CN105548386A - Rapid quantitative analysis method for antioxidant in rubber - Google Patents
Rapid quantitative analysis method for antioxidant in rubber Download PDFInfo
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- CN105548386A CN105548386A CN201510908716.6A CN201510908716A CN105548386A CN 105548386 A CN105548386 A CN 105548386A CN 201510908716 A CN201510908716 A CN 201510908716A CN 105548386 A CN105548386 A CN 105548386A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention aims at to provide a method for rapid quantification of the content of an organic antioxidant in vulcanized and mixed rubber, which belongs to the fields of rubber and analysis of rubber formulas, wherein the vulcanized and mixed rubber comprises, but not limited to, natural or synthetic raw material rubber and compounds thereof, a variety of aid products with rubber as a carrier, a vulcanized and mixed rubber complex and the like. According to a technical scheme in the invention, the method comprises the following concrete steps: preparing particles with a size of less than 2 mm<3> from a rubber compound; subjecting the particles to ultrasonic extraction with a solvent; accurately adding an internal-standard substance into extract; subjecting the extract to separation and testing by using capillary column gas chromatography; and quantitatively determining the content of the antioxidant in the vulcanized and mixed rubber through comparison with a standard antioxidant solution. The method is simple in treatment steps and fast in an analysis speed, uses consistent chromatographic conditions and can quantify a plurality of antioxidants in the rubber compound at the same time.
Description
Technical field
The invention belongs to rubber and rubber compounding analysis field, be specifically related to the quick quantitative analytic method of various organic aging resister in all kinds sulfuration and mixing of rubber.Described sulfuration and mixing of rubber include but not limited to natural or synthesis crude rubber (including but not limited to NR, BR, SBR, IIR, CIIR, BIIR, EPDM, CR, silica gel etc.) and their compound; Take rubber as the various Additives Products of carrier; Sulfuration and mixing rubber composition etc.
Background technology
Along with the development of rubber industry, the research of rubber and rubber compounding is more and more subject to people's attention.Aging resister content in accurate quantitative analysis sizing material, has important meaning to rubber and rubber compounding analysis.
At present, in rubber size, especially constituent analysis adopts soxhlet extraction methods usually in rubber composition, Soxhlet extractor is utilized to be extracted by organic principle in sizing material, and then extract is carried out qualitative and quantitative analysis, soxhlet type requires that solvent reflux temperature is higher, be generally more than 90 DEG C, and by longer for complete for organic principle in sizing material extraction times, be generally more than 24h.Under long-time high temperature extraction conditions, aging resister can be degraded under hot oxygen environment, also reacts to cause with other compounding ingredient in extract simultaneously and self loses, cause quantitative result on the low side.How to carry out quantitatively to aging resister organic in sizing material fast and accurately, it is the problem extremely paid close attention in industry, the present invention is intended to announce and a kind ofly utilizes ultrasonic extraction and the method for gas chromatography in conjunction with quantitative aging resister, this method avoids the impact of high temperature extracting on extract, substantially reduce organism extraction time, quantitative test fast and accurately, is better than the quantivative approach of all aging resister announced at present.
Summary of the invention
The present invention aims to provide the method for organic aging resister content in a kind of fast quantification sulfuration and mixing of rubber, described sulfuration and mixing of rubber include but not limited to natural or synthesis crude rubber (including but not limited to NR, BR, SBR, IIR, CIIR, BIIR, EPDM, CR, silica gel etc.) and their compound; Take rubber as the various Additives Products of carrier; Sulfuration and mixing rubber composition etc.
