy radical qiao step of going forward side by side and carry out method for measuring.
Purpose of the present invention is achieved through the following technical solutions:
A kind of high temperature causes and captures the method for hydroxy radical qiao, it is characterized in that, after aqueous hydrogen peroxide solution and aqueous sodium hydroxide solution are mixed, joins temperature and is in 70 ℃～130 ℃ the dimethyl sulphoxide solution; Or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide solution mixed, and mixing solutions is warming up to 70 ℃～130 ℃; The add-on of described hydrogen peroxide, sodium hydroxide and dimethyl sulfoxide (DMSO) is that the mol ratio of hydrogen peroxide and sodium hydroxide is 140: 1～1: 1, and the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 20: 1～0.5: 1.
For further realizing the object of the invention, the add-on of hydrogen peroxide and sodium hydroxide is preferred 70: 1～1.5: 1 of the mol ratio of hydrogen peroxide and sodium hydroxide.The add-on of dimethyl sulfoxide (DMSO) is preferred 10: 1～2: 1 of the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide.Preferred 80 ℃～120 ℃ of the mixeding liquid temperature of dimethyl sulphoxide aqueous solution or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide aqueous solution.
The mixed solution of hydrogen peroxide and sodium hydroxide added in 70 ℃～130 ℃ the dimethyl sulphoxide solution, keep within the insulation 15 minutes; Or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide solution mixed, and mixing solutions is warming up to 70 ℃～130 ℃, keep within the insulation 15 minutes.
The hydroxy radical qiao method for measuring that high temperature causes and captures comprises the steps and processing condition:
(1) aqueous hydrogen peroxide solution and aqueous sodium hydroxide solution are mixed, the add-on of hydrogen peroxide and sodium hydroxide is that the mol ratio of hydrogen peroxide and sodium hydroxide is 140: 1～1: 1, measures 2mL～40mL mixing solutions;
(2) compound concentration is the dimethyl sulphoxide aqueous solution of 2mol/L～12.8mol/L;
(3) cause and capture reaction: by capturing the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide in the reaction system is 0.5: 1～20: 1 amount, it is the reaction vessel of nonmetal high temperature material that the dimethyl sulphoxide aqueous solution of measuring step (2) configuration places inwall, preferred glass or tetrafluoroethylene, solution in the reaction vessel is warming up to 70 ℃～130 ℃, the solution of step (1) the preparation speed with 2mL/min～8mL/min is splashed in the reactor; The dropping process constantly stirs or sways reactor, is added dropwise to complete the back and keeps temperature to continue reaction 0～15 minute; Perhaps with the dimethyl sulphoxide solution of measuring step (2) configuration with after solution that step (1) disposes mixes, insert in the reaction vessel that inwall is nonmetal high temperature material, reaction vessel is rapidly heated to 70 ℃～130 ℃;
(4) solution in the reaction vessel of step (3) is cooled to room temperature rapidly, with the pH value to 4 of hydrochloric acid conditioning solution; With the deionized water dilution, the concentration that makes methyl-sulfinic acid in the diluent is at 0.5 μ mol/L～60 μ mol/L;
(5) take out the diluent of 1mL step (4) gained in centrifuge tube or test tube, add the phosphate buffer soln of 1mL pH=4 and the fast blue BB salt solution that 2mL concentration is no more than 25mmol/L, at room temperature place dark place reaction 10 minutes after mixing, add the 4mL ethyl acetate again; Fully sway extraction at least 5 minutes, centrifugal then or standing demix is got the upper strata and is contained diazonium sulfone derivatives organic phase as sample to be analyzed;
(6) with the diazonium sulfone derivatives in the organic phase sample of ultraviolet-visible spectrophotometer determination step (5) gained (quantitative analysis needs at 3 hours with interior mensuration), characterize the capture of hydroxy radical qiao by the charateristic avsorption band of 410～420nm, calculate the concentration of hydroxy radical qiao according to the typical curve of 410～420nm absorption value being done by methyl-sulfinic acid concentration.
