CN103674879A - Quick determination method of structural composition of polypropylene glycol ethylene oxide adduct - Google Patents
Quick determination method of structural composition of polypropylene glycol ethylene oxide adduct Download PDFInfo
- Publication number
- CN103674879A CN103674879A CN201310717812.3A CN201310717812A CN103674879A CN 103674879 A CN103674879 A CN 103674879A CN 201310717812 A CN201310717812 A CN 201310717812A CN 103674879 A CN103674879 A CN 103674879A
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- China
- Prior art keywords
- ethylene oxide
- mass percentage
- polypropylene glycol
- oxide adduct
- percentage content
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Links
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229920001451 polypropylene glycol Polymers 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 19
- 239000000203 mixture Substances 0.000 title abstract description 3
- 238000012360 testing method Methods 0.000 claims description 26
- 238000003556 assay Methods 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 8
- 230000005477 standard model Effects 0.000 claims description 8
- 238000002835 absorbance Methods 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000002329 infrared spectrum Methods 0.000 abstract description 2
- 238000000862 absorption spectrum Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- -1 polyoxyethylene Polymers 0.000 description 11
- 229940117927 ethylene oxide Drugs 0.000 description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002736 nonionic surfactant Substances 0.000 description 5
- 238000005481 NMR spectroscopy Methods 0.000 description 4
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a quick determination method of structural composition of a polypropylene glycol ethylene oxide adduct. The method comprises the steps of determining infrared absorbance spectrum of a sample to be determined, based on a wave trough position within the wavelength interval of 1450-1400cm<-1>, reading peak heights of wave peaks within the wavelength intervals of 1380-1370cm<-1> and 1350-1340cm<-1> relative to the baseline, recording as X1 and X2, calculating to obtain a peak height ratio X2/X1, determining standard samples with different ethylene oxide mass percentage contents, and establishing a standard working curve, and calculating to obtain an ethylene oxide mass percentage content by bringing X2/X1 of the sample to be determined into the standard working curve. Compared with the traditional determination method, the method employs the fourier infrared spectrum, the equipment input cost is low, an establishment and detection process of the method is simpler, the requirement on an operator is lower, the ethylene oxide mass percentage content information can be obtained within 3-5min, the requirement of rapid analysis is met, and the method is easy to popularize in the industrial production.
Description
Technical field
The present invention relates to the rapid assay methods that a kind of polypropylene glycol ethylene oxide adduct structure forms.
Background technology
The ethylene oxide adduct of polypropylene glycol (polyether nonionic surfactant) is by polyaddition reaction, to generate polypropylene glycol by epoxypropane, and it is that relative molecular mass is 1000-15000 compound.Due to the spatial obstacle of methyl in molecule, it water-soluble very little and be applicable to doing the lipophilic group raw material of surfactant.When polypropylene glycol forms the multipolymer high molecular surfactant of polyoxyethylene, the embedding of polyoxypropylene phase during with ethyleneoxide addition or with oxirane and epoxypropane copolymerization, this series products is called polyether nonionic surfactant, and general formula is RO (C
3h
60) m (C
2h
4o) nH.
Polyether nonionic surfactant just has the ability of reduction interfacial tension can make the emulsifying agent of w/o type and O/W type emulsion fluid when very low concentrations, and calcium soap in hard water is had peptizaiton and has good solubilization, the defoamer done having, foam inhibitor.Polyether nonionic surfactant has odorless, nontoxic, non-irritating feature, and it is a kind of novel non-ionic surfactant that chemical reagent is had to good stability.
The large I of the lipophilicity of this type of surfactant (hydrophobicity), water wettability and defoaming is by regulating the ratio of polyoxyethylene and polyoxypropylene to be controlled.Different proportion and different polymerization methods obtain the surfactant of various different performances.Simple and direct, to measure quickly and accurately polyoxyethylene and polyoxypropylene ratio, it is one of controlling of production process key parameter, being requisite internal control index in product inspection, is also that the good copolymer material of industrial large-scale production plant long-period stable operation and production department is necessary.
The method of the existing ratio about analysis polyoxyethylene and polyoxypropylene comprises:
1. substance assistant laser desorpted ionized mass spectrum
2. high performance liquid chromatography
3.
1h-nuclear magnetic resonance
4.
13c-nuclear magnetic resonance
Above-mentioned these method running programs are complicated, do not reach the requirement of express-analysis, are difficult to universal in suitability for industrialized production.High performance liquid chromatography is because the bad test error that causes of degree of separation performance is greatly also seldom used.Nmr sensitivity and resolution are high, structure and composition with nuclear magnetic resonance research polyoxyethylene and polyoxypropylene, quantitative test multipolymer ethoxy alkene content exactly, just because nuclear magnetic resonance apparatus is expensive, analytical instrument complicated operation, analytical cycle is long, the requirement in the large production of inadaptable industry.
Summary of the invention
Object of the present invention, the rapid assay methods that provides exactly a kind of polypropylene glycol ethylene oxide adduct structure to form in order to address the above problem.