The object of the present invention is to provide the method for organic aging resister content in a kind of fast quantification sulfuration and mixing of rubber, specifically comprise the following steps:
Step 1, sample preparation: rubber is made 0 ~ 2mm
3rubber grain, take rubber grain described in 1 weight portion, add solvent orange 2 A ultrasonic extraction, in gained extract, add internal standard compound matter, concentrated stand-by;
Prepared by step 2, standard serial solution: the aging resister standard substance getting 3 ~ 8 parts of different qualities is placed in independently container respectively, after adding internal standard compound matter and solvent orange 2 A mixing, prepares 3 ~ 8 parts of standard solution;
Step 3, quantitative test: the chromatogram using gas chromatography test aging resister standard serial solution, draw out typical curve; Use the chromatogram of gas chromatography test sample, by contrasting with typical curve, the content of aging resister in quantitative measurement sizing material;
Gas chromatography test condition: use fid detector, detector temperature 250 ~ 350 DEG C, hydrogen flowing quantity 20 ~ 50mL/min, air mass flow 200 ~ 500mL/min, make-up gas 20 ~ 50mL/min, flow rate of carrier gas 1.0 ~ 2.0mL/min, injector temperature: 200 ~ 350 DEG C;
The control program of column temperature is: initial temperature 30 ~ 60 DEG C, and 5 ~ 20 DEG C/min rises to 260 ~ 360 DEG C, keeps 5 ~ 30min;
Wherein chromatographic column filler is non-substituted or partially substituted dimethyl polysiloxane or dimethyl arlydene silicone copolymers;
Wherein said partially substituted dimethyl polysiloxane, substituting group to be molar ratio the be diphenyl of 5 ~ 50%, phenyl, the cyanogen propylbenzene of 5 ~ 20%, the one in 5 ~ 20% dipropyl benzene of 5 ~ 50%; Described partially substituted dimethyl arlydene silicone copolymers is 5 ~ 50%-diphenyl, 50 ~ 95%-dimethyl arlydene silicone copolymers.
Preferably, in step 1, the mode preparing sizing material particle is hammer-shears system or prepares through liquid nitrogen frozen mill; Rubber powder granule size is preferably less than 1mm
3;
Preferably, in step 1, for vulcanized rubber, solvent orange 2 A can be one or more in alcohol, ketone, ether, aromatic hydrocarbons, halogenated hydrocarbons, the mixed solvent of preferred acetone-chloroform, in solvent orange 2 A, the ratio of acetone and chloroform adjusts according to the complexity extracted, and being preferably volume ratio is 20:80 ~ 80:20; Further, the volume ratio of preferred acetone and chloroform is 32:68;
Preferably, in step 1, for mixing of rubber, solvent orange 2 A can be one or more in alcohol, ketone, ether, preferred acetone;
Preferably, described step 1, ultrasonic frequency is single-frequency or multi-frequency combination, ultrasonic power be continuously or discontinuity ultrasonic, preferred ultrasonic frequency is 40 ~ 60KHz, the preferred continuous ultrasound of ultrasonic power, ultrasonic time is 10 ~ 90min preferably, ultrasonic temperature preferably 30 ~ 80 DEG C.Further, ultrasonic frequency is preferably 40KHz, and ultrasonic power is continuous ultrasound, and ultrasonic time is 20 ~ 60min preferably, ultrasonic temperature preferably 40 DEG C;
Preferably, in step 1 or 2, the consumption of internal standard compound matter is: 0.001-0.030 weight portion;
Wherein can quantitative aging resister comprise in p phenylenediamine type antioxidant, quinoline type antioxidant, naphthylamine antioxidant and phenol antiager one or more; Described internal standard compound matter be selected from caprylic acid methyl esters, isooctyl acid methyl esters, methyl hexadecanoate, methyl stearate, phenol, metacresol, catechol, resorcinol, p-dihydroxy-benzene one or more, preferred caprylic acid methyl esters is internal standard compound matter; Internal standard compound matter can be the internal standard compound matter directly weighed also can be the internal standard compound matter solution of preparation.
The invention has the advantages that:
(1) method of preparing sample variation, respectively has advantage, and the sample preparation of hammer-shears glue is convenient, and freeze grinding sample preparation particle is thinner, make aging resister be easy to by
Extract.
(2) ultrasonic extraction, has saved extraction time greatly.
(3) extraction temperature is lower, and extraction time is short, avoids the degraded of aging resister under hot oxygen environment and occurs with other compounding ingredient in proposition liquid
Reaction causes self loses.
(4) for vulcanized rubber and mixing of rubber, choose different solvents respectively and extract, propose better effects if, subsequent sample process is more convenient.
(5) quantitatively detect use fid detector, Accurate Determining can be carried out to the content of aging resister organic in extract; Quantitative detection uses vapor-phase chromatography, by contrasting with aging resister standard solution, and the content of aging resister in quantitative measurement sizing material.
(6) experimental repeatability, favorable reproducibility, analysis result accuracy rate is high, and error is little.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiments are only for purpose of explanation, and do not limit the scope of the invention and essence.
