CN104458487A - Analysis method of wire and cable - Google Patents
Analysis method of wire and cable Download PDFInfo
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- CN104458487A CN104458487A CN201410773575.7A CN201410773575A CN104458487A CN 104458487 A CN104458487 A CN 104458487A CN 201410773575 A CN201410773575 A CN 201410773575A CN 104458487 A CN104458487 A CN 104458487A
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Abstract
The invention relates to an analysis method of a wire and cable. The analysis method comprises the following steps: providing a wire and cable, wherein the wire and cable consists of PE and PVA, thus obtaining a first to-be-tested sample; analyzing the first to-be-tested sample by utilizing TGA to obtain the first VA content; dissolving the first to-be-tested sample by utilizing chloroform, separating PE/EVA, calculating mass of a dissolved matter and a soluble substance, and drying the soluble substance to obtain a second to-be-tested sample; analyzing the second to-be-tested sample by utilizing TGA to obtain second VA content; and calculating the content of EVA in a PEEVA system according to the first VA content and the second VA content.
Description
Technical field
The present invention relates to analysis field, be specifically related to microgram spectral analysis technology, particularly the analytical approach of electric wire.
Background technology
Wire cable insulating and sheath plastics are commonly called as CABLE MATERIALS, which includes the multiple kinds such as rubber, plastics, nylon.CABLE MATERIALS manufacturing enterprise is with cable manufacturing enterprise for user, as long as live wire cabling requirements just has the market of CABLE MATERIALS.Except the bare wire such as steel-cored aluminium strand, electromagnetic wire product, insulation course mouth is nearly all needed in electric wire product.Wherein PE/EVA CABLE MATERIALS is one of more CABLE MATERIALS of domestic application.
In prior art, ethene EVA co-mixing system is good flexibility and a little elasticity just, and wherein the ratio of PE is higher, and tack is poorer.By regulating two kinds of chemical substance ratios, make it meet different application needs, wherein the content of EVA medium vinyl acetate is higher, and its transparency, pliability and toughness can improve relatively.So the determination of EVA content in co-mixing system just seems extremely important.
PE/EVA system is mainly the mechanical blending system of PE and EVA, PE and the EVA key distinction is that PE is formed by the addition polymerization of ethene, the Polymer be formed by connecting by-CH2-the unit repeated, EVA then forms for ethene and vinyl acetate random copolymerization, and ratio is variable between two kinds of components, therefore, by conventional method as infrared, nuclear-magnetism all cannot carry out quantitatively composition each in PE/EVA system.
Summary of the invention
In order to solve the problems of the technologies described above, an object of the present invention is the analytical approach providing a kind of electric wire, comprises the following steps:
The analytical approach of electric wire, comprises the following steps:
There is provided electric wire, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
In described PE/EVA, the content of EVA is lower than 46%.
Described electric wire also comprises pigment and/or filler.
Described filler is one or more in silicon dioxide, titania, calcium carbonate.
Described pigment is inorganic pigment.
Described leachable is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
Described PE/EVA separating step comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
Use method of the present invention can obtain EVA content in PE/EVA effectively and accurately, quantitative deviation all lower than 9%, and the quantitative deviation of conventional separation methods to have height to have low.Visible method of the present invention is more general.
Existing EVA major part VA content distribution is wider, the content of the VA of major part business EVA product is all average content, ooze effect owing to exceeding simultaneously, when EVA content lower than 46% time, all EVA in PE/EVA can not dissolve by chloroform, but EVA can dissolve with identical VA content distribution by chloroform.Adopt the method be separated, quantitative deviation is greater than 25% substantially, adopts method of the present invention, and quantitative deviation is less than 9%.
Embodiment
Leachable of the present invention refers to that chloroform dissolves remaining material after electric wire, and solvend refers to the chloroformic solution obtained after chloroform dissolves electric wire.
The analytical approach of electric wire, comprises the following steps:
The analytical approach of electric wire, comprises the following steps:
There is provided electric wire, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
In described PE/EVA, the content of EVA is lower than 46%.
Described electric wire also comprises pigment and/or filler.
Described filler is one or more in silicon dioxide, titania, calcium carbonate.
Described pigment is inorganic pigment.
Described solvend is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
Described PE/EVA is separated and adopts apparatus,Soxhlet's to be separated.