The object of the present invention is achieved like this:
The rapid assay methods that a kind of polypropylene glycol ethylene oxide adduct structure of the present invention forms, is characterized in that, comprises the following steps:
(1) measure the infrared absorbency spectrum of testing sample, with range of wavelengths 1450-1400cm
-1wave trough position in scope is baseline, reads range of wavelengths 1380-1370cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
1, then read range of wavelengths 1350-1340cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
2, calculate ratio of peak X
2/ X
1;
(2) oxirane mass percentage content is respectively to 10%, 20%, 30%, 40% and 50% standard model carries out the mensuration identical with step (1), with ratio of peak X
2/ X
1for horizontal ordinate, oxirane mass percentage content is ordinate, Criterion working curve;
(3) ratio of peak X step (1) being recorded
2/ X
1, bring the standard working curve that step (2) is set up into, try to achieve the mass percentage content of oxirane in testing sample.
The rapid assay methods that above-mentioned a kind of polypropylene glycol ethylene oxide adduct structure forms, wherein, while measuring the infrared absorbency spectrum of testing sample and standard model, first at range of wavelengths 4000-600cm
-1the air of usining in scope carries out background scans as background.
The rapid assay methods that above-mentioned a kind of polypropylene glycol ethylene oxide adduct structure forms, wherein, during the infrared absorbency spectrum of mensuration testing sample and standard model, scanning times is 32 times, resolution is 4cm
-1, spectral scan scope 4000-600cm
-1, absorbance data form is log1/R, environment temperature is 25 ± 5 ℃, ambient humidity: RH≤60%.
Compare with traditional assay method, the inventive method adopts Fourier's infrared spectrum, equipment investment cost is low, method foundation and testing process are simpler, requirement to operating personnel is lower, within 3～5 minutes, can obtain oxirane mass percentage content information, reach the requirement of express-analysis, be easy in suitability for industrialized production universal.
Accompanying drawing explanation
Fig. 1 is range of wavelengths 1600-1200cm on the infrared absorbency spectrogram of testing sample
-1local spectrum.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
One, testing tool:
U.S. Thermo Fisher iS10 type Fourier infrared spectrograph
Resolution 4.0cm
-1
Scanning times: 32 times
Two, test condition:
Test environment temperature: 25 ± 5 ℃
Test environment humidity: RH≤60%
Three, testing procedure:
1) before test, whether temperature, the humidity of checkout environment meets the requirements, and under the temperature of stipulating, humidity, operate.
2), after FTIR infrared spectrometer start, whether inspection apparatus resolution, energy is up to standard.
3) at 4000cm
-1to 600cm
-1scope in using air and carry out background scans as background.
4) testing sample of multipolymer is coated on the atr crystal of Fourier infrared spectrograph equably, measures transmissivity infrared spectrogram, spectral scan scope 4000-600cm
-1, test rear deposit.
Four, testing sample test result and calculating:
(1) by the machine processing as calculated of gained multipolymer transmissivity infrared spectrogram, convert infrared absorbency spectrogram (absorbance data form is log1/R) to.
(2) on infrared absorbency spectrogram, utilize computing machine to amplify range of wavelengths 1600-1200cm
-1local spectrum (as shown in Figure 1).With range of wavelengths 1450-1400cm
-1wave trough position in scope is baseline, reads range of wavelengths 1380-1370cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
1, then read range of wavelengths 1350-1340cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
2, calculate ratio of peak X
2/ X
1.
Five, Criterion working curve:
The polypropylene glycol ethylene oxide adduct that employing BASF provides is as standard model, and wherein oxirane mass percentage content is respectively 10%, 20%, and 30%, 40% and 50%.
Standard model is measured according to the method for (2) step in above-mentioned " testing sample test result and calculating " step, with ratio of peak X
2/ X
1for horizontal ordinate, oxirane mass percentage content is ordinate, Criterion working curve, and this standard working curve is Y=172.32X-76.354(R
2=0.996).
Six, the calculating of the mass percentage content of oxirane in testing sample
By the ratio of peak X calculating in " testing sample test result and calculating " step
2/ X
1bring in standard working curve formula Y=172.32X-76.354, try to achieve the mass percentage content of oxirane in testing sample.
Six, this method relative error range
The polypropylene glycol ethylene oxide adduct of known oxirane mass percentage content is carried out to the mensuration of oxirane mass percentage content by this method, measurement result is as follows:
| X 2/X 1 | EO%(actual value) | EO%(measured value) | Absolute error | Relative error |
| 0.497 | 10 | 9.3 | -0.7 | 7.1% |
| 0.560 | 20 | 20.1 | 0.1 | 0.7% |
| 0.627 | 30 | 31.7 | 1.7 | 5.6% |
| 0.672 | 40 | 39.4 | -0.6 | 1.4% |
| 0.730 | 50 | 49.4 | -0.6 | 1.1% |
Wherein, EO% represents oxirane mass percentage content;
Absolute error=measured value-actual value (represents analysis result, "+": more higher than actual value positive and negative number; "-": more on the low side than actual value);
Relative error=| absolute error |/actual value * 100%.
As seen from the above table, the relative error range of the inventive method to be less than the measurement range of 10%(oxirane mass percentage content be 0-50%).