Embodiment 1: the quantitative test of aging resister in 1# elastomeric compound and vulcanized rubber is made in laboratory by oneself
Elastomeric compound basic recipe is (mass parts):
Component 1: Natural rubber 100; Carbon black N33045, white carbon 7000GR40, stearic acid (technical grade) 2.0, zinc paste 3.5, silane coupling agent X50S8.0, zinc stearate (laboratory self-control) 2.5, stearic acid pentaerythritol ester 1.0,
Component 2: aging resister 6PPD1.5, antioxidant A 2.0,
Component 3: sulphur 1.8, vulcanization accelerator NS 1.5,
Preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add the mixing 60s of Natural rubber, then add stearic acid, zinc paste continues mixing 40s, finally add carbon black, white carbon, silane coupling agent, zinc stearate, stearic acid pentaerythritol ester, mixing to temperature 160 DEG C, binder removal slice, cools stand-by, obtains one section of elastomeric compound; Adding mixing 60s in Banbury Banbury mixer by parking the one section of elastomeric compound being no less than 16 hours, adding component 2 and mixing 5 minutes, at 145 DEG C of binder removals, obtaining two-stage mixing glue; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients 3 in two-stage mixing glue, at the temperature of 70 DEG C, mixing 10min is carried out to said mixture, thus acquisition rubber composition, this composition and mixing of rubber sample to be measured; By above-mentioned mixing of rubber sample to be measured by vulcanizing press 150 DEG C of sulfurations 30 minutes, namely obtain cured rubber samples to be measured, be respectively used to following analytical test.
Mark storing solution preparation in 1.1: take 150.21mg caprylic acid methyl esters in 50mL volumetric flask, acetone constant volume.
1.2 hybrid standard stock sample solution preparations: take 254.65mg aging resister 6PPD, 278.75mg antioxidant A respectively in 50mL volumetric flask, acetone solution constant volume.
1.3 standard serial solution preparations: pipette standard model storing solution 0.5mL, 1.0mL, 1.5mL, 2.5mL, 3.5mL successively in 5 10mL volumetric flasks, add respectively in 1.0mL and use acetone constant volume after mark storing solution.
1.4 sizing material extract preparations:
Mixing of rubber: with MM400 mixed freezing beveller (German Retsch company produces), mixing of rubber sizing material is prepared into and is less than 0.01mm
3fine particle, take sizing material particulate samples 1010.22mg, 1005.61mg, 1009.12mg respectively and be placed in three 50mL tool plug rub oral examination tubes, as Duplicate Samples.Adding 15mL acetone with transfer pipet along test tube wall week, is 40KHz in ultrasonic frequency, temperature 50 C, continuous ultrasound 30min, and adding in 1.0mL and mix after mark storing solution, is extract.
Vulcanized rubber: with MM400 mixed freezing beveller (German Retsch company produces), vulcanizate compound is prepared into and is less than 0.01mm
3fine particle, take sizing material particulate samples 1075.41mg, 1195.15mg, 1056.87mg respectively and be placed in three 50mL tool plug rub oral examination tubes, as Duplicate Samples.Adding the mixed solvent (volume ratio is 32:68) of 15mL acetone-chloroform along test tube wall week with transfer pipet, is 40KHz in ultrasonic frequency, temperature 50 C, continuous ultrasound 30min, and adding in 1.0mL and use mixing after mark storing solution, is extract.
Standard serial solution and extract are entered GC systematic analysis.
Arranging chromatographic condition is: chromatographic column HP-5MS30m length * 0.25mm internal diameter * 0.25 μm of thickness; The control program of column temperature is: initial temperature 50 DEG C, and keep 2min, 10 DEG C/min rises to 310 DEG C, keeps 10min.Carrier gas: N2; Flow rate of carrier gas: 1mL/min.
Arranging FID test condition is: detector temperature 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 300mL/min, make-up gas 30mL/min, and test obtains the chromatogram of sample.
1.5 results calculate:
The content of aging resister calculates according to formula (1), (2):
The peak area A of aging resister and internal standard compound matter is obtained by extract and standard serial solution chromatogram
x, A
s, with the area ratio RA of aging resister in standard serial solution and internal standard compound matter for horizontal ordinate, in standard serial solution, the quality m of aging resister is ordinate drawing standard curve.
