CN109270019A - The measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide - Google Patents
The measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide Download PDFInfo
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- CN109270019A CN109270019A CN201811399659.3A CN201811399659A CN109270019A CN 109270019 A CN109270019 A CN 109270019A CN 201811399659 A CN201811399659 A CN 201811399659A CN 109270019 A CN109270019 A CN 109270019A
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 133
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002835 absorbance Methods 0.000 claims abstract description 48
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 229960001760 dimethyl sulfoxide Drugs 0.000 claims description 66
- 239000000243 solution Substances 0.000 claims description 63
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012086 standard solution Substances 0.000 claims description 10
- 230000008033 biological extinction Effects 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims 2
- WXQDFOGZIYLEGP-UHFFFAOYSA-N C(C(C)C)#N.C(C(C)C)#N.[N] Chemical compound C(C(C)C)#N.C(C(C)C)#N.[N] WXQDFOGZIYLEGP-UHFFFAOYSA-N 0.000 claims 1
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 11
- 239000004917 carbon fiber Substances 0.000 abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 11
- 238000007380 fibre production Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 3
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- -1 azo Nitrile Chemical class 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
This application discloses a kind of measuring methods of azodiisobutyronitrile concentration in dimethyl sulfoxide, comprising the following steps: establishes standard working curve: configuring the azodiisobutyronitrile solution of various concentration；At 350nm wavelength and 210nm wavelength, the absorbance of each solution of configuration is measured；Standard working curve is established as ordinate using the absorbance measured, and calculates regression formula；Azodiisobutyronitrile concentration in measurement dimethyl sulfoxide: at 350nm wavelength and/or 210nm wavelength, solution absorbance to be measured is measured；Azodiisobutyronitrile concentration in dimethyl sulfoxide is calculated according to regression formula.The application makes the concentration mensuration of azodiisobutyronitrile in dimethyl sulfoxide have suitable method, has filled up technological gap；It it also allows to recycle in carbon fiber production using the azodiisobutyronitrile that is mingled in dimethyl sulfoxide, avoid being difficult to carbon fiber caused by measuring because of concentration of low quality.
Description
Technical field
The application belongs to carbon fiber production technical field, and in particular to azodiisobutyronitrile concentration in a kind of dimethyl sulfoxide
Measuring method.
Background technique
Azodiisobutyronitrile (AIBN) be white crystals or crystalline powder, it is not soluble in water, be dissolved in ether, methanol, ethyl alcohol,
Propyl alcohol chloroform, dichloroethanes, ethyl acetate, benzene etc., mostly oil-soluble initiator.
Azodiisobutyronitrile is oil-soluble azo initiator, and azo-initiator stable reaction is first order reaction, does not have
Side reaction, relatively good control, so being widely used in high molecular research and production.Furthermore, it can also be used to other organic syntheses.
The concentration determination of azodiisobutyronitrile is at home mainly using being decomposition using azodiisobutyronitrile at present, according to
Nitrogen content that it is released determines the content of azodiisobutyronitrile；And in carbon fiber production, the method not only instrument
Valuableness, test it is cumbersome, test be then azodiisobutyronitrile in dimethyl sulfoxide (DMSO) concentration, due to two isobutyl of azo
Nitrile is in dimethyl sulfoxide, so it is not available kjeldahl apparatus, so at home and in industry, azo two in dimethyl sulfoxide
The measurement of isobutyronitrile concentration is without detection method, and there are technology vacancies.Therefore, it in carbon fiber production process, is mixed if recycling uses
The miscellaneous azodiisobutyronitrile in dimethyl sulfoxide is easy to appear because being difficult to cause carbon due to measuring azodiisobutyronitrile actual concentrations
The undesirable consequence of fiber quality.
Summary of the invention
In view of drawbacks described above in the prior art or deficiency, it is dense to be intended to provide azodiisobutyronitrile in a kind of dimethyl sulfoxide
The measuring method of degree.
The application provides a kind of measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide, comprising the following steps:
It establishes standard working curve: configuring the dimethyl sulphoxide solution of the azodiisobutyronitrile of various concentration；With reagent sky
It is white at 350nm wavelength and 210nm wavelength, to measure the suction of each solution of configuration using ultraviolet-uisible spectrophotometer for reference
Luminosity；Using the absorbance measured as ordinate, using azodiisobutyronitrile concentration in each solution of configuration as abscissa, standard is established
Working curve, and calculate regression formula；
It measures azodiisobutyronitrile concentration in dimethyl sulfoxide to be measured: using reagent blank as reference, using UV, visible light
Spectrophotometer measures the dimethyl sulphoxide solution of azodiisobutyronitrile to be measured at 350nm wavelength and/or 210nm wavelength
Absorbance；Azodiisobutyronitrile concentration in dimethyl sulfoxide is calculated according to regression formula.
