CN103308358B - The preparation method of the Analysis of Heavy Metal standard substance of a kind of modified polyvinyl chloride and ABS mixture - Google Patents
The preparation method of the Analysis of Heavy Metal standard substance of a kind of modified polyvinyl chloride and ABS mixture Download PDFInfo
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- CN103308358B CN103308358B CN201310139076.8A CN201310139076A CN103308358B CN 103308358 B CN103308358 B CN 103308358B CN 201310139076 A CN201310139076 A CN 201310139076A CN 103308358 B CN103308358 B CN 103308358B
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Abstract
The present invention relates to the preparation method of the Analysis of Heavy Metal standard substance of a kind of modified polyvinyl chloride and ABS mixture, the steps include: load weighted base material to drop in heating in vacuum mixer according to mass ratio, make as required content of beary metal, dropping into should be containing the pure heavy metallic salt of quantitative analysis, and add the tetrahydrofuran solution of 3-5 times of solid matter and a small amount of diffusant and toner, soak 1-2 hour; Heavy metallic salt and pigment are evenly diffused in plastics; Plastic hybrid is taken out, be applied on glass plate, form plastic sheeting, dry approximately 2 hours, solvent is volatilized completely; Plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine; After dusting cover, also fully mix, make containing heavy metal plastics standard substance. Adopt dissolution with solvents paddling process, can produce containing heavy metal plastics standard substance by rapid batch, production efficiency is high.
Description
Technical field
The present invention relates to tester value Transfer Technology field, especially relate to and be widely used in harmful substance field tests,The particularly modified polyvinyl chloride in the consumer goods such as electric equipment products, toy product and ABS mixture Analysis of Heavy Metal standardThe preparation method of material.
Background technology
ABS (acrylonitrile-butadiene-styrene terpolymer) resin has impact resistance, high rigidity, and oil resistivity, resistance toLow temperature properties, chemical proofing, is a kind of purposes thermoplastic very widely. Polyvinyl chloride(PolyvinylChloride is called for short PVC) is China first, second-biggest-in-the-world universal synthetic resin material. At present, PVCBecome application one of plastics variety the most widely, in industry, building, agricultural, daily life, packaging, electric power, public affairsAll be widely used with fields such as causes, with polyethylene (PE), polypropylene (PP), polystyrene (PS) and acrylonitrile and butadieneBe referred to as five large resins for universal use with the copolymer (ABS) of benzene. But general polyvinyl chloride (PVC) micelle is easily heated and easily decomposes,The softer difficulty of material of final moulding is worn into uniform powder, and character is unstable. Particularly in the time of processing and forming, easily de-Remove HCl molecule, introduce unsaturated bond in macromolecular chain, this has just affected the ageing-resistant performance of resin greatly. Therefore, scientific researchWorker has carried out a large amount of study on the modification work to improve its toughness and heat endurance to it. After mid-term in 20th century, peopleBe subject to the inspiration of metal alloy thought, utilize the method for physical blending to carry out a large amount of study on the modification to polyvinyl chloride resin. ABS withThe ABS/PVC plastic alloy that PVC blend obtains can have ABS and PVC advantage separately concurrently, has good weatherability and comprehensivePhysical property.
European Union has announced ROHS instruction in 2003, within 2011, be updated to ROHS2.0 instruction, ban use of leaded (Pb),Mercury (Hg), cadmium (Cd), Cr VI (Cr6+) etc. harmful substance for electric equipment products, expanded to now multiple fields, becomeFor one of important environmental protection standard in the whole world.
Summary of the invention
The object of the invention is to overcome weak point of the prior art, provide a kind of easy to use fast, diffusion allThe preparation method of the Analysis of Heavy Metal standard substance of the modified polyvinyl chloride even, cost is low and ABS mixture.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for the Analysis of Heavy Metal standard substance of modified polyvinyl chloride and ABS mixture, is characterized in that,Wherein the content of base material polyvinyl chloride colloidal particle is 25%-68%, acrylonitrile, butadiene and cinnamic terpolymer ABS micelleContent is 25%-68%, and toner and content of beary metal are 3-8%, the steps include:
A, by load weighted polyvinyl chloride colloidal particle, acrylonitrile, butadiene and cinnamic terpolymer ABS micelle are pressedDrop in heating in vacuum mixer according to mass ratio, make as required content of beary metal, the analysis that drops into this content of beary metal is pureHeavy metallic salt, and add the tetrahydrofuran solution of 3-5 times of solid matter and a small amount of diffusant and toner, soak 1-2 hour; ProtectHold vacuum tank airtight, slowly start heating in vacuum mixer, rapid stirring 1-2 hour, makes plastic hybrid dissolve completely and mixClose evenly, heavy metallic salt and pigment are evenly diffused in plastics;
B, close mixer, plastic hybrid is taken out from heating in vacuum tank, be applied on glass plate, form plastics thinFilm, is positioned over glass plate in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely;
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine;
D, pulverize with common plastics flour mill, after crossing dusting cover and fully mix, make containing heavy metal plastics markAccurate material.
