CN105784630A - Silicone-rubber rubber-content detecting method based on infrared spectroscopic analysis method - Google Patents
Silicone-rubber rubber-content detecting method based on infrared spectroscopic analysis method Download PDFInfo
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- CN105784630A CN105784630A CN201610114577.4A CN201610114577A CN105784630A CN 105784630 A CN105784630 A CN 105784630A CN 201610114577 A CN201610114577 A CN 201610114577A CN 105784630 A CN105784630 A CN 105784630A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 85
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000012844 infrared spectroscopy analysis Methods 0.000 title abstract 2
- 238000010521 absorption reaction Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims description 62
- 238000002329 infrared spectrum Methods 0.000 claims description 42
- 238000004458 analytical method Methods 0.000 claims description 41
- 238000001514 detection method Methods 0.000 claims description 31
- 238000001179 sorption measurement Methods 0.000 claims description 19
- 229920000260 silastic Polymers 0.000 claims description 14
- 238000001228 spectrum Methods 0.000 claims description 12
- 230000002238 attenuated effect Effects 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 4
- 238000005297 material degradation process Methods 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 abstract description 5
- 238000004566 IR spectroscopy Methods 0.000 abstract 3
- 238000000862 absorption spectrum Methods 0.000 abstract 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- XFBXDGLHUSUNMG-UHFFFAOYSA-N alumane;hydrate Chemical compound O.[AlH3] XFBXDGLHUSUNMG-UHFFFAOYSA-N 0.000 description 5
- -1 polydimethylsiloxane Polymers 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 2
- 238000000611 regression analysis Methods 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- 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)
Abstract
The invention discloses a silicone-rubber rubber-content detecting method based on an infrared spectroscopic analysis method.The silicone-rubber rubber-content detecting method is characterized by including the following steps that a, an infrared spectroscopy absorption spectrum of a silicon rubber sample is detected; b, the absorption peak value at the specific absorption wave number position of the detected infrared spectroscopy absorption spectrum of the silicon rubber sample is measured; c, the rubber content of the silicon rubber sample is calculated based on the absorption peak value at the specific absorption wave number position of the detected infrared spectroscopy absorption spectrum of the silicon rubber sample.The result can be used for judging the aging degree and the running state of silicon rubber materials, and the silicone-rubber rubber-content detecting method has the advantages of being reliable, accurate, portable and nondestructive.
Description
Technical field
The present invention relates to a kind of silicone rubber glue detection method of content based on infrared spectrum analysis.
Background technology
Silastic material is the insulant being widely used in network system, and the device and products being made up of silastic material includes but not limited to composite insulator, antifouling flush paint, cable termination adnexa etc..But silicone rubber is a kind of high-molecular organic material, is easily subject to the effect of external environment stress and occurs aging in long-term operation.High-temperature silicon disulfide rubber is the most widely used insulant in power system.Some high-temperature silicon disulfide rubber insulant are not good due to the raw material used or technological level, cause that the ageing-resistant performance of material itself is poor.The topmost composition of silicone rubber is polydimethylsiloxane and white carbon, filling aluminium hydrate, and the ratio of filler is very big to the performance impact of silicone rubber.Too high proportion of filler can cause that silastic material hydrophobicity, migration of hydrophobicity are poor, and mechanical strength is low, ageing-resistant performance is poor.Therefore, the runnability tool for judging silastic material that measures of glue content plays a very important role.
Summary of the invention
Present invention is primarily targeted at for the deficiencies in the prior art, it is provided that a kind of silicone rubber glue detection method of content based on infrared spectrum analysis, reliably, accurately, conveniently, nondestructively measure silicone rubber glue content.
For achieving the above object, the present invention is by the following technical solutions:
A kind of silicone rubber glue detection method of content based on infrared spectrum analysis, it is characterised in that comprise the following steps:
A. the Infrared spectra adsorption collection of illustrative plates of silicone rubber sample is detected；
B. for detecting the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample obtained, its absworption peak peak value in specific absorption beam location is measured；
C. based on the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample absworption peak peak value in specific absorption beam location, the glue content of silicone rubber sample is calculated.