The concentration mensuration of azodiisobutyronitrile is different from the measurement of other solution, the azodiisobutyronitrile solution of various concentration
Under ultraviolet-uisible spectrophotometer Same Wavelength, not linear rule.Experiment discovery, within the scope of a certain concentration, azo
The dimethyl sulphoxide solution of bis-isobutyronitrile absorbance at 350nm wavelength is linearly regular, in another concentration range, azo two
Absorbance of the dimethyl sulphoxide solution of isobutyronitrile at 210nm wavelength is in another linear rule；This makes in dimethyl sulfoxide
The concentration mensuration of azodiisobutyronitrile has suitable method, has filled up technological gap；In addition, the union of this two sections of concentration ranges
The concentration range for covering the dimethyl sulphoxide solution of azodiisobutyronitrile recyclable in carbon fiber production, so that carbon fiber
It can be recycled in dimension production using the azodiisobutyronitrile being mingled in dimethyl sulfoxide, Accurate Determining azodiisobutyronitrile is dense
Degree avoids being difficult to raw material investment ratio inaccuracy caused by measuring because of concentration, it is of low quality in turn result in carbon fiber.
Further, in establishing standard working curve step, at 350nm wavelength, two isobutyl of azo of configuration is measured
Absorbance of the nitrile mass percentage concentration in the solution of 0.50%-4.00%.Test discovery, azodiisobutyronitrile in dimethyl sulfoxide
For mass percentage concentration in 0.50%-4.00%, the absorbance at 350nm wavelength is linearly regular, meets lambert Bill
Law, obtained curve can be used as in dimethyl sulfoxide azodiisobutyronitrile mass percentage concentration in 0.50%-4.00%
Standard working curve, for measuring concentration of the azodiisobutyronitrile in the concentration range in dimethyl sulfoxide to be measured.
Further, in establishing standard working curve step, at 210nm wavelength, two isobutyl of azo of configuration is measured
Absorbance of the nitrile mass percentage concentration in the solution of 4.00%-7.01%.Test discovery, azodiisobutyronitrile in dimethyl sulfoxide
For mass percentage concentration in 4.00%-7.01%, the absorbance at 210nm wavelength is linearly regular, meets lambert Bill
Law, obtained curve can be used as in dimethyl sulfoxide azodiisobutyronitrile mass percentage concentration in 4.00%-7.01%
Standard working curve, for measuring concentration of the azodiisobutyronitrile in the concentration range in dimethyl sulfoxide to be measured.
Further, regression formula are as follows:
Further, it measures azodiisobutyronitrile concentration step in dimethyl sulfoxide and specifically includes operation step in detail below
It is rapid:
Azodiisobutyronitrile mass concentration in solution to be measured is estimated, if estimation result is with reagent blank less than 4.00%
Reference measures solution to be measured absorbance at 350nm using ultraviolet-uisible spectrophotometer, and according to y350=0.8209x+
0.0510 calculates azodiisobutyronitrile concentration in solution to be measured；If estimating result is greater than 4.00%, solution to be measured is measured in 210nm
Locate absorbance, and according to y210=-0.0103x+0.3502 calculates azodiisobutyronitrile concentration in solution to be measured.
Further, it measures azodiisobutyronitrile concentration step in dimethyl sulfoxide and specifically includes operation step in detail below
It is rapid:
Using reagent blank as reference, using ultraviolet-uisible spectrophotometer, solution to be measured is inhaled at 210nm wavelength
Luminosity measurement；If absorbance is measured between 0.278-0.309, according to y210=-0.0103x+0.3502 calculates concentration；If surveying
The absorbance obtained is greater than 0.309, solution to be measured is carried out absorbance test at 350nm wavelength, according to y350=0.8209x+
0.0510 calculates azodiisobutyronitrile concentration；If measuring absorbance less than 0.278 or close to 0.278, redeterminated after dilution.
Further, the application is further comprising the steps of:
Configuration standard solution: the dimethyl sulfoxide standard solution of azodiisobutyronitrile is configured.
Further, the storage temperature of standard solution, dilution and solution to be measured is 20-28 DEG C, avoids temperature too low
It causes dimethyl sulfoxide to crystallize or temperature is excessively high that azodiisobutyronitrile is caused to decompose.