Obtain m=a × RA+b (1)
In formula (1),
A, b-standard curve fit coefficient;
The quality of m-aging resister;
The area ratio of RA-aging resister and internal standard compound matter, RA=A
x/ A
s.
The area ratio of aging resister and internal standard compound matter in sample extraction liquid is substituted into typical curve, calculates the quality of aging resister in sample.According to formula (2), calculate the content of aging resister in sizing material sample.
Wt% in formula (2)-be the content (unit: %) of aging resister in sizing material;
M
x-be the quality of aging resister in sizing material;
M
0-be the quality of sizing material.
Standard serial solution test data and typical curve list in table 1:
Table 1 standard serial solution test data and typical curve
In mixing and vulcanizate, aging resister 6PPD and antioxidant A result of calculation are listed in the table below 2 and table 3:
Aging resister 6PPD, antioxidant A result of calculation in table 2 elastomeric compound
Aging resister 6PPD, antioxidant A result of calculation in table 3 vulcanizate
By the theoretical percentage composition of aging resister in the known sizing material of basic recipe be: aging resister 6PPD0.72%, antioxidant A 0.96%.The relative error of elastomeric compound quantitative result is: aging resister 6PPD1.39%, antioxidant A 1.04%; The relative error of vulcanizate quantitative result is: aging resister 6PPD1.39%, antioxidant A 1.04%.
Embodiment 2: the quantitative test of aging resister in 2# elastomeric compound and vulcanized rubber is made in laboratory by oneself
Elastomeric compound basic recipe is (mass parts):
Component 1: Natural rubber 100; Carbon black N33045, white carbon 7000GR40, stearic acid (technical grade) 2.0, zinc paste 3.5, silane coupling agent X50S8.0, zinc stearate (laboratory self-control) 2.5, stearic acid pentaerythritol ester 1.0,
Component 2: antioxidant 4010NA 2.5, antioxidant D 1.5,
Component 3: sulphur 1.8, vulcanization accelerator NS 1.5,
Preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add the mixing 60s of Natural rubber, then add stearic acid, zinc paste continues mixing 40s, finally add carbon black, white carbon, silane coupling agent, zinc stearate, stearic acid pentaerythritol ester, mixing to temperature 160 DEG C, binder removal slice, cools stand-by, obtains one section of elastomeric compound; Adding mixing 60s in Banbury Banbury mixer by parking the one section of elastomeric compound being no less than 16 hours, adding component 2 and mixing 5 minutes, at 145 DEG C of binder removals, obtaining two-stage mixing glue; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients 3 in two-stage mixing glue, at the temperature of 70 DEG C, mixing 10min is carried out to said mixture, thus acquisition rubber composition, this composition and mixing of rubber sample to be measured; By above-mentioned mixing of rubber sample to be measured by vulcanizing press 150 DEG C of sulfurations 30 minutes, namely obtain cured rubber samples to be measured, be respectively used to following analytical test.
Mark storing solution preparation in 2.1: take 150.21mg caprylic acid methyl esters in 50mL volumetric flask, acetone constant volume.
2.2 hybrid standard stock sample solution preparations: take 245.85mg antioxidant 4010NA, 292.30mg antioxidant D respectively in 50mL volumetric flask, acetone solution constant volume.
2.3 standard serial solution preparations: pipette standard model storing solution 0.5mL, 1.0mL, 1.5mL, 2.5mL, 3.5mL successively in 5 10mL volumetric flasks, add respectively in 1.0mL and use acetone constant volume after mark storing solution.
2.4 sizing material extract preparations:
Mixing of rubber: with scissors mixing of rubber sizing material is prepared into and is less than 1.0mm
3particle, take sizing material particulate samples 1105.64mg, 1095.25mg, 1053.42mg respectively and be placed in three 50mL tool plug rub oral examination tubes, as Duplicate Samples.Adding 15mL acetone with transfer pipet along test tube wall week, is 40KHz in ultrasonic frequency, temperature 50 C, continuous ultrasound 60min, and adding in 1.0mL and mix after mark storing solution, is extract.
Vulcanized rubber: with scissors vulcanizate compound is prepared into and is less than 1.0mm
3particle, take sizing material particulate samples 1094.37mg, 1081.68mg, 1073.84mg respectively and be placed in three 50mL tool plug rub oral examination tubes, as Duplicate Samples.Adding the mixed solvent (volume ratio is 32:68) of 15mL acetone-chloroform along test tube wall week with transfer pipet, is 40KHz in ultrasonic frequency, temperature 50 C, continuous ultrasound 60min, and adding in 1.0mL and use mixing after mark storing solution, is extract.