Further:
In step a, adopt attenuated total reflectance-ftir analysis method that silicone rubber sample is detected, to its Infrared spectra adsorption collection of illustrative plates.
Described specific absorption beam location is at (792 ± 5) cm in Infrared spectra adsorption collection of illustrative plates-1(1018 ± 5) cm-1The absworption peak peak value at wave number place.
Described specific absorption beam location is at 792cm in Infrared spectra adsorption collection of illustrative plates-1And 1018cm-1The absworption peak peak value at wave number place.
In step c, at the absworption peak peak value of specific absorption beam location measured place described in two places, following linear equation in two unknowns will be substituted into:
Glue content=3.1050 × I1-2.0415 × I2+0.34627
Wherein, I1And I2Represent absworption peak peak value silicone rubber sample carried out after ftir analysis in its infared spectrum at the first wave number place and the second wave number place respectively.
Described method uses hand-held ftir analysis equipment.
A kind of silastic material degradation detecting method, including:
The silicone rubber glue detection method of content based on infrared spectrum analysis as described in any one of claim 1 to 6 is used to detect silicone rubber glue content；
Silicone rubber glue content according to detection judges the degree of aging of silastic material.
A kind of network system insulant method for testing performance, described insulant includes silicone rubber, including the step using the described silicone rubber glue detection method of content based on infrared spectrum analysis to detect silicone rubber glue content.
A kind of silicone rubber glue content detection system, adopts the described silicone rubber glue detection method of content based on infrared spectrum analysis that silicone rubber glue content is detected.
Described system includes hand-held ftir analysis equipment.
Beneficial effects of the present invention:
The present invention proposes a kind of silicone rubber glue detection method of content based on infrared spectrum analysis, it is without being sampled silastic material, hand-held ftir analysis equipment is utilized can material to be analyzed, and then calculate glue content and the inorganic filler content of silastic material, this result may be used for judging degree of aging and the running status of silastic material have reliable, accurate, portable, lossless feature.
Accompanying drawing explanation
Fig. 1 is the typical silicone rubber sample infared spectrum detected in the embodiment of the present invention；
Fig. 2 is the silicone rubber sample infared spectrum that instantiation of the present invention obtains.
Detailed description of the invention
Hereinafter embodiments of the present invention are elaborated.It is emphasized that the description below is merely exemplary, rather than in order to limit the scope of the present invention and application thereof.
In one embodiment, a kind of silicone rubber glue detection method of content based on infrared spectrum analysis, it is characterised in that comprise the following steps:
A. the Infrared spectra adsorption collection of illustrative plates of silicone rubber sample is detected；
B. for detecting the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample obtained, its absworption peak peak value in specific absorption beam location is measured；
C. based on the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample absworption peak peak value in specific absorption beam location, the glue content of silicone rubber sample is calculated.
Further:
In step a, adopt attenuated total reflectance-ftir analysis method that silicone rubber sample is detected, to its Infrared spectra adsorption collection of illustrative plates, consult Fig. 1.
Described specific absorption beam location is at (792 ± 5) cm in Infrared spectra adsorption collection of illustrative plates-1(1018 ± 5) cm-1The absworption peak peak value at wave number place.
Described specific absorption beam location is at 792cm in Infrared spectra adsorption collection of illustrative plates-1And 1018cm-1The absworption peak peak value at wave number place.
In step c, at the absworption peak peak value of specific absorption beam location measured place described in two places, following linear equation in two unknowns will be substituted into:
Glue content=3.1050 × I1-2.0415 × I2+0.34627
Wherein, I1And I2Represent absworption peak peak value silicone rubber sample carried out after ftir analysis in its infared spectrum at the first wave number place and the second wave number place respectively.