The application has the advantages and positive effects of:
1, it changes domestic at present decompose merely with azodiisobutyronitrile and discharges nitrogen to measure azodiisobutyronitrile concentration
Test method；
2, by ultraviolet spectrometry degree meter, the concentration of unknown sample effectively can quickly be measured；
3, easy to operate, be easily achieved；
4, required instrument price is cheap.
The technical issues of in addition to the application described above solution, constitutes the technical characteristic of technical solution and by these
Except advantage brought by the technical characteristic of technical solution, wrapped in other technologies problem that the application can solve, technical solution
Advantage brought by the other technical characteristics contained and these technical characteristics, makees further details of hereinafter in conjunction with attached drawing
Explanation.
Detailed description of the invention
By reading a detailed description of non-restrictive embodiments in the light of the attached drawings below, the application's is other
Feature, objects and advantages will become more apparent upon:
Fig. 1 be azodiisobutyronitrile provided by the embodiments of the present application dimethyl sulphoxide solution at 350nm wavelength extinction
Degree-concentration curve；
Fig. 2 be azodiisobutyronitrile provided by the embodiments of the present application dimethyl sulphoxide solution at 210nm wavelength extinction
Degree-concentration curve；
Fig. 3 is azodiisobutyronitrile standard working curve figure in dimethyl sulfoxide provided by the embodiments of the present application.
Specific embodiment
The application is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining related invention, rather than the restriction to the invention.Below with reference to the accompanying drawings and combine real
Example is applied the application is described in detail.
The present embodiment provides a kind of measuring methods of azodiisobutyronitrile concentration in dimethyl sulfoxide.
1, configuration standard solution
7.01g azodiisobutyronitrile is accurately weighed, is dissolved in 92.99g dimethyl sulfoxide, obtaining mass concentration is
The dimethyl sulfoxide standard solution of 7.01% azodiisobutyronitrile；Ready-to-use, the holding time is no more than after the completion of configuration
30min, storage temperature is at 25 DEG C or so.
2, standard working curve is established
(1) standard solution is diluted with dimethyl sulfoxide, obtain azodiisobutyronitrile mass concentration 0.50%,
1.00%, 1.50%, 2.00%, 2.50%, 3.00%, 3.50%, 4.00%, 4.50%, 5.00%, 5.50%, 6.00%,
6.50%, 7.01% dilution；Using reagent blank as reference, using U-3900 ultraviolet-uisible spectrophotometer, with 1cm colorimetric
Ware measures the absorbance of each dilution at 350nm wavelength, using absorbance at the 350nm wavelength measured as ordinate, with dilute
Releasing azodiisobutyronitrile mass percentage concentration in liquid is abscissa, and the dimethyl sulphoxide solution for obtaining azodiisobutyronitrile exists
Absorbance (A at 350nm wavelength350)-concentration (CAIBN) curve graph, as shown in Figure 1.
It will be seen from figure 1 that absorbance of the azodiisobutyronitrile at 350nm wavelength in dimethyl sulfoxide, in azo two
Isobutyronitrile mass percentage concentration is presented linear within the scope of 0.50%-4.00% with azodiisobutyronitrile mass percentage concentration
Rule, fitting, obtains formula:
y350=0.8209x+0.0510,0.50≤x < 4.00, R2=0.9992 (I)
It is seen also in fig. l that absorbance of the azodiisobutyronitrile at 350nm wavelength in dimethyl sulfoxide, in azo
After bis-isobutyronitrile mass percentage concentration is greater than 4.00%, linear rule is not presented with azodiisobutyronitrile mass percentage concentration；Together
When can also be seen that azodiisobutyronitrile mass percentage concentration be greater than 4.00% after, extinction of the solution at 350nm wavelength
Degree will not be equal with absorbance of the azodiisobutyronitrile mass percentage concentration within the scope of 0.50%-4.00%.