The separated and dissolved of PE/EVA co-mixing system:
Described PE/EVA separating step comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
According to the different dissolubilities of PE and EVA in chloroform, use chloroform to be separated PE/EVA co-mixing system, concrete operations are as follows:
Get 0.1gPE/EVA blend and send survey TGA, become the flake parcel of 1mm*1mm with filter paper residue electric wire cable cutter, record mixture weight m0.
The filter paper being enclosed with sample is placed in 100ml beaker, add chloroform to 80ml, make chloroform submergence sample, and be placed on 150 degrees Centigrade plates and heat, be transferred in another clean beaker when chloroformic solution in beaker remains about 30ml, and be placed in equally and heating plate dried heavy, and record is equipped with the mass change value m of the beaker of leachable
1, namely first time leachable quality, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records the m of each quality cotton
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.Survey TGA is sent by finally obtaining solvend sampling.
The separated and dissolved of PE/EVA co-mixing system also can adopt apparatus,Soxhlet's 5-10 hour to be separated.
According to the decomposition feature of EVA, it is the process of de-acetic acid at 370 degrees centigrade, and remember that former mixed system send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W1, final solvend send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W2, then, the mass ratio wt(EVA of EVA in PE/EVA) be:
For the co-mixing system containing pigment or filler, method of the present invention is suitable for too.
Specific embodiment:
Raw material sources:
HDPE, LDPE, LLDPE come from Iranian petrochemical complex.
EVA18-3(VA content 18%), EVA14J4(VA content 14%), EVA18J3(VA content 18%), EVA6J2(VA content 6%), EVA4F2(VA content 4.7%), EVA12J4(VA content 12%), EVA9F2(VA content 9%, actual content 7.6%), EVA K3212(VA content 21%) come from Yanshan Petrochemical.
EVA250(VA content 28%), EVA560(VA content 15%) come from E.I.Du Pont Company.
In order to verify the general applicability of the co-mixing system that the inventive method forms for the EVA of variety classes and different VA content, get after beaker weighs PE and EVA according to the scheme of form below, add 60ml toluene heating for dissolving, stir and toluene evaporate to dryness is obtained PE/EVA co-mixing system.
Get 0.1gPE/EVA blend and send survey TGA, become the flake parcel of 1mm*1mm with filter paper residue electric wire cable cutter, record mixture weight m0.
The filter paper being enclosed with sample is placed in 100ml beaker, add chloroform to 80ml, make chloroform submergence sample, and be placed on 150 degrees Centigrade plates and heat, be transferred in another clean beaker when chloroformic solution in beaker remains about 30ml, and be placed in equally and heating plate dried heavy, and record is equipped with the mass change value m of the beaker of leachable
1, namely first time leachable quality, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records the m of each quality cotton
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
Visible, adopting leachable to carry out calculating the quantitative deviation of the mass percent of EVA in PE/EVA system has very large amplitude, does not have versatility.Especially, when EVA content is lower than 46%, its quantitative deviation is larger.
By finally obtain solvend sampling and former state send survey TGA.Remember that former mixed system send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W1, final solvend send the survey de-process of acetic acid weight-loss ratio that TGA obtains to be W2, then, and and the mass ratio wt(EVA of EVA in PE/EVA) be:
The data obtained see the following form:
Use method of the present invention can obtain EVA content in PE/EVA effectively and accurately, quantitative deviation all lower than 9%, and the quantitative deviation of conventional separation methods to have height to have low.Visible method of the present invention is more general.
In existing most of EVA, VA content distribution is wider, the content of the VA of major part business EVA product is all average content, simultaneously present inventor has found that the quantitative deviation of conventional separation methods larger reason of floating there occurs to exceed to ooze effect, when EVA content lower than 46% time, all EVA in PE/EVA can not dissolve by chloroform, but ooze effect because exceed, EVA can dissolve with identical VA content distribution by chloroform.Adopt the method be separated, quantitative deviation is greater than 25% substantially, adopts method of the present invention, and quantitative deviation is less than 9%.
Claims (8)
1. the analytical approach of electric wire, comprises the following steps:
There is provided electric wire, obtain the first testing sample, described first testing sample is made up of PE, EVA;
Use TGA to analyze the first testing sample, obtain a VA content;
Be separated by PE, EVA in first testing sample, solvend obtains the second testing sample after drying;
Use TGA to analyze the second testing sample, obtain the 2nd VA content;
The content of EVA in PEEVA system is obtained by a VA content, the 2nd VA cubage.
2. the analytical approach of electric wire according to claim 1, is characterized in that, in described PE/EVA, the content of EVA is lower than 46%.
