CN105738496A - Quantitative analysis method of low-content azodiisobutyronitrile - Google Patents
Quantitative analysis method of low-content azodiisobutyronitrile Download PDFInfo
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- CN105738496A CN105738496A CN201410768781.9A CN201410768781A CN105738496A CN 105738496 A CN105738496 A CN 105738496A CN 201410768781 A CN201410768781 A CN 201410768781A CN 105738496 A CN105738496 A CN 105738496A
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- 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 111
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 7
- UBYDSYHGCPVBEQ-UHFFFAOYSA-N chloroform;propan-1-ol Chemical compound CCCO.ClC(Cl)Cl UBYDSYHGCPVBEQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N alpha-methyl toluene Natural products CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- -1 isopropyl cyanide free radical Chemical class 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 229960004756 ethanol Drugs 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920005479 Lucite® Polymers 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical group O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A quantitative analysis method of low-content azobisisobutyronitrile comprises the following steps: (1) drawing a standard curve of the azobisisobutyronitrile by using a gas chromatography-mass spectrometer and a gas chromatograph, taking the peak area of the azobisisobutyronitrile as a vertical coordinate and the content of the azobisisobutyronitrile as a horizontal coordinate, and solving a standard curve equation; (2) and (3) detecting the peak area of the azobisisobutyronitrile by using a gas chromatograph-mass spectrometer and a gas chromatograph, substituting the peak area into the standard curve equation of the azobisisobutyronitrile obtained in the step (1), and calculating to obtain the content of the azobisisobutyronitrile in the sample to be detected.
Description
Technical field
The present invention relates to a kind of analysis method, be specifically related to a kind of quantitative analysis method suitable in low content azodiisobutyronitrile.Its instrument used is gas chromatograph and gas chromatograph-mass spectrometer (GC-MS).
Background technology
Azodiisobutyronitrile is mainly used in plastics, rubber foaming agent, also the polymerization initiator of the high molecular polymers such as polrvinyl chloride, polyvinyl acetate, polyacrylonitrile, lucite and ion exchange resin is made, fusing point is (102～104) DEG C, easily decomposes owing to being heated and at room temperature slowly decomposition produces free radical and discharges nitrogen (catabolic process is shown in Scheme1).Therefore, the effective content measuring azodiisobutyronitrile is necessary.
About the quantitative approach of azodiisobutyronitrile, and Tian Fengbi etc. (Sichuan chemical industry, 1997, (2), 35～37) adopt gas method, by heating the volume recording the nitrogen that azodiisobutyronitrile decomposes release, converse the percentage composition of azodiisobutyronitrile；The diligent employing of Pan makes sample decompose in high boiling solvent Ketohexamethylene, measures the nitrogen precipitated out with eudiometry, thus calculating the content of azodiisobutyronitrile.There is the shortcoming such as troublesome poeration, calculating process complexity in both approaches.Polyacrylonitrile in acrylonitrile polymerization liquid through precipitating, being filtered to remove, is adopted liquid chromatograph to make standard curve determination azodiisobutyronitrile residual volume by Lu Dairen etc. (Patent publication No: CN101915844A).Owing to azodiisobutyronitrile dissolubility in precipitant is non-normally low, therefore the method is only applicable in sample containing the analysis lower than 200 μ g/g azodiisobutyronitriles.Therefore, set up a kind of easy to operate, calculate simple, analyze accurately quickly and be applicable to the analysis method tool of low content azodiisobutyronitrile and be of great significance.
Summary of the invention
The present invention seeks to a kind of easy to operate, calculate analysis method that is simple and that be applicable to low content azodiisobutyronitrile.
The present invention provides the quantitative analysis method of a kind of low content azodiisobutyronitrile, comprises the steps:
(1) Specification Curve of Increasing of azodiisobutyronitrile
The standard specimen of the different azodiisobutyronitrile content of preparation, adopt gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph, with the peak area of azodiisobutyronitrile for vertical coordinate, with azodiisobutyronitrile content for abscissa, it is depicted as the standard curve of azodiisobutyronitrile, tries to achieve standard curve equation；
(2) the azodiisobutyronitrile mass fraction in testing sample is calculated
Adopt gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph to detect the peak area of azodiisobutyronitrile, substitute into the standard curve equation of the azodiisobutyronitrile that step (1) is tried to achieve, calculate the content of azodiisobutyronitrile in testing sample.
Wherein, the standard specimen process for preparation of different azodiisobutyronitrile content is preferably with dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate or benzene for solvent, and more preferably dimethyl sulfoxide is solvent.
