CN102344624A - Preparation method of standard sample for testing phthalic ester plasticizer - Google Patents
Preparation method of standard sample for testing phthalic ester plasticizer Download PDFInfo
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- CN102344624A CN102344624A CN2011101852791A CN201110185279A CN102344624A CN 102344624 A CN102344624 A CN 102344624A CN 2011101852791 A CN2011101852791 A CN 2011101852791A CN 201110185279 A CN201110185279 A CN 201110185279A CN 102344624 A CN102344624 A CN 102344624A
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Abstract
The invention provides a preparation method of a standard sample for testing a phthalic ester plasticizer. The preparation method comprises the following steps of: uniformly mixing a phthalic ester plasticizer serving as a target compound with a stabilizer, a lubricant and the like to form a mixture; stirring the mixture and a substrate material at a high speed; stirring, cooling, extruding and blowing to obtain a film of which the thickness is 25-30 mum; and performing serial processing on the film to obtain the standard sample. The invention has the advantages: the standard sample for testing the phthalic ester plasticizer is obtained with the preparation method which is easy and convenient to operate, the comparability and consistence of detection data of the phthalic ester plasticizer in plastic among laboratories are improved, and a basis for uniformly testing the standard of the phthalic ester plasticizer in plastic is laid.
Description
[technical field]
The present invention relates to a kind of preparation method of standard model, relate in particular to a kind of phthalic ester plasticizer and measure preparation method with standard model.
[background technology]
Phthalic ester plasticizer is mainly used in and improves processing of plastic performance and intensity, is widely used in plastics and elastomeric material production.Be connected with Van der Waals force by hydrogen bond between phthalic ester plasticizer and the plastic molecules, keep relatively independent separately chemical property each other, then phthalic ester plasticizer is moved to the environment from plastics easily.Scientific research finds that this compounds of phthalic ester plasticizer can disturb human endocrine; Infringement reproduction and growth; States such as European Union, the U.S., Japan formulate the use of such material of regulation limitations in food contact material, toy and youngster's articles for use one after another; Like the 2005/84/EC of European Union instruction, 2002/72/EC instruction, U.S.'s consumer's goods improvements in security in 2008 bill etc.Most of toys and articles for children and packaging material for food all contain plastic components, and the problem of phthalic ester plasticizer has caused the extensive pass of society in the plastics.
More about the examination criteria and the method for phthalic ester plasticizer in the plastics both at home and abroad, examination criteria and the method that adopt different test experience chamber are not quite similar.Recognized prison committee (full name is a China national Certification and Accreditation Administration) " mensuration of phthalic ester plasticizer the plastics " proficiency testing project and see in 2009 that bear from the applicant; Many laboratory test results differ greatly; Through investigating and analyze, lack the plastics phthalic ester plasticizer standard model that is used for test process quality monitoring further is an important factor.Therefore; Develop in the plastics phthalic ester plasticizer as early as possible and measure with standard model for improving food contact material, toy and articles for children manufacturing enterprise and supervision department and the breadboard detection level of social third party, aspects such as assurance toy and articles for children quality safety have crucial meaning.
[summary of the invention]
Technical problem to be solved by this invention is to provide a kind of phthalic ester plasticizer to measure the preparation method with standard model; For possibility is laid a good foundation, provided to the unified standard that detects phthalic ester plasticizer in the plastics, and simple and convenient, workable characteristics are arranged.
The present invention solves the problems of the technologies described above through following technical scheme: a kind of phthalic ester plasticizer is measured the preparation method with standard model, specifically comprises the steps:
Step 1: the supplementary material of standard specimen is made up of target compound phthalic ester plasticizer, stablizer, lubricant and body material; According to required an amount of target compound phthalic ester plasticizer and stablizer, the lubricant of taking by weighing of standard specimen; And the three mixed the formation mixture, and wherein stabilizer comprises standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight;
Step 2: get body material and above-mentioned said mixture, and will stir in the two input high speed agitator, the speed setting of agitator is 2400 commentaries on classics/min, treats that the interior temperature of agitator stops when rising to 110 ℃～120 ℃ stirring and being cooled to below 45 ℃;
Step 3: the mixture that step 2 is stirred cooling back gained is extruded blown film; To produce the film that obtains film thickness 25 μ m～30 μ m; Then preceding 1/5 and back 1/5 part of this film are given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion; Excise the part of each 20cm of its both sides again, the film portion that remains at last is standard model.