Begin to be reacted to the operation of step (6) from step (3) capture reaction product methyl-sulfinic acid and fast blue BB salt, calculate to be controlled in 3 hours for hydroxy radical qiao concentration and finish with spectrophotometric determination.
The principle that the present invention causes the hydroxy radical qiao generation is:
Hydrogen peroxide decomposition under suitable alkaline condition produces hydrogen and crosses oxygen anion (HOO
-):
Improving temperature makes hydrogen cross oxygen anion further to decompose, cause producing hydroxy radical qiao:
Hydrogen peroxide generation homolytic reaction under the high temperature, cause producing hydroxy radical qiao:
Since dimethyl sulfoxide (DMSO) have boiling point height, high temperatures, can with characteristics such as water is miscible, the present invention when high temperature causes hydroxy radical qiao, with dimethyl sulfoxide (DMSO) as the hydroxy radical qiao trapping agent under the hot conditions.Trap conditions of the present invention is compared with people's such as Steiner and Babbs trap conditions, the hot conditions (70 ℃～130 ℃) that adopts is all different with it with alkaline condition, having overcome prior art is the deficiency of using under normal temperature and non-alkaline condition, and a kind of capture method that can produce high temperature hydrogen peroxide bleaching and pulp oxygen delignification technology in the reality in conjunction with pulping and paper-making is provided thus.
Compare with the technology of existing initiation hydroxy radical qiao, the invention provides the method that at high temperature causes and capture hydroxy radical qiao, need not add transition metal ion in the initiation reaction system and cause hydroxy radical qiao (the Fenton reaction as classics causes), do not need by the equipment (as people's such as Steiner and Babbs initiation) that produces gamma-rays radiation or UV-light yet, this initiation is close with the pulp oxygen delignification processing condition with the high temperature hydrogen peroxide bleaching in alkaline environment and the actual production with the temperature condition that captures hydroxy radical qiao, therefore is well suited for being applied to the field of pulping chemistry.The present invention simultaneously has the simple and processing ease of the catching apparatus of initiation, characteristics fast.In this external mensuration process, the present invention adopts ethyl acetate extraction diazonium sulfone derivatives, and does not adopt the organic solvent extraction of containing benezene compound, thereby helps alleviating in the measurement operation objectionable impurities to operator's influence.
Description of drawings
Fig. 1 is the measurement result that causes hydroxy radical qiao among the embodiment 1 under 60 ℃ to 70 ℃ conditions.
Fig. 2 is the measurement result that causes hydroxy radical qiao among the embodiment 1 under 70 ℃ to 100 ℃ conditions.
Fig. 3 is the measurement result that causes hydroxy radical qiao among the embodiment 2 under 100 ℃ to 140 ℃ conditions
Fig. 4 causes the result of hydroxy radical qiao after different soaking times under 120 ℃ of conditions among the embodiment 5
Fig. 5 is the measurement result that causes hydroxy radical qiao among the embodiment 6 under 120 ℃ of conditions during different hydrogen peroxide add-on
Fig. 6 is the typical curve that is used for the methyl-sulfinic acid concentration and the 415nm place absorption value relation of hydroxy radical qiao quantitative assay among the embodiment 7
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but the scope of protection of present invention is not limited to the scope that embodiment is represented.