Heavy metallic salt is for analyzing pure lead stearate, barium chromate, cadmium stearate, mercury chloride.
Heavy metal lead, chromium, cadmium, every kind of constituent content interpolation scope of mercury are 10mg/kg-2000mg/kg.
Injection molded or granulation in comminutor in injection machine, make it more meet the sample profile of detection.
Beneficial effect of the present invention is: adopt dissolution with solvents paddling process, can produce containing heavy metal plastics by rapid batchStandard substance, production efficiency is high, and the good dispersion of heavy metal element in sample has also just ensured the uniformity of sample; SelectThe compatibility of the material of two kinds of raw materials is fine, and the sample of preparation has more representativeness; Under room temperature, preparing sample materials can not occurDecompose, thereby make plastic alloy more stable, also just ensured the stability of specimen material. This method can be to sample heavy metalContent adopts the method preparation of progressively dilution to become linear series standard substance.
Detailed description of the invention
The invention will be further described below:
A preparation method for modified polyvinyl chloride and ABS mixture Analysis of Heavy Metal standard substance, the steps include:
A, by load weighted white polyvinyl chloride (PVC) micelle and acrylonitrile, butadiene and cinnamic terpolymer(ABS) micelle drops in heating in vacuum mixer according to mass ratio, makes as required content of beary metal, drops into this heavy metal and containsThe pure heavy metallic salt of quantitative analysis, and add the tetrahydrofuran solution of 3-5 times of solid matter and a small amount of diffusant and toner, soak1-2 hour. Keep vacuum tank airtight, slowly start heating in vacuum mixer, rapid stirring 1-2 hour, makes plastic hybrid completeCL also mixes, and this process is for heavy metallic salt and pigment are evenly diffused in plastics.
B, close mixer, plastic hybrid is taken out from heating in vacuum tank, be applied on glass plate, form plastics thinFilm. Glass plate is positioned in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely.
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine.
D, pulverize with common plastics flour mill, after crossing 0.5mm sieve and fully mixes, make this standard material.
In order to make its sample profile that more meets detection, injection molded or granulation in comminutor in injection machine, exampleAs be prepared into the quantitative analysis of disk for XRF.
The heavy metallic salt that the present invention adds is: analyze pure lead stearate, barium chromate, cadmium stearate, mercury chloride.
Injection molded or granulation in comminutor in injection machine, make it more meet the sample profile of detection.
Embodiment 1(making 1Kg content is approximately the sample of 500mg/kg):
White polyvinyl chloride and 0.5Kg acrylonitrile, butadiene and the cinnamic terpolymer of a, weighing 0.5KgDrop in heating in vacuum mixer, progressively drop into lead stearate 3g, barium chromate 3g, cadmium stearate 6g, mercury chloride 0.9g powder,And add the tetrahydrofuran solution of about 5L and a small amount of diffusant and toner, soak 1-2 hour. Slowly start vacuum stirringMachine, rapid stirring 1-2 hour, makes mixture dissolve completely and mix. This process is in order to make heavy metallic salt and pigment equalEven being diffused in plastics.
B, close mixer, plastic hybrid is taken out from heating in vacuum tank, be applied on glass plate, form plastics thinFilm. Glass plate is positioned in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely.
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine.
D, pulverize with common plastics flour mill, after crossing 0.5mm sieve and fully mix, this sample is containing a huge sum of moneyBelong to plastics standard substance.