Above embodiment is used for illustrative purposes only, but not limitation of the present invention, person skilled in the relevant technique, without departing from the spirit and scope of the present invention, can also make various conversion or modification, therefore all technical schemes that are equal to also should belong to category of the present invention, should be limited by each claim.
Claims (3)
1. the rapid assay methods that polypropylene glycol ethylene oxide adduct structure forms, is characterized in that, comprises the following steps:
(1) measure the infrared absorbency spectrum of testing sample, with range of wavelengths 1450-1400cm
-1wave trough position in scope is baseline, reads range of wavelengths 1380-1370cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
1, then read range of wavelengths 1350-1340cm
-1crest in scope is with respect to the peak height of baseline and be designated as X
2, calculate ratio of peak X
2/ X
1;
(2) oxirane mass percentage content is respectively to 10%, 20%, 30%, 40% and 50% standard model carries out the mensuration identical with step (1), with ratio of peak X
2/ X
1for horizontal ordinate, oxirane mass percentage content is ordinate, Criterion working curve;
(3) ratio of peak X step (1) being recorded
2/ X
1, bring the standard working curve that step (2) is set up into, try to achieve the mass percentage content of oxirane in testing sample.
2. the rapid assay methods that a kind of polypropylene glycol ethylene oxide adduct structure as claimed in claim 1 forms, is characterized in that, while measuring the infrared absorbency spectrum of testing sample and standard model, first at range of wavelengths 4000-600cm
-1the air of usining in scope carries out background scans as background.
3. the rapid assay methods that a kind of polypropylene glycol ethylene oxide adduct structure as claimed in claim 1 forms, is characterized in that, while measuring the infrared absorbency spectrum of testing sample and standard model, scanning times is 32 times, and resolution is 4cm
-1, spectral scan scope 4000-600cm
-1, absorbance data form is log1/R, environment temperature is 25 ± 5 ℃, ambient humidity: RH≤60%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310717812.3A CN103674879A (en) | 2013-12-23 | 2013-12-23 | Quick determination method of structural composition of polypropylene glycol ethylene oxide adduct |
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|---|---|---|---|
| CN201310717812.3A CN103674879A (en) | 2013-12-23 | 2013-12-23 | Quick determination method of structural composition of polypropylene glycol ethylene oxide adduct |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2573172C1 (en) * | 2014-11-07 | 2016-01-20 | Общество с ограниченной ответственностью "Научно-исследовательский институт природных газов и газовых технологий - Газпром ВНИИГАЗ" | Method for detection of ethyleneglycol in water solutions |
| CN111398209A (en) * | 2020-05-04 | 2020-07-10 | 中钢集团郑州金属制品研究院有限公司 | Infrared spectrum method for measuring polyvinyl chloride content in hard polyvinyl chloride pipe |
| CN116242805A (en) * | 2023-02-03 | 2023-06-09 | 温州泛波激光有限公司 | Laser detection method, laser detection device, and computer storage medium |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102262055A (en) * | 2011-01-29 | 2011-11-30 | 重庆大学 | Method for measuring residual quantity of acrylamide monomer in polyacrylamide substances |
| CN102393378A (en) * | 2011-11-01 | 2012-03-28 | 湖南省湘维有限公司 | Method for rapidly detecting alcoholysis degree and polymerization degree in production of polyvinyl alcohol by utilizing near infrared spectrum technology |
-
2013
- 2013-12-23 CN CN201310717812.3A patent/CN103674879A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102262055A (en) * | 2011-01-29 | 2011-11-30 | 重庆大学 | Method for measuring residual quantity of acrylamide monomer in polyacrylamide substances |
| CN102393378A (en) * | 2011-11-01 | 2012-03-28 | 湖南省湘维有限公司 | Method for rapidly detecting alcoholysis degree and polymerization degree in production of polyvinyl alcohol by utilizing near infrared spectrum technology |
Non-Patent Citations (2)
| Title |
|---|
| 庞宝才 等: "PO_EO_嵌段共聚物的合成与光谱分析", 《精细石油化工》 * |
| 张履芳 等: "聚氛乙烯型非离子表面活性剂的红外光谱定性及氧乙烯数的分析", 《分析化学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2573172C1 (en) * | 2014-11-07 | 2016-01-20 | Общество с ограниченной ответственностью "Научно-исследовательский институт природных газов и газовых технологий - Газпром ВНИИГАЗ" | Method for detection of ethyleneglycol in water solutions |
| CN111398209A (en) * | 2020-05-04 | 2020-07-10 | 中钢集团郑州金属制品研究院有限公司 | Infrared spectrum method for measuring polyvinyl chloride content in hard polyvinyl chloride pipe |
| CN116242805A (en) * | 2023-02-03 | 2023-06-09 | 温州泛波激光有限公司 | Laser detection method, laser detection device, and computer storage medium |
| CN116242805B (en) * | 2023-02-03 | 2024-01-23 | 温州泛波激光有限公司 | Laser detection method, laser detection device, and computer storage medium |
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Application publication date: 20140326 |