The quantitative analysis method of the low content azodiisobutyronitrile of the present invention, simple to operate, convenience of calculation, analysis accurate quick.
Accompanying drawing explanation
Fig. 1 is the total ion current figure of the dimethyl sulfoxide solution of azodiisobutyronitrile；
Fig. 2 is the bar graph of retention time 19.74min spectral peak；
Fig. 3 is the bar-shaped spectrogram of azodiisobutyronitrile standard；
Fig. 4 is the standard working curve of azodiisobutyronitrile in dimethyl sulfoxide solution.
Detailed description of the invention
Hereinafter embodiments of the invention are elaborated: the present embodiment is carried out under premised on technical solution of the present invention; give detailed embodiment and process; but protection scope of the present invention is not limited to following embodiment; the experimental technique of unreceipted actual conditions in the following example, generally conventionally condition.
Standard specimen preparation solvent:
In the present invention, standard specimen is prepared solvent be not particularly limited, the standard specimen process for preparation being typically different azodiisobutyronitrile content is with dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate or benzene for solvent, preferably with dimethyl sulfoxide for solvent, selection dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate or the benefit that benzene is solvent are that boiling point is low, and dissolubility is good.
Embodiment 1
Experimental principle
Azodiisobutyronitrile is dissolved in dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate, benzene equal solvent, and dissolubility is relatively low, and its decomposition temperature is 64 DEG C.When entering gas chromatograph-mass spectrometer (GC-MS) or gas chromatograph when the azodiisobutyronitrile dissolved, owing to the temperature of injection port is higher, azodiisobutyronitrile is decomposed, the spectrogram of gas chromatograph-mass spectrometer (GC-MS) can prove that azodiisobutyronitrile is decomposed into isopropyl cyanide free radical and nitrogen, the concentration of 2mol isopropyl cyanide free radical is equivalent to the concentration of 1mol azodiisobutyronitrile, and the peak area of isobutyl group free radical is proportional with concentration.
Key instrument and reagent
Gas chromatograph-mass spectrometer (GC-MS)；
Gas chromatograph；
Azodiisobutyronitrile；
Dimethyl sulfoxide.
Experimental technique
1, the preparation of different content azodiisobutyronitrile standard specimen
Preparation about contains the dimethyl sulfoxide solution of 0.001%, 0.01%, 1.0%, 5%, 10% azodiisobutyronitrile, the mass fraction of the azodiisobutyronitrile recorded respectively 0.002%, 0.005%, 0.998%, 4.99% and 9.95%, owing to azodiisobutyronitrile dissolubility in dimethyl sulfoxide is relatively low, therefore mass fraction be 4.99% and 9.95% standard specimen need to 50 DEG C of heating be completely dissolved to azodiisobutyronitrile.
Accompanying drawing 1 is the total ion current figure of the dimethyl sulfoxide solution of azodiisobutyronitrile, accompanying drawing 2 is bar graph that retention time is 19.74min spectral peak, compareed by the bar-shaped spectrogram of azodiisobutyronitrile standard with accompanying drawing 3, it was demonstrated that retention time is 19.74min spectral peak is azodiisobutyronitrile.
2, the determination step of standard specimen
Above-mentioned standard specimen is carried out gas chromatographic analysis, column temperature: 70 DEG C keep 10min, with 10 DEG C of min-1Programming rate be raised to 260 DEG C and keep 20min, each sample test twice, record sample peak area.
The table 1 standard specimen peak area containing different azodiisobutyronitrile mass fractions
| Mass fraction (%) | 0.002 | 0.005 | 0.998 | 4.99 | 9.95 |
| Peak area | 24.82309 | 56.68352 | 724.29321 | 3430.08521 | 7073.48145 |
| Peak area | 22.65413 | 54.68471 | 693.73096 | 3790.67622 | 7095.10693 |
| Meansigma methods | 23.7368 | 55.6841 | 709.0121 | 3610.4807 | 7084.2942 |
3, the drafting of azodiisobutyronitrile standard curve
With the mass fraction of azodiisobutyronitrile for abscissa, with the peak area meansigma methods of azodiisobutyronitrile for vertical coordinate, drawing standard working curve.
4, the accuracy of method
The mass fraction of azodiisobutyronitrile this law recorded, the mass fraction of the azodiisobutyronitrile recorded with liquid chromatograph (in patent CN101915844A introduce method) compares, and its result relative error, less than 10%, refers to table 3.