The initiation and the mensuration of hydroxy radical qiao below embodiment 1:100 ℃
(1) measuring sodium hydroxide solution that superoxol that 20mL concentration is 7moL/L and 1mL concentration is 1mol/L puts in the beaker and mixes; (mol ratio of hydrogen peroxide and sodium hydroxide is in the mixing solutions: 140: 1)
(2) measuring 20mL concentration is that the dimethyl sulphoxide aqueous solution of 3.5mol/L is inserted in the 250mL reaction flask, reaction flask is placed the thermostat water bath (same operation is carried out at the thermostat water bath of 60 ℃, 65 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃ respectively) of modulated good temperature, pre-heating temperature elevation 3～5min, then with the mixed solution that drips hydrogen peroxide and sodium hydroxide in the dimethyl sulphoxide aqueous solution of speed in reaction flask of 5mL/min, the dropping process is constantly swayed reaction flask, drip the back and continue reaction 10min, take out reaction flask then and cool off with cold water rapidly; (mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 0.5: 1)
(3) regulate in the bottle solution to pH=4 with dilute hydrochloric acid, be settled to 100mL with the deionized water dilution, take out 1mL solution with transfer pipet and place that 10mL's have a scale tool plug centrifuge tube, the concentration that adds the new preparation of 1mL phosphate buffered saline buffer (pH=4) and 2mL is the fast blue BB salt solution of 25mmol/L, at room temperature put dark place reaction 10min, add the 4mL ethyl acetate then, fully sway extraction 5min, centrifugal layering, get upper organic phase as analytical sample after separating fully, with ethyl acetate as reference, with the absorption curve of spectrophotometric determination sample, the characteristic absorbance that to be the dimethyl sulfoxide (DMSO) product methyl-sulfinic acid of catching hydroxy radical qiao produced with the diazonium sulfone derivatives of fast blue BB salt generation of the absorption peak at the 415nm place.
Fig. 1 and Fig. 2 are the measurement result that causes hydroxy radical qiao under 60 ℃ to the 100 ℃ conditions, show that the temperature condition that causes hydroxy radical qiao need be more than 65 ℃, and near 70 ℃, the concentration of the hydroxy radical qiao that produces increases along with the rising of temperature.A represents the numerical value (with A in figure below together) of ultraviolet-visible spectrophotometer mensuration gained absorption value among the figure.
The initiation and the mensuration of hydroxy radical qiao under the hot conditions more than embodiment 2:100 ℃
(1) measuring sodium hydroxide solution that superoxol that 3mL concentration is 7moL/L and 1mL concentration is 1mol/L puts in the beaker and mixes; (mol ratio of hydrogen peroxide and sodium hydroxide is in the mixing solutions: 21: 1)
(2) measuring 20mL concentration is that the dimethyl sulphoxide aqueous solution of 3.5mol/L is inserted in the 250mL reaction flask.Earlier reaction flask is placed the oil bath (same operation is carried out in the oil bath of 110 ℃, 120 ℃, 130 ℃ and 140 ℃ respectively) of modulated good temperature, pre-heating temperature elevation 1～2min, then with the mixed solution that drips hydrogen peroxide and sodium hydroxide in the dimethyl sulphoxide solution of speed in reaction flask of 2mL/min, the dropping process is constantly swayed reaction flask, drips the back and continues reaction 5min.Taking out reaction flask then cools off with cold water rapidly; (mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 3.3: 1)
After adding the 4mL ethyl acetate in the subsequent step, fully sway extraction 10min, adopt centrifugal layering, other is identical with step (3) among the embodiment 1.
Fig. 3 causes the measurement result that hydroxy radical qiao produces under 110 ℃～140 ℃ conditions, show that the concentration that produces hydroxy radical qiao in 110 ℃～130 ℃ scopes rises along with the increase of initiation reaction temperature, no longer changes but continue elevated temperature hydroxy radical qiao concentration after 130 ℃ again.
Change the initiation and the mensuration of reagent mol ratio below embodiment 3:100 ℃
(1) measuring sodium hydroxide solution that superoxol that 10mL concentration is 7moL/L and 1mL concentration is 1mol/L puts in the beaker and mixes; (mol ratio of hydrogen peroxide and sodium hydroxide is in the mixing solutions: 70: 1)
(2) measuring 80mL concentration is that the dimethyl sulphoxide aqueous solution of 7mol/L is inserted in the 250mL reaction flask, it is 90 ℃ thermostat water bath that reaction flask is placed modulated good temperature, pre-heating temperature elevation 5min, then with the mixed solution that drips hydrogen peroxide and sodium hydroxide in the dimethyl sulphoxide aqueous solution of speed in reaction flask of 5mL/min, the dropping process is constantly swayed reaction flask, drip the back and continue reaction 10min, take out reaction flask then and cool off with cold water rapidly; Step (3) is identical among (dimethyl sulfoxide (DMSO) is 8: 1 with the mol ratio of hydrogen peroxide) subsequent step and the embodiment 1.