Standard serial solution and extract are entered GC systematic analysis.
Arranging chromatographic condition is: chromatographic column HP-5MS30m length * 0.25mm internal diameter * 0.25 μm of thickness; The control program of column temperature is: initial temperature 50 DEG C, and keep 2min, 10 DEG C/min rises to 310 DEG C, keeps 10min.Carrier gas: N2; Flow rate of carrier gas: 1mL/min.
Arranging FID test condition is: detector temperature 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 300mL/min, make-up gas 30mL/min, and test obtains the chromatogram of sample.
2.5 results calculate:
Calculate according to formula (1), (2) described in embodiment 1, standard serial solution test data and typical curve list in table 4, and in elastomeric compound and vulcanizate, antioxidant 4010NA and antioxidant D result of calculation are listed in the table below 5 and table 6:
Table 4 standard serial solution test data and typical curve
Antioxidant 4010NA, antioxidant D result of calculation in table 5 elastomeric compound
Antioxidant 4010NA, antioxidant D result of calculation in table 6 vulcanizate
By the theoretical percentage composition of aging resister in the known sizing material of basic recipe be: antioxidant 4010NA 1.19%, antioxidant D 0.72%.The relative error of elastomeric compound quantitative result is: antioxidant 4010NA 0.84%, antioxidant D 1.41%; The relative error of vulcanizate quantitative result is: aging resister 6PPD1.68%, antioxidant A 1.41%.
Embodiment 3: the quantitative test (having been determined in sizing material containing aging resister 6PPD and aging resister 4030 by other analysis means) of aging resister in snowfield tire (205/55R16) sidewall rubber of German continent
Mark storing solution preparation in 3.1: take 150.21mg caprylic acid methyl esters in 50mL volumetric flask, acetone constant volume.
3.2 hybrid standard stock sample solution preparations: take 254.65mg aging resister 6PPD, 246.59mg aging resister 4030 respectively in 50mL volumetric flask, acetone solution constant volume.
3.3 standard serial solution preparations: pipette standard model storing solution 0.5mL, 1.0mL, 1.5mL, 2.5mL, 3.5mL successively in 5 10mL volumetric flasks, add respectively in 1.0mL and use acetone constant volume after mark storing solution.
3.4 sizing material extract preparations: with MM400 mixed freezing beveller (German Retsch company produces), sizing material is prepared into and is less than 0.01mm
3fine particle, take sizing material particulate samples 1020.52mg, 1085.35mg, 1064.27mg respectively and be placed in three 50mL tool plug rub oral examination tubes, as Duplicate Samples.Adding the mixed solvent (volume ratio is 32:68) of 15mL acetone-chloroform along test tube wall week with transfer pipet, is 40KHz in ultrasonic frequency, temperature 50 C, continuous ultrasound 30min, and adding in 1.0mL and use mixing after mark storing solution, is extract.
Standard series and extract are entered GC systematic analysis.
Arranging chromatographic condition is: chromatographic column HP-5MS30m length * 0.25mm internal diameter * 0.25 μm of thickness; The control program of column temperature is: initial temperature 50 DEG C, and keep 2min, 10 DEG C/min rises to 310 DEG C, keeps 10min.Carrier gas: N2; Flow rate of carrier gas: 1mL/min.
Arranging FID test condition is: detector temperature 300 DEG C, hydrogen flowing quantity 30mL/min, air mass flow 300mL/min, make-up gas 30mL/min, and test obtains the chromatogram of sample.