Table 3 accuracy is tested
| Sequence number | Azodiisobutyronitrile mass fraction/% | Azodiisobutyronitrile mass fraction/% (LC) | Relative error/% |
| 1 | 0.0062 | 0.0064 | 3.2 |
| 2 | 0.011 | 0.012 | 8.3 |
5, the precision of method
Under selected experiment condition, same sample carrying out 6 times and measures, its relative standard deviation is 3.3%, refers to table 4.
Table 4 Precision Experiment
| Mass fraction/the % of measurement result | Meansigma methods/% | Standard deviation/% | Relative standard deviation/% |
| 0.062,0.065,0.063,0.065,0.066,0.069 | 0.06 | 0.002 | 3.3 |
Embodiment 2
Experimental principle
Azodiisobutyronitrile is dissolved in dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate, benzene equal solvent, and dissolubility is relatively low, and its decomposition temperature is 64 DEG C.When entering gas chromatograph-mass spectrometer (GC-MS) or gas chromatograph when the azodiisobutyronitrile dissolved, owing to the temperature of injection port is higher, azodiisobutyronitrile is decomposed, the spectrogram of gas chromatograph-mass spectrometer (GC-MS) can prove that azodiisobutyronitrile is decomposed into isopropyl cyanide free radical and nitrogen, the concentration of 2mol isopropyl cyanide free radical is equivalent to the concentration of 1mol azodiisobutyronitrile, and the peak area of isobutyl group free radical is proportional with concentration.
Key instrument and reagent
Gas chromatograph-mass spectrometer (GC-MS)；
Gas chromatograph；
Azodiisobutyronitrile；
Absolute methanol.
Experimental technique
1, the preparation of different content azodiisobutyronitrile standard specimen
Preparation about contains the dimethyl sulfoxide solution of 0.005%, 0.03%, 2.0%, 4.0%, 10.0% azodiisobutyronitrile, the mass fraction of the azodiisobutyronitrile recorded respectively 0.003%, 0.015%, 2.6%, 4.9% and 8.6%, owing to azodiisobutyronitrile dissolubility in dimethyl sulfoxide is relatively low, therefore mass fraction be 4.9% and 8.6% standard specimen need to 50 DEG C of heating be completely dissolved to azodiisobutyronitrile.
2, the determination step of standard specimen
Above-mentioned standard specimen is carried out gas chromatographic analysis, column temperature: 60 DEG C keep 10min, with 10 DEG C of min-1Programming rate be raised to 200 DEG C and keep 20min, each sample test twice, record sample peak area.
3, the drafting of azodiisobutyronitrile standard curve
With the mass fraction of azodiisobutyronitrile for abscissa, with the peak area meansigma methods of azodiisobutyronitrile for vertical coordinate, drawing standard working curve.
4, the accuracy of method
The mass fraction of azodiisobutyronitrile this law recorded, the mass fraction of the azodiisobutyronitrile recorded with liquid chromatograph (in patent CN101915844A introduce method) compares, and its result relative error is less than 10%.
5, the precision of method
Under selected experiment condition, same sample carrying out 6 times and measures, its relative standard deviation is 6.8%.
Embodiment 3
Experimental principle
Azodiisobutyronitrile is dissolved in dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate, benzene equal solvent, and dissolubility is relatively low, and its decomposition temperature is 64 DEG C.When entering gas chromatograph-mass spectrometer (GC-MS) or gas chromatograph when the azodiisobutyronitrile dissolved, owing to the temperature of injection port is higher, azodiisobutyronitrile is decomposed, the spectrogram of gas chromatograph-mass spectrometer (GC-MS) can prove that azodiisobutyronitrile is decomposed into isopropyl cyanide free radical and nitrogen, the concentration of 2mol isopropyl cyanide free radical is equivalent to the concentration of 1mol azodiisobutyronitrile, and the peak area of isobutyl group free radical is proportional with concentration.
Key instrument and reagent
Gas chromatograph-mass spectrometer (GC-MS)；
Gas chromatograph；
Azodiisobutyronitrile；
Dehydrated alcohol.
Experimental technique
1, the preparation of different content azodiisobutyronitrile standard specimen
Preparation about contains the dimethyl sulfoxide solution of 0.002%, 0.05%, 3.0%, 6.0%, 9.0% azodiisobutyronitrile, the mass fraction of the azodiisobutyronitrile recorded respectively 0.004%, 0.03%, 2.8%, 5.8% and 8.6%, owing to azodiisobutyronitrile dissolubility in dimethyl sulfoxide is relatively low, therefore mass fraction be 5.8% and 8.6% standard specimen need to 50 DEG C of heating be completely dissolved to azodiisobutyronitrile.