Change the initiation and the mensuration of reagent mol ratio more than embodiment 4:100 ℃
(1) measuring sodium hydroxide solution that superoxol that 2mL concentration is 3moL/L and 2mL concentration is 3mol/L puts in the beaker and mixes; (mol ratio of hydrogen peroxide and sodium hydroxide is in the mixing solutions: 1: 1)
(2) measuring 20mL concentration is that the dimethyl sulphoxide aqueous solution of 6mol/L is inserted in the 250mL reaction flask, it is 120 ℃ oil bath that reaction flask is placed modulated good temperature, pre-heating temperature elevation 1min, then with the mixed solution that drips hydrogen peroxide and sodium hydroxide in the dimethyl sulphoxide aqueous solution of speed in reaction flask of 2mL/min, the dropping process is constantly swayed reaction flask, drip the back and continue reaction 5min, take out reaction flask then and cool off with cold water rapidly; (mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 20: 1)
After adding the 4mL ethyl acetate in the subsequent step, fully sway extraction 20min, adopt standing demix, other is identical with step (3) among the embodiment 1.
Embodiment 5: high temperature causes the result behind the insulation different time down
The temperature of reaction of oil bath is 120 ℃, and the time that drips the reaction of follow-up continuation of insurance temperature is got 0min, 5min, 10min and 15min respectively as a comparison, and all the other operations and condition are with identical described in the embodiment 2.Fig. 4 is the measurement result to the income analysis sample, and the absorption curve of visible initiation reaction insulation 10min and 15min almost overlaps among the figure, shows that the time of continuing reaction under 120 ℃ of high temperature needs not exceed 10min.
Embodiment 6: the hydrogen peroxide add-on is to causing the influence that hydroxy radical qiao produces
The temperature of reaction of oil bath is 120 ℃, and the volume of measuring the 7moL/L superoxol is respectively 1mL, 2mL, 3mL and 4mL, and all the other operations and condition are with identical described in the above-mentioned example 2.Fig. 5 is the measurement result to the income analysis sample, shows among the figure under same temperature and reaction conditions, and along with the increase of hydrogen peroxide add-on, the corresponding increase of the hydroxy free radical concentration of generation.
Embodiment 7: the quantitative assay of hydroxy radical qiao
Earlier (be equal to reaction formula (1) in the scape technology of passing away with the product of hydroxy radical qiao after by the dimethyl sulfoxide (DMSO) capture with pure methyl-sulfinic acid reagent.) as reference material, itself and fast blue BB salt reaction back are measured the relation (A=0.0142C+0.0466 of methyl-sulfinic acid concentration (C) and 415nm place absorption value (A) among acquisition Fig. 6 to product; R
2=0.9901), can carry out quantitative analysis to the hydroxy radical qiao concentration that initiation reaction produces on this basis.
Claims (8)
1. a high temperature causes and captures the method for hydroxy radical qiao, it is characterized in that, after aqueous hydrogen peroxide solution and aqueous sodium hydroxide solution are mixed, joins temperature and is in 70 ℃～130 ℃ the dimethyl sulphoxide solution; Or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide solution mixed, and mixing solutions is warming up to 70 ℃～130 ℃; The add-on of described hydrogen peroxide, sodium hydroxide and dimethyl sulfoxide (DMSO) is that the mol ratio of hydrogen peroxide and sodium hydroxide is 140: 1～1: 1, and the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 20: 1～0.5: 1.
2. high temperature according to claim 1 causes and captures the method for hydroxy radical qiao, it is characterized in that the add-on of hydrogen peroxide and sodium hydroxide is that the mol ratio of hydrogen peroxide and sodium hydroxide is 70: 1～1.5: 1.
3. high temperature according to claim 1 causes and captures the method for hydroxy radical qiao, it is characterized in that the add-on of dimethyl sulfoxide (DMSO) is that the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide is 10: 1～2: 1.