Find based on ir data analysis, (792 ± 5) cm-1Locate especially 792cm-1The absworption peak at place represents the Si-C key absworption peak in siloxanes, (1018 ± 5) cm-1Locate especially 1018cm-1Absworption peak represent Si-O key absworption peak, filling aluminium hydrate composition is also presented simultaneously, therefore it is considered herein that (792 ± 5) cm-1Place represents the organic principle in silicone rubber, i.e. " glue content ", and (1018 ± 5) cm-1Place represents the inorganic constituents in silicone rubber, i.e. " filer content ".Stepwise regression analysis method is utilized to find, calculate the above-mentioned linear equation in two unknowns of glue content, namely the above-mentioned formula that the two wave number and the determined coefficient of the embodiment of the present invention are constituted, being the actual parameter meeting all tested samples most, the glue content calculated by formula has good accuracy.
3 coefficients in above-mentioned linear equation in two unknowns, are on the basis obtaining lot of experimental data, utilize multiple linear regression model to obtain in a preferred embodiment.Typically, choosing 12 high-temperature silicon disulfide rubber samples, its glue content is known.Utilizing attenuated total reflectance-ftir analysis method to obtain its infrared spectrum, then measure the absorption peak of its spectrum wave number everywhere, each sample spectra obtains 10 absworption peaks altogether.With these 10 absworption peak alternately independent variables, glue content, as dependent variable, carries out stepwise regression analysis.Final superseded wherein 8 absworption peaks, only retain 2 independent variables as final formula, and this is to utilize progressively to analyze the result of calculation that method obtains, and is absent from manual intervention, and accuracy is good.
Described method uses hand-held ftir analysis equipment.
A kind of silastic material quality determining method, including:
The silicone rubber glue detection method of content based on infrared spectrum analysis such as any one embodiment aforementioned is used to detect silicone rubber glue content；
Silicone rubber glue content according to detection judges the degree of aging of silastic material.
A kind of network system insulant method for testing performance, described insulant includes silicone rubber, detects the step of silicone rubber glue content including the silicone rubber glue detection method of content based on infrared spectrum analysis used such as any one embodiment aforementioned.
A kind of silicone rubber glue content detection system, adopts the silicone rubber glue detection method of content based on infrared spectrum analysis such as any one embodiment aforementioned that silicone rubber glue content is detected.
Described system includes hand-held ftir analysis equipment.
The glue detection method of content of specific embodiment further explained below.
(1) mass fraction that " glue content " is defined as in silastic material polydimethylsiloxane.Glue content is more high, then in silicone rubber, polydimethyl siloxane content is more high, and white carbon, filling aluminium hydrate content are more low；Glue content is more low, then in silicone rubber, polydimethyl siloxane content is more low, and white carbon, filling aluminium hydrate content are more high.
(2) utilize ftir analysis method that silicone rubber sample is measured, obtain its Infrared spectra adsorption collection of illustrative plates, carry out the judgement of silicone rubber glue content followed by the absworption peak peak value under specific wave number.
(3) adopting attenuated total reflectance-ftir analysis method that silicone rubber sample is detected, bulk sample can be carried out infrared spectrum analysis by this detection method, it is not necessary to individually sample preparation, it is adaptable to on-the-spot Non-Destructive Testing.
(4) the silicone rubber sample infared spectrum that detection is obtained, it is necessary to measure, read its absworption peak peak value in specific absorption beam location.According to experiment test, in an advantageous embodiment, for the calculating of polydimethylsiloxane mass fraction in silicone rubber, measure 792cm-1And 1018cm-1The absworption peak peak value of vicinity, then substitutes into following linear equation in two unknowns by value, can calculate and obtain glue content value.
Operating procedure
The calculating process of glue content is as follows:
The equation used is as follows:
Glue content=3.1050 × I792-2.0415×I1018+0.34627(1)
Wherein, I792And I1018Represent respectively and silicone rubber sample is carried out after ftir analysis in its infared spectrum at (792 ± 5) cm-1(1018 ± 5) cm-1The absworption peak peak value at wave number place.The infared spectrum of silicone rubber sample should pass through attenuated total reflectance-ftir analysis method and obtain.Typical silicone rubber sample infared spectrum is as shown in Figure 1.