In practical measurement dimethyl sulfoxide when azodiisobutyronitrile, establish in standard working curve step, it is not necessary to measure
Dilution of the mass concentration greater than 4.00% absorbance A at 350nm wavelength350。
(2) standard solution is diluted with dimethyl sulfoxide, obtain azodiisobutyronitrile mass concentration 0.50%,
1.00%, 1.50%, 2.00%, 2.50%, 3.00%, 3.50%, 4.00%, 4.50%, 5.00%, 5.50%, 6.00%,
6.50%, 7.01% dilution；Using reagent blank as reference, using U-3900 ultraviolet-uisible spectrophotometer, with 1cm colorimetric
Ware measures the absorbance of each dilution at 210nm wavelength, using absorbance at the 210nm wavelength measured as ordinate, with dilute
Releasing azodiisobutyronitrile mass percentage concentration in liquid is abscissa, and the dimethyl sulphoxide solution for obtaining azodiisobutyronitrile exists
Absorbance (A at 210nm wavelength210)-concentration (CAIBN) curve graph, as shown in Figure 2.
Figure it is seen that absorbance of the azodiisobutyronitrile at 210nm wavelength in dimethyl sulfoxide, in azo two
Linear rule is presented within the scope of 4.00%-7.01% in isobutyronitrile concentration, and fitting obtains formula:
y210=-0.0103x+0.3502,4.00≤x≤7.01, R2=0.9992 (II)
It can further be seen from figure 2 that absorbance of the azodiisobutyronitrile at 210nm wavelength in dimethyl sulfoxide, works as azo
When bis-isobutyronitrile mass percentage concentration is less than 4.00%, linear rule is not presented with azodiisobutyronitrile mass percentage concentration；Together
When can also be seen that when azodiisobutyronitrile mass percentage concentration is less than 4.00%, absorbance of the solution at 350nm wavelength
Will not with azodiisobutyronitrile mass percentage concentration be greater than 4.00% when absorbance it is equal.
In practical measurement dimethyl sulfoxide when azodiisobutyronitrile, establish in standard working curve step, it is not necessary to measure
Dilution of the mass concentration less than 4.00% absorbance A at 210nm wavelength210。
(3) according to Fig. 1 and Fig. 2, standard working curve as shown in Figure 3 is established；And according to formula I and formula II, obtain returning public
Formula:
3, azodiisobutyronitrile concentration in dimethyl sulfoxide to be measured is measured
Using reagent blank as reference, using ultraviolet-uisible spectrophotometer, with 1cm cuvette, in 350nm wavelength and/or
At 210nm wavelength, the dimethyl sulphoxide solution absorbance of azodiisobutyronitrile to be measured is measured；It is counted according to regression formula (formula III)
Calculation obtains azodiisobutyronitrile concentration in dimethyl sulfoxide.
In this step, need to prejudge azodiisobutyronitrile concentration range in solution to be measured in advance.It was produced in carbon fiber
Cheng Zhong, azodiisobutyronitrile concentration can rule of thumb be estimated in solution to be measured.If estimating result less than 4.00%, with reagent sky
It is white using ultraviolet-uisible spectrophotometer to measure solution to be measured absorbance at 350nm for reference, and calculated according to formula I to be measured
Azodiisobutyronitrile concentration in solution；If estimating result is greater than 4.00%, solution to be measured absorbance at 210nm, and root are measured
Azodiisobutyronitrile concentration in solution to be measured is calculated according to formula II.
For cannot rule of thumb prejudge the solution to be measured of concentration range, first solution should be inhaled at 210nm wavelength
Luminosity measurement；If measuring absorbance between 0.278-0.309, illustrate that azodiisobutyronitrile concentration exists in solution to be measured
4.00%-7.01% calculates concentration according to formula II；If measuring absorbance less than 0.278 or close to 0.278, illustrate to be measured
Azodiisobutyronitrile concentration is prejudged again after should diluting and is measured (in fact, in dimethyl sulfoxide 7.01% or so in solution
Azodiisobutyronitrile concentration be greater than 7.01% after, with solution shake etc. have at any time azodiisobutyronitrile be precipitated, usually not
Have the stablizing solution presence that concentration is greater than 7.01%)；If the absorbance measured is greater than 0.309, illustrate azo in solution to be measured
Bis-isobutyronitrile concentration should change survey solution to be measured and carry out absorbance test at 350nm wavelength less than 4.00%, and be counted according to formula I
Calculate azodiisobutyronitrile concentration.
In the other embodiments of the application, standard solution can not also be configured, is directly dissolved in azodiisobutyronitrile
In dimethyl sulfoxide, it is configured to the solution of various concentration, to establish standard curve.