3. the analytical approach of electric wire according to claim 1, is characterized in that, described electric wire also comprises pigment and/or filler.
4. the analytical approach of electric wire according to claim 1, is characterized in that, described filler is one or more in silicon dioxide, titania, calcium carbonate.
5. the analytical approach of electric wire according to claim 1, is characterized in that, described pigment is inorganic pigment.
6. the analytical approach of electric wire according to claim 1, is characterized in that, described solvend is through repeatedly chloroform and is dissolved to after double leachable is less than 0.005g and obtains.
7. the analytical approach of electric wire according to claim 1, is characterized in that, described PE/EVA is separated and adopts apparatus,Soxhlet's to be separated.
8. the analytical approach of electric wire according to claim 1, is characterized in that, described PE/EVA separating step comprises:
The filter paper being enclosed with the first testing sample is placed in beaker, add chloroform, make chloroform submergence first testing sample, and be placed on heating plate and heat, by chloroformic solution residue in another clean beaker, and be placed in by sample heating plate dries and weigh, and record is equipped with the mass change value m of the beaker of leachable
1, subsequent operation is with above-mentioned, and each leachable is transferred in same beaker, records each mass change value m
n, until when double leachable quality is all less than or equal to 0.005g, think that PE/EVA system has been separated completely.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410773575.7A CN104458487A (en) | 2014-12-16 | 2014-12-16 | Analysis method of wire and cable |
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| CN201410773575.7A CN104458487A (en) | 2014-12-16 | 2014-12-16 | Analysis method of wire and cable |
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| CN104458487A true CN104458487A (en) | 2015-03-25 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269681A (en) * | 2011-04-30 | 2011-12-07 | 常州天合光能有限公司 | Method for measuring vinyl acetate (VA) content in ethylene vinyl acetate (EVA) |
| EP2442091A1 (en) * | 2010-10-12 | 2012-04-18 | Mettler-Toledo AG | Method and test sample for checking a measuring device for gravimetric humidity calculation |
| CN103207177A (en) * | 2012-01-16 | 2013-07-17 | 阿特斯(中国)投资有限公司 | Test method for content of crosslinking agent in EVA |
| CN103709296A (en) * | 2013-12-30 | 2014-04-09 | 上海微谱化工技术服务有限公司 | Method for extracting pure ethylene-ethylene vinyl-acetate copolymer |
| US20140334515A1 (en) * | 2011-05-26 | 2014-11-13 | Arkema France | Method for characterizing an ethylene and vinyl acetate copolymer |
-
2014
- 2014-12-16 CN CN201410773575.7A patent/CN104458487A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2442091A1 (en) * | 2010-10-12 | 2012-04-18 | Mettler-Toledo AG | Method and test sample for checking a measuring device for gravimetric humidity calculation |
| CN102269681A (en) * | 2011-04-30 | 2011-12-07 | 常州天合光能有限公司 | Method for measuring vinyl acetate (VA) content in ethylene vinyl acetate (EVA) |
| US20140334515A1 (en) * | 2011-05-26 | 2014-11-13 | Arkema France | Method for characterizing an ethylene and vinyl acetate copolymer |
| CN103207177A (en) * | 2012-01-16 | 2013-07-17 | 阿特斯(中国)投资有限公司 | Test method for content of crosslinking agent in EVA |
| CN103709296A (en) * | 2013-12-30 | 2014-04-09 | 上海微谱化工技术服务有限公司 | Method for extracting pure ethylene-ethylene vinyl-acetate copolymer |
Non-Patent Citations (6)
| Title |
|---|
| BIN LI等: ""A Novel Intumescent Flame-Retardant System forFlame-Retarded LLDPE/EVA Composites"", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
| J.A. REYES-LABARTA: ""DSC and TGA study of the transitions involved in the thermal treatmentof binary mixtures of PE and EVA copolymer with a crosslinking agent"", 《POLYMER》 * |
| M. FAKER ET AL.: ""Rheology, morphology and mechanical propertiesof polyethylene/ethylene vinyl acetate copolymer (PE/EVA) blends"", 《EUROPEAN POLYMER JOURNAL》 * |
| 华正江等: ""无卤阻燃型交联乙烯-乙酸乙烯酯共聚物的剖析"", 《理化检验-化学分册》 * |
| 吕瑞瑞等: ""太阳能封装胶膜EVA中Va含量的测定"", 《合成材料老化与应用》 * |
| 田建军等: ""基于TGA - FTIR 联用技术的EVA 热解研究"", 《分析测试学报》 * |
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