Calculated examples
For certain high-temperature silicon disulfide rubber sample, its formula is: polydimethylsiloxane 100 parts, filling aluminium hydrate 185 parts, white carbon black filler 35 parts, it is known that its filler gross mass is 100 parts, and therefore glue content is 100/ (220+100)=0.3125.
Utilize attenuated total reflectance-ftir analysis method, obtain its infared spectrum, as shown in Figure 2.
In collection of illustrative plates, I792=0.1593, I1018=0.25649, it is 0.317266 that substitution equation (1) can obtain glue content, and the glue content of actual sample is 0.3125, and the calculating error of equation is:
Above content is to combine concrete/preferred embodiment further description made for the present invention, it is impossible to assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; these embodiments having described that can also be made some replacements or modification by it, and these substitute or variant all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. the silicone rubber glue detection method of content based on infrared spectrum analysis, it is characterised in that comprise the following steps:
A. the Infrared spectra adsorption collection of illustrative plates of silicone rubber sample is detected；
B. for detecting the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample obtained, its absworption peak peak value in specific absorption beam location is measured；
C. based on the Infrared spectra adsorption collection of illustrative plates of the silicone rubber sample absworption peak peak value in specific absorption beam location, the glue content of silicone rubber sample is calculated.
2. as claimed in claim 1 based on the silicone rubber glue detection method of content of infrared spectrum analysis, it is characterized in that, in step a, adopt attenuated total reflectance-ftir analysis method that silicone rubber sample is detected, to its Infrared spectra adsorption collection of illustrative plates.
3. as claimed in claim 1 based on the silicone rubber glue detection method of content of infrared spectrum analysis, it is characterised in that described specific absorption beam location is at (792 ± 5) cm in Infrared spectra adsorption collection of illustrative plates-1(1018 ± 5) cm-1The absworption peak peak value at wave number place.
4. as claimed in claim 1 based on the silicone rubber glue detection method of content of infrared spectrum analysis, it is characterised in that described specific absorption beam location is at 792cm in Infrared spectra adsorption collection of illustrative plates-1And 1018cm-1The absworption peak peak value at wave number place.
5., based on the silicone rubber glue detection method of content of infrared spectrum analysis as described in any one of Claims 1-4, it is characterised in that in step c, at the absworption peak peak value of specific absorption beam location measured place described in two places, following linear equation in two unknowns will be substituted into:
Glue content=3.1050 × I1-2.0415 × I2+0.34627
Wherein, I1And I2Represent absworption peak peak value silicone rubber sample carried out after ftir analysis in its infared spectrum at the first wave number place and the second wave number place respectively.
6. based on the silicone rubber glue detection method of content of infrared spectrum analysis as described in any one of claim 1 to 5, it is characterised in that described method uses hand-held ftir analysis equipment.
7. a silastic material degradation detecting method, it is characterised in that including:
The silicone rubber glue detection method of content based on infrared spectrum analysis as described in any one of claim 1 to 6 is used to detect silicone rubber glue content；
Silicone rubber glue content according to detection judges the degree of aging of silastic material.
8. a network system insulant method for testing performance, described insulant includes silicone rubber, it is characterized in that, detect the step of silicone rubber glue content including the silicone rubber glue detection method of content based on infrared spectrum analysis used as described in any one of claim 1 to 6.
9. a silicone rubber glue content detection system, it is characterised in that adopt the silicone rubber glue detection method of content based on infrared spectrum analysis as described in any one of claim 1 to 5 that silicone rubber glue content is detected.
10. silicone rubber glue content detection system as claimed in claim 9, it is characterised in that include hand-held ftir analysis equipment.
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| CN113777070A (en) * | 2021-09-06 | 2021-12-10 | 江苏神马电力股份有限公司 | Method for evaluating aging degree of silicone rubber through inorganic degree |
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| CN104713844A (en) * | 2015-03-30 | 2015-06-17 | 武汉大学 | Method for evaluating composite insulator silicone rubber aging degree based on Fourier infrared spectroscopy |
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