3.5 results calculate:
Calculate according to formula (1), (2), standard serial solution test data and typical curve list in table 7, and in sidewall rubber, aging resister 6PPD and aging resister 4030 result of calculation list in table 8:
Table 7 standard serial solution test data and typical curve
Aging resister 6PPD, aging resister 4030 result of calculation in table 8 sidewall rubber
Claims (10)
1. the quick quantitative analytic method of aging resister in rubber, is characterized in that, comprise the following steps:
Step 1, sample preparation: rubber is made 0 ~ 2mm
3rubber grain, take 1 parts by weight of rubber particle, add solvent orange 2 A ultrasonic extraction, in gained extract, add internal standard compound matter, concentrated stand-by;
Prepared by step 2, standard serial solution: the aging resister standard substance getting 3 ~ 8 parts of different qualities is placed in independently container respectively, after adding internal standard compound matter and solvent orange 2 A mixing, prepares 3 ~ 8 parts of standard solution;
Step 3, quantitative test: the chromatogram using gas chromatography test aging resister standard serial solution, draw out typical curve; Use the chromatogram of gas chromatography test sample, by contrasting with typical curve, the content of aging resister in quantitative measurement sizing material;
Gas chromatography test condition: use fid detector, detector temperature 250 ~ 350 DEG C, hydrogen flowing quantity 20 ~ 50mL/min, air mass flow 200 ~ 500mL/min, make-up gas 20 ~ 50mL/min, flow rate of carrier gas 1.0 ~ 2.0mL/min, injector temperature: 200 ~ 350 DEG C;
The control program of column temperature is: initial temperature 30 ~ 60 DEG C, and 5 ~ 20 DEG C/min rises to 260 ~ 360 DEG C, keeps 5 ~ 30min;
Wherein chromatographic column filler is non-substituted or partially substituted dimethyl polysiloxane or dimethyl arlydene silicone copolymers;
Wherein said partially substituted dimethyl polysiloxane, substituting group is the diphenyl of 5 ~ 50% of molar ratio, phenyl, the cyanogen propylbenzene of 5 ~ 20%, the one in 5 ~ 20% dipropyl benzene of 5 ~ 50%; Described partially substituted dimethyl arlydene silicone copolymers is 5 ~ 50%-diphenyl, 50 ~ 95%-dimethyl arlydene silicone copolymers.
2. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, it is characterized in that, described rubber is sulfuration or half finished rubber, be selected from natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, chlorinated scoline, brombutyl, ethylene-propylene-diene rubber, neoprene, silica gel a kind of or their compound, take rubber as the various Additives Products of carrier, and sulfuration or mixing rubber composition.
3. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, is characterized in that, for the organic aging resister in quantitative sizing material, comprise p phenylenediamine type antioxidant, quinoline type antioxidant, naphthylamine antioxidant and phenol antiager.
4. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, is characterized in that, the mode preparing rubber grain in described step 1 is for by scissors hammer-shears system or prepare through liquid nitrogen frozen mill.
5. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, is characterized in that, described solvent orange 2 A be selected from alcohol, ketone, ether, aromatic hydrocarbons, halogenated hydrocarbons one or more.
6. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, is characterized in that, when testing half finished rubber, and the preferred acetone of described solvent orange 2 A; When testing vulcanized rubber, the mixed solvent of the preferred acetone-chloroform of described solvent orange 2 A.
7. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, it is characterized in that, ultrasonic frequency is single-frequency or multi-frequency combination, ultrasonic power be continuous or discontinuity ultrasonic, ultrasonic time is 10 ~ 90min preferably, ultrasonic temperature preferably 30 ~ 80 DEG C.
8. in a kind of rubber as described in claim 1 or 7, the quick quantitative analytic method of aging resister, is characterized in that, described ultrasonic frequency is 40KHz, and ultrasonic power is continuous ultrasound.
9. the quick quantitative analytic method of aging resister in a kind of rubber as claimed in claim 1, is characterized in that, described internal standard compound matter is the internal standard compound matter solution of internal standard compound matter or the preparation directly weighed; Internal standard compound matter is selected from the one in caprylic acid methyl esters, isooctyl acid methyl esters, methyl hexadecanoate, methyl stearate, phenol, metacresol, catechol, resorcinol, p-dihydroxy-benzene.
10. in a kind of rubber as described in claim 1 or 9, the quick quantitative analytic method of aging resister, is characterized in that, described internal standard compound matter is caprylic acid methyl esters.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110220997A (en) * | 2019-07-08 | 2019-09-10 | 哈尔滨学院 | A kind of method of antioxidant in the detection flesh of fish |
| CN110220997B (en) * | 2019-07-08 | 2022-10-11 | 哈尔滨学院 | Method for detecting antioxidant in fish meat |
| CN112834655A (en) * | 2020-12-31 | 2021-05-25 | 上海微谱化工技术服务有限公司 | Qualitative detection method for vulcanization accelerator in rubber and application thereof |
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