Embodiment 2(making 1Kg content is approximately the sample of 200mg/kg):
White polyvinyl chloride and 0.5Kg acrylonitrile, butadiene and the cinnamic terpolymer of a, weighing 0.5KgDrop in heating in vacuum mixer, progressively drop into lead stearate 1.2g, barium chromate 1.2g, cadmium stearate 2.4g, mercury chloride0.36g, and add tetrahydrofuran solution and a small amount of diffusant and the toner of about 5L, soak 1-2 hour. Continue to keep vacuumTank is airtight, and slowly starts heating in vacuum mixer, and rapid stirring 1-2 hour makes mixture dissolve completely and mix. ThisProcess is for heavy metallic salt and pigment are evenly diffused in plastics.
B, close mixer, plastic hybrid is taken out from heating in vacuum tank, be applied on glass plate, form plastics thinFilm. Glass plate is positioned in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely.
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine.
D, pulverize with common plastics flour mill, after crossing 0.5mm sieve and fully mix, this sample is both for containing a huge sum of moneyBelong to plastics standard substance.
Embodiment 3(making 1Kg content is approximately the sample of 100mg/kg)
White polyvinyl chloride and 0.5Kg acrylonitrile, butadiene and the cinnamic terpolymer of a, weighing 0.5KgDrop in heating in vacuum mixer, progressively drop into lead stearate 0.6g, barium chromate 0.6g, cadmium stearate 1.2g, mercury chloride0.18g, and add the tetrahydrofuran solution of about 5L, soak 1-2 hour. Continue to keep vacuum tank airtight, and slowly start trueEmpty heating mixer, rapid stirring 1-2 hour, makes mixture dissolve completely and mix. This process is in order to make heavy metalSalt and pigment are evenly diffused in plastics.
B, close mixer, plastic hybrid is taken out from heating in vacuum tank, be applied on glass plate, form plastics thinFilm. Glass plate is positioned in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely.
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine.
D, pulverize with common plastics flour mill, after crossing 0.5mm sieve and fully mix, this sample is containing a huge sum of moneyBelong to plastics standard substance.
Of the present invention having the following advantages:
1. adopt dissolution with solvents paddling process, can produce containing heavy metal plastics standard substance by rapid batch, production efficiency is high,The good dispersion of heavy metal element in sample, has also just ensured the uniformity of sample.
2. two kinds of plastics of the blend of selecting are two general large plastics, and these two kinds of Compatibility in Plastics are fine, the sample of preparationProduct are representative. By the method for dissolution with solvents physical mixed modification, two kinds of plastics low temperature physical mixed are unlikely toDecompose, material character superiority improves, thereby makes plastic alloy more stable, has also just ensured the stable of specimen materialProperty.
3. can adopt the method preparation of progressively dilution to become linear series standard substance to sample content of beary metal.
4. the present invention's material pvc, ABS, toner, diffusant used can be buied from plastic material market; StearicLead plumbate, barium chromate, cadmium stearate, mercury chloride, oxolane all can be buied from chemical reagent shop. Prepare mixer used,The general-purpose machinery that pulverizer, disintegrating machine, flour mill are plastic industry.
5. also can expand to the preparation of other heavy metal sample of similar plastics material.
The above is only to preferred embodiment of the present invention, not scope of the present invention is limited, therefore not de-Design from the present invention under the prerequisite of spirit, the common engineers and technicians in this area are to structure of the present invention, feature and principleThe equivalence of doing changes or decorates, and all should fall in the protection domain of the present patent application patent.
Claims (4)
1. a preparation method for the Analysis of Heavy Metal standard substance of modified polyvinyl chloride and ABS mixture, is characterized in that, itsThe content of middle base material polyvinyl chloride colloidal particle is 25%-68%, and acrylonitrile, butadiene and cinnamic terpolymer ABS micelle containAmount is 25%-68%, and toner and content of beary metal are 3-8%, the steps include:
A, by load weighted polyvinyl chloride colloidal particle, acrylonitrile, butadiene and cinnamic terpolymer ABS micelle are according to matterAmount, than dropping in heating in vacuum mixer, is made content of beary metal as required, drops into the pure huge sum of money of analysis of this content of beary metalBelong to salt, and add the tetrahydrofuran solution of 3-5 times of solid matter and a small amount of diffusant and toner, soak 1-2 hour; Keep trueSlack tank is airtight, slowly starts heating in vacuum mixer, and rapid stirring 1-2 hour dissolves plastic hybrid completely and mixes allEven, heavy metallic salt and pigment are evenly diffused in plastics;
B, close mixer, plastic hybrid taken out from heating in vacuum tank, be applied on glass plate, form plastic sheeting,Glass plate is positioned in drying box, and temperature is controlled at 50-60 DEG C, dry approximately 2 hours, solvent is volatilized completely;
C, the plastic hybrid after drying and volatilizing is taken off from glass plate, be ground into fragment with disintegrating machine;
D, pulverize with common plastics flour mill, after crossing dusting cover and fully mix, make containing heavy metal plastics reference materialMatter.