4. high temperature according to claim 1 causes and captures the method for hydroxy radical qiao, it is characterized in that the mixeding liquid temperature of dimethyl sulphoxide aqueous solution or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide aqueous solution is 80～120 ℃.
5. high temperature according to claim 1 causes down the method that captures hydroxy radical qiao, it is characterized in that, the mixed solution of hydrogen peroxide and sodium hydroxide is added in 70 ℃～130 ℃ the dimethyl sulphoxide solution, within keeping being incubated 15 minutes; Or aqueous hydrogen peroxide solution, aqueous sodium hydroxide solution and dimethyl sulphoxide solution mixed, and mixing solutions is warming up to 70 ℃～130 ℃, keep within the insulation 15 minutes.
6. hydroxy radical qiao method for measuring to any described high temperature initiation of claim 1～5 and capture is characterized in that this measuring method comprises the steps and processing condition:
(1) aqueous hydrogen peroxide solution and aqueous sodium hydroxide solution are mixed, the add-on of hydrogen peroxide and sodium hydroxide is that the mol ratio of hydrogen peroxide and sodium hydroxide is 140: 1～1: 1, measures 2mL～40mL mixing solutions;
(2) compound concentration is the dimethyl sulphoxide aqueous solution of 2mol/L～12.8mol/L;
(3) cause and capture reaction: by capturing the mol ratio of dimethyl sulfoxide (DMSO) and hydrogen peroxide in the reaction system is 0.5: 1～20: 1 amount, it is the reaction vessel of nonmetal high temperature material that the dimethyl sulphoxide aqueous solution of measuring step (2) configuration places inwall, solution in the reaction vessel is warming up to 70 ℃～130 ℃, the solution of step (1) the preparation speed with 2mL/min～8mL/min is splashed in the reactor; The dropping process constantly stirs or sways reactor, is added dropwise to complete the back and keeps temperature to continue reaction 0～15 minute; Perhaps with the dimethyl sulphoxide solution of measuring step (2) configuration with after solution that step (1) disposes mixes, insert in the reaction vessel that inwall is nonmetal high temperature material, reaction vessel is rapidly heated to 70 ℃～130 ℃;
(4) solution in the reaction vessel of step (3) is cooled to room temperature rapidly, with the pH value to 4 of hydrochloric acid conditioning solution; With the deionized water dilution, the concentration that makes methyl-sulfinic acid in the diluent is at 0.5 μ mol/L～60 μ mol/L;
(5) take out the diluent of 1mL step (4) gained in centrifuge tube or test tube, add the phosphate buffer soln of 1mL pH=4 and the fast blue BB salt solution that 2mL concentration is no more than 25mmol/L, at room temperature place dark place reaction 10 minutes after mixing, add the 4mL ethyl acetate again; Fully sway extraction at least 5 minutes, centrifugal then or standing demix is got the upper strata and is contained diazonium sulfone derivatives organic phase as sample to be analyzed;
(6) with the diazonium sulfone derivatives in the organic phase sample of ultraviolet-visible spectrophotometer determination step (5) gained (quantitative analysis needs at 3 hours with interior mensuration), characterize the capture of hydroxy radical qiao by the charateristic avsorption band of 410～420nm, calculate the concentration of hydroxy radical qiao according to the typical curve of 410～420nm absorption value being done by methyl-sulfinic acid concentration.
7. capture and method for measuring according to the described hydroxy radical qiao of claim 6, it is characterized in that the reaction vessel inwall in the described step (3) is glass or tetrafluoroethylene.