Further; Phthalic ester plasticizer is measured the preparation method with standard model; It is characterized in that: the condition of extruding blown film in the said step 3 is: the blown film rotating speed of motor is 1000～1200 commentaries on classics/min, and the temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5.
Further, said body material is a polyvinyl chloride.
Beneficial effect of the present invention is: obtain phthalic ester plasticizer mensuration standard model through preparation method of the present invention; Help to improve between the laboratory comparability and consistence that phthalic ester plasticizer in the plastics detects data; For possibility is laid a good foundation, provided to the unified standard that detects phthalic ester plasticizer in the plastics, have great importance to guaranteeing aspects such as plastic toy and articles for children quality safety; In addition, preparation method of the present invention has simple and convenient, workable characteristics.
[embodiment]
Phthalic ester plasticizer of the present invention is measured the preparation method with standard model; The supplementary material that specifically comprises the steps: (1) standard specimen is made up of target compound phthalic ester plasticizer, stablizer, lubricant and body material; According to required an amount of target compound phthalic ester plasticizer and stablizer, the lubricant of taking by weighing of standard specimen; And the three mixed the formation mixture, and wherein stabilizer comprises standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight; (2) get body material and above-mentioned said mixture, and will stir in the two input high speed agitator, the speed setting of agitator is 2400 commentaries on classics/min, treats that the interior temperature of agitator stops when rising to 110 ℃～120 ℃ stirring and being cooled to below 45 ℃; (3) mixture that step 2 is stirred cooling back gained is extruded blown film; To produce the acquisition film thickness is the film of 25 μ m～28 μ m; Then preceding 1/5 and back 1/5 part of this film are given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion; Excise the part of each 20cm of its both sides again, the film portion that remains at last is standard model.In addition, in the present invention, in order to make the film that blows out comparatively desirable, with the condition enactment of extruding blown film be: the blown film rotating speed of motor is 1000～1200 commentaries on classics/min, and the temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5; Phthalic ester plasticizer can be any one or more in phthalic acid two (2-ethylhexyl) ester (DEHP), dibutyl phthalate (DBP), the dinoctyl phthalate (DNOP); Stablizer is an organotin, and lubricant is 16～octadecyl alcohol ester and polyene wax; Body material is generally selected for use has material stable preferably than tool under strong representativeness, the normal temperature and that be convenient to deposit in the use, such as polyvinyl chloride (PVC); The phthalic ester plasticizer Determination on content generally adopts solvent extraction in the plastics; Therefore the size of standard model will be guaranteed the consistence of detected result; This to this point; The present invention has processed the plastics film of thickness 25 μ m～30 μ m with standard model, has guaranteed the unanimity of detected result basically.
For better the present invention will be described, the present invention has lifted following several embodiment.
Embodiment one
The content of preparation DEHP, DBP, DNOP accounts for the standard model of standard specimen supplementary material gross weight 0.19%, 0.12%, 0.25% respectively:
When the gross weight of standard specimen supplementary material is about 174kg; Take by weighing 330.6g DEHP, 208.8g DBP, 435gDNOP, 1.74kg organotin and 3.48kg lubricant respectively; And the three mixed; Earlier said mixture is dropped in the high speed agitator; Start high speed agitator; Drop into polyvinyl chloride (PVC) powder of about 165kg again from the top of agitator, continue to stir, speed setting is 2400 commentaries on classics/min; Treat that the interior temperature of agitator stops when rising to 110 ℃ stirring and being cooled to below 45 ℃; Adopt inflation film manufacturing machine to extrude blown film in the mixture that stirs cooling back gained; The blown film rotating speed of motor is 1100 commentaries on classics/min; The blown film temperature is 165 ℃; And blow-up ratio is 2.5, and producing and obtaining film thickness is the film of 28 μ m, then preceding 1/5 and back 1/5 part of this film is given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion, the part of excising each 20cm of its both sides again, the film portion that remains at last is standard model.
Embodiment two
The content of preparation DEHP, DBP, DNOP accounts for the standard model of standard specimen supplementary material gross weight 0.28%, 0.25%, 0.20% respectively:
When the gross weight of standard specimen supplementary material is about 174kg; Take by weighing 487.2g DEHP, 435g DBP, 348gDNOP, 2.61kg organotin and 4.35kg lubricant respectively; And the three mixed; Earlier said mixture is dropped in the high speed agitator; Start high speed agitator; Drop into about 165kg polyvinyl chloride (PVC) powder from the top of high speed agitator again, continue to stir, speed setting is 2400 commentaries on classics/min; Treat that the interior temperature of agitator stops when rising to 120 ℃ stirring and being cooled to below 45 ℃; Adopt inflation film manufacturing machine to extrude blown film in the mixture that stirs cooling back gained; The blown film rotating speed of motor is 1000 commentaries on classics/min; The blown film temperature is 170 ℃; And blow-up ratio is 2.5, and producing and obtaining film thickness is the film of 30 μ m, then preceding 1/5 and back 1/5 part of this film is given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion, the part of excising each 20cm of its both sides again, the film portion that remains at last is standard model.
Embodiment three
The content of preparation DEHP, DBP, DNOP accounts for the standard model of standard specimen supplementary material gross weight 0.28%, 0.25%, 0.20% respectively:
When the gross weight of standard specimen supplementary material is about 174kg; Take by weighing 487.2g DEHP, 435gDBP, 348gDNOP, 3.48kg organotin and 5.22kg lubricant respectively; And the three mixed; Earlier said mixture is dropped in the high speed agitator; Start high speed agitator; Drop into about 165kg polyvinyl chloride (PVC) powder from the top of high speed agitator again, continue to stir, speed setting is 2400 commentaries on classics/min; Treat that the interior temperature of agitator stops when rising to 115 ℃ stirring and being cooled to below 45 ℃; Adopt inflation film manufacturing machine to extrude blown film in the mixture that stirs cooling back gained; The blown film rotating speed of motor is 1200 commentaries on classics/min; The blown film temperature is 160 ℃; And blow-up ratio is 2.5, and producing and obtaining film thickness is the film of 25 μ m, then preceding 1/5 and back 1/5 part of this film is given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion, the part of excising each 20cm of its both sides again, the film portion that remains at last is standard model.
With standard model that above-mentioned each embodiment obtained respectively according to GB/T 15000 series standards; Adopt GB/T 22048-2008 detection method to carry out uniformity test and stability test; Wherein: uniformity test adopts one-factor analysis of variance method (F method), and the F value that test draws made standard model is all less than threshold value F
α(f
1, f
2) (α=0.05 wherein, f
1=14, f
2=30), show that promptly made standard model is uniform; " mean value consistency check " method in the t method of inspection is adopted in stability test, and be 10 days, 1 month, 6 months, 12 months the pitch time in the checkout procedure, and the t value that test draws made standard model is all less than threshold value t
α(n
1+ n
2-2) (α=0.05 wherein, n
1=45, n
2=10), show that promptly made standard model is stable.
To sum up; Obtain phthalic ester plasticizer mensuration standard model through preparation method of the present invention; Help to improve between the laboratory comparability and consistence that phthalic ester plasticizer in the plastics detects data, laying a good foundation, provide for the unified standard that detects phthalic ester plasticizer in the plastics maybe; In addition, preparation method of the present invention has simple and convenient, workable characteristics.
Claims (3)
1. a phthalic ester plasticizer is measured the preparation method with standard model, and it is characterized in that: it specifically comprises the steps:
Step 1: the supplementary material of standard specimen is made up of target compound phthalic ester plasticizer, stablizer, lubricant and body material; According to required an amount of target compound phthalic ester plasticizer and stablizer, the lubricant of taking by weighing of standard specimen; And the three mixed the formation mixture, and wherein stabilizer comprises standard specimen supplementary material gross weight 1～2%, lubricant accounts for 2～3% of standard specimen supplementary material gross weight;
Step 2: get body material and above-mentioned said mixture, and will stir in the two input high speed agitator, the speed setting of agitator is 2400 commentaries on classics/min, treats that the interior temperature of agitator stops when rising to 110 ℃～120 ℃ stirring and being cooled to below 45 ℃;
Step 3: the mixture that step 2 is stirred cooling back gained is extruded blown film; To produce the film that obtains film thickness 25 μ m～30 μ m; Then preceding 1/5 and back 1/5 part of this film are given up; Only stay the film of middle portion; Afterwards after the film rolling of this middle portion; Excise the part of each 20cm of its both sides again, the film portion that remains at last is standard model.
2. phthalic ester plasticizer as claimed in claim 1 is measured the preparation method with standard model; It is characterized in that: the condition of extruding blown film in the said step 3 is: the blown film rotating speed of motor is 1000～1200 commentaries on classics/min; The temperature of blown film is 160 ℃～170 ℃, and blow-up ratio is 2.5.
3. phthalic ester plasticizer as claimed in claim 1 is measured the preparation method with standard model, and it is characterized in that: said body material is a polyvinyl chloride.
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| CN 201110185279 CN102344624B (en) | 2011-06-30 | 2011-06-30 | Preparation method of standard sample for testing phthalic ester plasticizer |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103293037A (en) * | 2013-02-06 | 2013-09-11 | 东莞龙昌智能技术研究院 | Lead-containing paint coating standard substance and preparation method thereof |
| CN103308357A (en) * | 2013-04-20 | 2013-09-18 | 东莞龙昌智能技术研究院 | Lead-containing paint coating standard substance and preparation method thereof |
| 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 |
| CN105510450A (en) * | 2014-10-09 | 2016-04-20 | 株式会社岛津制作所 | Reference sample for analysis |
| CN105602022A (en) * | 2016-01-29 | 2016-05-25 | 福建出入境检验检疫局检验检疫技术中心 | Preparation method of standard rubber sample for determining phenol |
| CN105647046A (en) * | 2016-04-11 | 2016-06-08 | 北京市理化分析测试中心 | Preparation method of phenolic-antioxidant-containing positive control substance of food contact plastics |
| CN106633505A (en) * | 2016-11-26 | 2017-05-10 | 金发科技股份有限公司 | Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC) |
| CN106751217A (en) * | 2016-12-28 | 2017-05-31 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN106832881A (en) * | 2017-01-16 | 2017-06-13 | 浙江省计量科学研究院 | Phthalic ester plasticizer and phosphorus flame retardant standard sample and sample preparation methods in polyurethane |
| CN107462450A (en) * | 2017-08-22 | 2017-12-12 | 中纺协检验（泉州）技术服务有限公司 | A kind of production method of standard specimen textile |
| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
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| CN103293037A (en) * | 2013-02-06 | 2013-09-11 | 东莞龙昌智能技术研究院 | Lead-containing paint coating standard substance and preparation method thereof |
| CN103308357A (en) * | 2013-04-20 | 2013-09-18 | 东莞龙昌智能技术研究院 | Lead-containing paint coating standard substance and preparation method thereof |
| 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 |
| CN108132320A (en) * | 2014-10-09 | 2018-06-08 | 株式会社岛津制作所 | The bearing calibration of thermal cracking gas chromatography mass spectrometer |
| CN105510450A (en) * | 2014-10-09 | 2016-04-20 | 株式会社岛津制作所 | Reference sample for analysis |
| US11204342B2 (en) | 2014-10-09 | 2021-12-21 | Shimadzu Corporation | Reference sample for analysis |
| CN105602022A (en) * | 2016-01-29 | 2016-05-25 | 福建出入境检验检疫局检验检疫技术中心 | Preparation method of standard rubber sample for determining phenol |
| CN105602022B (en) * | 2016-01-29 | 2018-03-23 | 福建出入境检验检疫局检验检疫技术中心 | A kind of preparation method of phenol measure standard rubbers sample |
| CN105647046A (en) * | 2016-04-11 | 2016-06-08 | 北京市理化分析测试中心 | Preparation method of phenolic-antioxidant-containing positive control substance of food contact plastics |
| CN106633505A (en) * | 2016-11-26 | 2017-05-10 | 金发科技股份有限公司 | Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC) |
| CN106751217A (en) * | 2016-12-28 | 2017-05-31 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN106832881A (en) * | 2017-01-16 | 2017-06-13 | 浙江省计量科学研究院 | Phthalic ester plasticizer and phosphorus flame retardant standard sample and sample preparation methods in polyurethane |
| CN107462450A (en) * | 2017-08-22 | 2017-12-12 | 中纺协检验（泉州）技术服务有限公司 | A kind of production method of standard specimen textile |
| CN108254472A (en) * | 2017-09-30 | 2018-07-06 | 广东华科检测技术服务有限公司 | Phthalic acid ester standard sample and preparation method thereof in PVC coating textile fabrics |
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| CN112011125A (en) * | 2020-09-07 | 2020-12-01 | 石家庄海关技术中心 | Polypropylene film standard sample with plasticizer migration value and preparation method thereof |
| CN112011125B (en) * | 2020-09-07 | 2022-11-11 | 石家庄海关技术中心 | Polypropylene film standard sample with plasticizer migration value and preparation method thereof |
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