2. the preparation side of the Analysis of Heavy Metal standard substance of modified polyvinyl chloride according to claim 1 and ABS mixtureMethod, is characterized in that, heavy metallic salt is for analyzing pure lead stearate, barium chromate, cadmium stearate, mercury chloride.
3. the preparation side of the Analysis of Heavy Metal standard substance of modified polyvinyl chloride according to claim 1 and ABS mixtureMethod, is characterized in that, heavy metal lead, chromium, cadmium, every kind of constituent content interpolation scope of mercury are 10mg/kg-2000mg/kg.
4. the preparation side of the Analysis of Heavy Metal standard substance of modified polyvinyl chloride according to claim 1 and ABS mixtureMethod, is characterized in that, injection molded or granulation in comminutor in injection machine make it more meet the sample profile of detection.
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| CN103604678A (en) * | 2013-12-09 | 2014-02-26 | 广州赛宝计量检测中心服务有限公司 | Sample preparation method for uniformly distributing trace components in solid block matrix |
| CN104297422B (en) * | 2014-09-05 | 2016-02-17 | 国家电网公司 | Measure banded three metafiltration film bar and the manufacture methods of tenor tearing type in air |
| JP6303967B2 (en) * | 2014-10-09 | 2018-04-04 | 株式会社島津製作所 | Calibration method for pyrolysis gas chromatograph mass spectrometer |
| JP7217913B2 (en) * | 2018-02-16 | 2023-02-06 | 株式会社日立ハイテクサイエンス | Manufacturing method of plastic reference material |
| CN110819059A (en) * | 2019-11-04 | 2020-02-21 | 安徽建筑大学 | Preparation method of ABS plastic standard sample containing trace lead |
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| CN101329226A (en) * | 2007-10-29 | 2008-12-24 | 上海市计量测试技术研究院 | Method for preparing heavy metal ingredient standard substance in polyvinyl chloride |
| CN101793639A (en) * | 2010-02-10 | 2010-08-04 | 山东出入境检验检疫局检验检疫技术中心 | Preparation method of standard sample of high molecular material containing harmful substances |
| CN101857707A (en) * | 2010-06-29 | 2010-10-13 | 上海大学 | Environmental-protection type PVC/ABS plastic alloy material and preparation method thereof |
| CN102608225A (en) * | 2011-01-21 | 2012-07-25 | 中国检验检疫科学研究院 | Determination method of harmful organic substance residue in toy sample |
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| JPS5599052A (en) * | 1979-01-24 | 1980-07-28 | Horiba Ltd | Production of solid standard test piece used in measuring device of sulfur and chlorine with fluorescent x-ray |
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| CN101329226A (en) * | 2007-10-29 | 2008-12-24 | 上海市计量测试技术研究院 | Method for preparing heavy metal ingredient standard substance in polyvinyl chloride |
| CN101793639A (en) * | 2010-02-10 | 2010-08-04 | 山东出入境检验检疫局检验检疫技术中心 | Preparation method of standard sample of high molecular material containing harmful substances |
| CN101857707A (en) * | 2010-06-29 | 2010-10-13 | 上海大学 | Environmental-protection type PVC/ABS plastic alloy material and preparation method thereof |
| CN102608225A (en) * | 2011-01-21 | 2012-07-25 | 中国检验检疫科学研究院 | Determination method of harmful organic substance residue in toy sample |
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Effective date of registration: 20160708 Address after: Dongguan City, Guangdong province Changping 523000 Luqiao Industrial City Longchang Li Huang Chang Patentee after: DONGGUAN ZHONGSI DETECTION ELECTRONIC TECHNOLOGY CO., LTD. Patentee after: Lung Cheong International Holdings Limited Address before: Dongguan City, Guangdong province Changping 523000 Luqiao Industrial City Longchang Li Huang Chang Patentee before: Dongguan Lung Cheong Institute of Intelligent Technology Patentee before: Lung Cheong International Holdings Limited |
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