8. capture and method for measuring according to the described hydroxy radical qiao of claim 6, it is characterized in that, begin to be reacted to the operation of step (6) from step (3) capture reaction product methyl-sulfinic acid and fast blue BB salt, calculate to be controlled in 3 hours for hydroxy radical qiao concentration and finish with spectrophotometric determination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510102197 CN1789219A (en) | 2005-12-09 | 2005-12-09 | Method for initiating, capturing and measuring hydroxy radical under high temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510102197 CN1789219A (en) | 2005-12-09 | 2005-12-09 | Method for initiating, capturing and measuring hydroxy radical under high temperature |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1789219A true CN1789219A (en) | 2006-06-21 |
Family
ID=36787370
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510102197 Pending CN1789219A (en) | 2005-12-09 | 2005-12-09 | Method for initiating, capturing and measuring hydroxy radical under high temperature |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1789219A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413896B (en) * | 2008-12-02 | 2011-05-18 | 上海理工大学 | Method for measuring hydroxy free radical |
| CN103983592A (en) * | 2014-06-06 | 2014-08-13 | 哈尔滨工业大学 | Method for detecting concentration of hydroxyl radicals in solution |
-
2005
- 2005-12-09 CN CN 200510102197 patent/CN1789219A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413896B (en) * | 2008-12-02 | 2011-05-18 | 上海理工大学 | Method for measuring hydroxy free radical |
| CN103983592A (en) * | 2014-06-06 | 2014-08-13 | 哈尔滨工业大学 | Method for detecting concentration of hydroxyl radicals in solution |
| CN103983592B (en) * | 2014-06-06 | 2016-05-11 | 哈尔滨工业大学 | A kind of method that detects hydroxy free radical concentration in solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108384539B (en) | Green fluorescent carbon quantum dot, and preparation method and application thereof | |
| CN107056704B (en) | Lysosome-targeted hypochlorite ion fluorescent probe and application thereof | |
| CN1869666A (en) | Method for investigating carbonate in gypsum and its device | |
| CN1991339A (en) | Method for analyzing total phosphorus content in sample | |
| CN105462590B (en) | A kind of boration quantum dot ratio fluorescent probe and its preparation method and application | |
| CN111504961A (en) | Fluorescent sensor based on glutathione gold nanoclusters and application thereof | |
| CN102701265A (en) | Water-phase preparation method of near-infrared luminescent silver sulfide quantum dot | |
| CN110940648B (en) | Synthesis method of green fluorescent carbon quantum dots and application of green fluorescent carbon quantum dots in detection of nitrite | |
| CN1789219A (en) | Method for initiating, capturing and measuring hydroxy radical under high temperature | |
| CN105319088A (en) | Pre-treatment method of detection of liquid sample with laser-induced breakdown spectroscopy | |
| CN107084937A (en) | The assay method of lead content in dimethyl silicone polymer and its emulsion | |
| Truog | Methods for the Determination of Carbon Dioxide and a New Form of Absorption Tower Adapted to the Titrimetric Method. | |
| CN112362653B (en) | Method for detecting low chlorine content of photoinitiator | |
| CN105646349B (en) | A kind of organophosphorus pesticide molecular probe, preparation method, application process and inorganic/organic composite rare earth upconversion nano material | |
| CN1085662A (en) | Fluid analysis | |
| CN109796443A (en) | A kind of invertibity Ratiometric fluorescent probe detecting sulfur dioxide | |
| CN103323445A (en) | Method for quantitatively detecting aluminum content in food by utilizing laser Raman spectroscope | |
| CN108426867A (en) | Detection of Fe in Water3+MOF-Cd probe with antibiotic ceftriaxone sodium and preparation method and application thereof | |
| CN113009007B (en) | Method for detecting content of root-resisting agent in root-puncture-resistant material | |
| CN103497189A (en) | 1-OH-3,4:9,10-tetracarboxylic diimide and synthesis method as well as application thereof in measurement of fluorine content | |
| CN102863379A (en) | Analytical reagent for measuring heavy metal and method for preparing same | |
| CN109734824A (en) | A kind of N- succinyl group chitosan C-6 selective oxidation derivative and its preparation method and application | |
| Waddell et al. | Characterization and properties of dibenzo-18-crown-6 covalently bonded to silica gel | |
| CN113340862A (en) | Fluorescent molecular sensor, preparation method thereof and detection method of trace uranyl ions in water | |
| CN1807422A (en) | Reaction product of resorcin and methyl ethyl ketone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |