CN104950049B - A kind of analysis method of copolyamide PUR relative molecular weight and its distribution - Google Patents
A kind of analysis method of copolyamide PUR relative molecular weight and its distribution Download PDFInfo
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- CN104950049B CN104950049B CN201410167005.3A CN201410167005A CN104950049B CN 104950049 B CN104950049 B CN 104950049B CN 201410167005 A CN201410167005 A CN 201410167005A CN 104950049 B CN104950049 B CN 104950049B
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Abstract
The present invention relates to a kind of analysis method of copolyamide PUR relative molecular weight and its distribution, it is standard substance that the method chooses PMMA, it is dissolved to the standard specimen that mass concentration is 0.1% 0.5% with the chloroform methanol mixed solution that chloroform percent by volume is 35% 65%, using WATERS chromatograph of gel permeation, Composition distribution, silica gel chromatographic column, column length 300mm, internal diameter 7.8mm, 5 μm of silica gel particle diameter, the chloroform methanol mixed solution that mobile phase is 35% 65% using chloroform percent by volume, flow velocity 0.2 1.0ml/min, calorstat temperature is 30 DEG C 45 DEG C of chromatographic condition analytical standard sample one by one, make standard curve, determine calibration curve equation.Then accurately weigh copolyamide PUR sample, being dissolved to mass concentration with the chloroform methanol mixed solution that chloroform percent by volume is 35% 65% is 0.1% 1.0%, with the analysis of above-mentioned chromatographic condition sample introduction.The present invention has the advantages that operation is simple, favorable reproducibility, precision are high.
Description
Technical field
The invention belongs to Analysis of Macromolecular Materials technical field, it is related to a kind of gel osmoticing chromatogram analysis copolyamide hot melt
The method of glue relative molecular weight and its distribution.
Background technology
Copolyamide PUR, as a kind of PUR of high-performance high quality series, is widely used to dress lining cloth, vapour
The every field such as turner industry, furniture and shoemaking.The molecular weight of polymer and its distribution are the basic parameters weighing macromolecular material
One of, but due to copolyamide PUR self-characteristic, typically do not dissolve in usual vehicle, so be difficult to analyze its molecular weight and its
Distribution, often goes to replace using melt index, is unfavorable for the understanding to mechanism of polymerization for the people, thus the research and development affecting new product are entered
Journey.Analysis method about copolyamide PUR molecular weight and its distribution still belongs to blank at present.
It is an object of the invention to provide a kind of gel osmoticing chromatogram analysis copolyamide PUR relative molecular mass and
The method of distribution.
Content of the invention
A kind of analysis method of copolyamide PUR relative molecular weight and its distribution, mainly includes the following steps that：
(1) the preparation of standard sample solution
Choose the poly-methyl methacrylate of Mp=2825,4900,7500,11800,35000,122500,195000 respectively
Ester (PMMA) standard sample, and dissolved with a kind of mixed solution, make mass concentration in this mixed solution for the standard sample
For 0.1%-0.5%；
(2) the making of standard curve
Using WATERS 1515 chromatograph of gel permeation, Composition distribution, silica gel chromatographic column：Column length 300mm, internal diameter
7.8mm, silica gel particle diameter：5 μm, mobile phase is above-mentioned mixed solution, flow velocity 0.2-1.0ml/min, calorstat temperature be 30 DEG C-
45 DEG C of chromatographic condition, is analyzed one by one to the standard sample solution of above-mentioned preparation, makes standard curve, determines standard curve
Equation；
(3) the analysis of copolyamide PUR relative molecular mass and its distribution
It is dissolved in copolyamide PUR sample in above-mentioned mixed solution, being configured to mass concentration is 0.1%-1.0%
Solution, wait system balance and stability after, be analyzed with above-mentioned chromatographiccondition, obtain this sample molecular weight and its point
Cloth；
Described mixed solution is chloroform-methanol mixed solution, and wherein, chloroform percent by volume is 35%-
65%.
The range of number-average molecular weight of described copolyamide PUR is 10000-150000, and fusion range is 95 DEG C -135
℃.
The innovation of the present invention is：Provide a kind of mixed solvent, can be good at dissolving copolyamide PUR,
So that the mensure of molecular weight and its distribution can smoothly be carried out using gel permeation chromatography, the method operation that the present invention provides
Easy, precision is high, favorable reproducibility.
Specific embodiment
Will be further understood that the present invention from following examples.
(1) the preparation of standard sample solution
Choose the poly- first of Mp=2825,4900,7500,11800,35000,122500,195000 of APSC company respectively
Base acrylic acid methyl ester. (PMMA) standard sample, and dissolved with a kind of mixed solution, make standard sample in this mixed solution
Mass concentration be 0.1%, chloroform-methanol mixed that described mixed solution is 40% for chloroform percent by volume
Solution；
(2) the making of standard curve
Using WATERS chromatograph of gel permeation, 2414 Composition distribution, silica gel chromatographic column：Column length 300mm, internal diameter
7.8mm, silica gel particle diameter：5 μm, the chloroform that mobile phase is 40% for chloroform percent by volume-methanol mixed solution,
HPLC level, flow velocity 1.0ml/min, calorstat temperature is 35 DEG C of chromatographic condition, and the standard sample solution of above-mentioned preparation is carried out
Analyze one by one, with elution volume as abscissa, the logarithmic function of Mw is vertical coordinate, produces standard curve, obtains dependent equation
Formula LogMw=8.5599-0.2871V, wherein M-Mw molecular weight；V- elution volume；Linearly dependent coefficient is 0.9994.
(3) the analysis of copolyamide PUR relative molecular mass and its distribution
Weigh appropriate copolyamide PUR sample, be dissolved in chloroform that chloroform percent by volume is 40%-
Methanol mixed solution, is configured to the testing sample solution that mass concentration is 0.3%, after waiting system balance and stability, with above-mentioned color
Analysis of spectrum condition is measured, and obtains number-average molecular weight Mn=16647 of copolyamide PUR, weight average molecular weight Mw=
22529, polydispersity coefficient PD=1.3533.
(4) repeatability experiment
Weigh copolyamide PUR sample, be dissolved in chloroform-methanol that chloroform percent by volume is 40%
Mixed solution, is configured to the testing sample solution that mass concentration is 0.3%, treats that sample is completely dissolved, and is respectively placed in five samples
In bottle, after waiting system balance and stability, it is measured with above-mentioned chromatographiccondition.Concrete determination data is shown in Table 1.
Table 1 copolyamide PUR sample repeatability experimental result
Found out by the data that table 1 measures, relative standard deviation RSD of the copolyamide PUR sample recording, much little
5% requiring in chromatograph of gel permeation test specification, illustrates that the analysis method of the present invention is reproducible, precision is high.
Claims (2)
1. a kind of analysis method of copolyamide PUR relative molecular weight and its distribution, mainly includes the following steps that：
(1) the preparation of standard sample solution
Choose the polymethyl methacrylate of Mp=2825,4900,7500,11800,35000,122500,195000 respectively
(PMMA) standard sample, and being dissolved with a kind of mixed solution, makes the mass concentration in this mixed solution for the standard sample be
0.1%-0.5%；
(2) the making of standard curve
Using WATERS chromatograph of gel permeation, Composition distribution, silica gel chromatographic column：Column length 300mm, internal diameter 7.8mm, silicon particle
Footpath：5 μm, mobile phase is above-mentioned mixed solution, flow velocity 0.2-1.0ml/min, and calorstat temperature is 30 DEG C -45 DEG C of chromatostrip
Part, is analyzed one by one to the standard sample solution of above-mentioned preparation, makes standard curve, determines calibration curve equation；
(3) the analysis of copolyamide PUR relative molecular mass and its distribution
It is dissolved in copolyamide PUR sample in above-mentioned mixed solution, being configured to mass concentration is the molten of 0.1%-1.0%
Liquid, after waiting system balance and stability, is analyzed with above-mentioned chromatographiccondition, obtains molecular weight and its distribution of this sample；
Described mixed solution is chloroform-methanol mixed solution, and wherein, the percent by volume of chloroform is 35%-
65%.
2. a kind of analysis method of copolyamide PUR relative molecular weight and its distribution as claimed in claim 1, its feature
It is, the range of number-average molecular weight of described copolyamide PUR is 10000-150000, and fusion range is 95-135 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410167005.3A CN104950049B (en) | 2014-04-23 | 2014-04-23 | A kind of analysis method of copolyamide PUR relative molecular weight and its distribution |
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| CN201410167005.3A CN104950049B (en) | 2014-04-23 | 2014-04-23 | A kind of analysis method of copolyamide PUR relative molecular weight and its distribution |
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| CN104950049B true CN104950049B (en) | 2017-03-08 |
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| CN110220986B (en) * | 2019-05-27 | 2021-08-24 | 浙江巨化技术中心有限公司 | Analysis method for relative molecular mass and distribution of perfluorosulfonic acid |
| CN112798693B (en) * | 2019-11-13 | 2023-11-21 | 浙江圣兆药物科技股份有限公司 | Method for accurately monitoring PLG molecular weight change in microsphere preparation process |
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| RU2525311C2 (en) * | 2008-09-18 | 2014-08-10 | Мицубиси Гэс Кемикал Компани, Инк. | Polyamide resin |
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Address after: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505 Patentee after: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. Patentee after: Kunshan Tianyang New Material Co.,Ltd. Patentee after: EAST CHINA University OF SCIENCE AND TECHNOLOGY Address before: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505 Patentee before: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. Patentee before: KUNSHAN TIANYANG HOT MELT ADHESIVE Co.,Ltd. Patentee before: EAST CHINA University OF SCIENCE AND TECHNOLOGY |
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Address after: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505 Patentee after: Tianyang New Material (Shanghai) Technology Co.,Ltd. Patentee after: Kunshan Tianyang New Material Co.,Ltd. Patentee after: EAST CHINA University OF SCIENCE AND TECHNOLOGY Address before: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505 Patentee before: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd. Patentee before: Kunshan Tianyang New Material Co.,Ltd. Patentee before: EAST CHINA University OF SCIENCE AND TECHNOLOGY |