2, the determination step of standard specimen
Above-mentioned standard specimen is carried out gas chromatographic analysis, column temperature: 70 DEG C keep 10min, with 10 DEG C of min-1Programming rate be raised to 220 DEG C and keep 20min, each sample test twice, record sample peak area.
3, the drafting of azodiisobutyronitrile standard curve
With the mass fraction of azodiisobutyronitrile for abscissa, with the peak area meansigma methods of azodiisobutyronitrile for vertical coordinate, drawing standard working curve.
4, the accuracy of method
The mass fraction of azodiisobutyronitrile this law recorded, the mass fraction of the azodiisobutyronitrile recorded with liquid chromatograph (in patent CN101915844A introduce method) compares, and its result relative error is less than 9%.
5, the precision of method
Under selected experiment condition, same sample carrying out 6 times and measures, its relative standard deviation is 9.8%.
Claims (3)
1. the quantitative analysis method of a low content azodiisobutyronitrile, it is characterised in that:
(1) Specification Curve of Increasing of azodiisobutyronitrile
The standard specimen of the different azodiisobutyronitrile content of preparation, adopt gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph, with the peak area of azodiisobutyronitrile for vertical coordinate, with azodiisobutyronitrile content for abscissa, it is depicted as the standard curve of azodiisobutyronitrile, tries to achieve standard curve equation；
(2) the azodiisobutyronitrile mass fraction in testing sample is calculated
Adopt gas chromatograph-mass spectrometer (GC-MS) and gas chromatograph to detect the peak area of azodiisobutyronitrile, substitute into the standard curve equation of the azodiisobutyronitrile that step (1) is tried to achieve, calculate the content of azodiisobutyronitrile in testing sample.
2. the quantitative analysis method of low content azodiisobutyronitrile according to claim 1, it is characterized in that, the standard specimen process for preparation of different azodiisobutyronitrile content is with dimethyl sulfoxide, ether, methanol, ethanol, propanol chloroform, dichloroethanes, ethyl acetate or benzene for solvent.
3. the quantitative analysis method of low content azodiisobutyronitrile according to claim 2, it is characterised in that the standard specimen process for preparation of different azodiisobutyronitrile content is with dimethyl sulfoxide for solvent.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956810A (en) * | 2018-06-05 | 2018-12-07 | 中国电力科学研究院有限公司 | The detection method of perfluor isobutyronitrile purity in perfluor isobutyronitrile mixed gas |
| 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 |
| CN110954647A (en) * | 2018-09-26 | 2020-04-03 | 武汉武药科技有限公司 | Sample treatment method for measuring total nitrogen content in polyvinyl alcohol and method for measuring total nitrogen content in polyvinyl alcohol |
| CN111505166A (en) * | 2020-05-29 | 2020-08-07 | 山东省食品药品检验研究院 | Method for determining azodiisoheptonitrile in olmesartan medoxomil |
| CN114199667A (en) * | 2021-12-13 | 2022-03-18 | 山西钢科碳材料有限公司 | Pretreatment method of azobisisobutyronitrile and determination method of trace element content |
| CN114544784A (en) * | 2020-11-26 | 2022-05-27 | 珠海润都制药股份有限公司 | Method for detecting azodiisobutyronitrile in voriconazole M3 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956810A (en) * | 2018-06-05 | 2018-12-07 | 中国电力科学研究院有限公司 | The detection method of perfluor isobutyronitrile purity in perfluor isobutyronitrile mixed gas |
| CN108956810B (en) * | 2018-06-05 | 2022-04-12 | 中国电力科学研究院有限公司 | Method for detecting purity of perfluoroisobutyronitrile in perfluoroisobutyronitrile mixed gas |
| CN110954647A (en) * | 2018-09-26 | 2020-04-03 | 武汉武药科技有限公司 | Sample treatment method for measuring total nitrogen content in polyvinyl alcohol and method for measuring total nitrogen content in polyvinyl alcohol |
| 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 |
| CN111505166A (en) * | 2020-05-29 | 2020-08-07 | 山东省食品药品检验研究院 | Method for determining azodiisoheptonitrile in olmesartan medoxomil |
| CN114544784A (en) * | 2020-11-26 | 2022-05-27 | 珠海润都制药股份有限公司 | Method for detecting azodiisobutyronitrile in voriconazole M3 |
| CN114199667A (en) * | 2021-12-13 | 2022-03-18 | 山西钢科碳材料有限公司 | Pretreatment method of azobisisobutyronitrile and determination method of trace element content |
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