Application scheme utilizes UV, visible light by the dimethyl sulphoxide solution of the azodiisobutyronitrile of preparation various concentration
Spectrophotometer establishes the curve of various concentration according to langbobier law, obtains sample by the absorbance of test sample
Concentration solves the vacancy of azodiisobutyronitrile concentration determination in dimethyl sulfoxide in industry.The application produces carbon fiber
In can recycle using the azodiisobutyronitrile that is mingled in dimethyl sulfoxide, Accurate Determining azodiisobutyronitrile concentration avoids
Ratio inaccuracy is put into because concentration is difficult to raw material caused by measuring, to improve carbon fiber quality.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (8)
1. the measuring method of azodiisobutyronitrile concentration in a kind of dimethyl sulfoxide, which comprises the following steps:
It establishes standard working curve: configuring the dimethyl sulphoxide solution of the azodiisobutyronitrile of various concentration；It is with reagent blank
Reference at 350nm wavelength and 210nm wavelength, measures the extinction of each solution of configuration using ultraviolet-uisible spectrophotometer
Degree；Using the absorbance measured as ordinate, using azodiisobutyronitrile concentration in each solution of configuration as abscissa, standard work is established
Make curve, and calculates regression formula；
Measure azodiisobutyronitrile concentration in dimethyl sulfoxide: using reagent blank as reference, using ultraviolet-uisible spectrophotometer,
At 350nm wavelength and/or 210nm wavelength, the dimethyl sulphoxide solution absorbance of azodiisobutyronitrile to be measured is measured；According to
Azodiisobutyronitrile concentration in dimethyl sulfoxide is calculated in regression formula.
2. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 1, which is characterized in that
Described to establish in standard working curve step, at 350nm wavelength, the azodiisobutyronitrile mass concentration for measuring configuration exists
The absorbance of the solution of 0.50%-4.00%.
3. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 1, which is characterized in that
Described to establish in standard working curve step, at 210nm wavelength, the azodiisobutyronitrile mass concentration for measuring configuration exists
The absorbance of the solution of 4.00%-7.01%.
4. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 1, which is characterized in that institute
State regression formula are as follows:
5. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 4, which is characterized in that institute
It states azodiisobutyronitrile concentration step in measurement dimethyl sulfoxide and specifically includes operating procedure in detail below:
Estimate azodiisobutyronitrile mass concentration in solution to be measured, if estimation result less than 4.00%, using reagent blank as reference,
Using ultraviolet-uisible spectrophotometer, solution to be measured absorbance at 350nm is measured, and according to y350=0.8209x+0.0510
Calculate azodiisobutyronitrile concentration in solution to be measured；If estimating result is greater than 4.00%, solution to be measured extinction at 210nm is measured
Degree, and according to y210=-0.0103x+0.3502 calculates azodiisobutyronitrile concentration in solution to be measured.
6. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 4, which is characterized in that institute
It states azodiisobutyronitrile concentration step in measurement dimethyl sulfoxide and specifically includes operating procedure in detail below:
Using reagent blank as reference, using ultraviolet-uisible spectrophotometer, extinction of the solution to be measured at 210nm wavelength is measured
Degree；If absorbance is measured between 0.278-0.309, according to y210=-0.0103x+0.3502 calculates concentration；If the suction measured
Luminosity is greater than 0.309, absorbance of the solution to be measured at 350nm wavelength is measured, according to y350=0.8209x+0.0510 calculates even
Nitrogen bis-isobutyronitrile concentration；If measuring absorbance less than 0.278 or close to 0.278, redeterminated after dilution.
7. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 1, which is characterized in that mark
The storage temperature of quasi- solution, dilution and solution to be measured is 20-28 DEG C.
8. the measuring method of azodiisobutyronitrile concentration in dimethyl sulfoxide according to claim 1, which is characterized in that also
The following steps are included:
Configuration standard solution: the dimethyl sulfoxide standard solution of azodiisobutyronitrile is configured.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609007A (en) * | 2019-09-19 | 2019-12-24 | 兰州蓝星纤维有限公司 | Method for quantitatively determining azobisisobutyronitrile by ultraviolet spectroscopy |
| CN110824087A (en) * | 2019-11-14 | 2020-02-21 | 兰州蓝星纤维有限公司 | Quantitative detection method for residual azodiisobutyronitrile in solvent |
-
2018
- 2018-11-22 CN CN201811399659.3A patent/CN109270019A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609007A (en) * | 2019-09-19 | 2019-12-24 | 兰州蓝星纤维有限公司 | Method for quantitatively determining azobisisobutyronitrile by ultraviolet spectroscopy |
| CN110824087A (en) * | 2019-11-14 | 2020-02-21 | 兰州蓝星纤维有限公司 | Quantitative detection method for residual azodiisobutyronitrile in solvent |
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