CN104950049A - Method for analyzing relative molecular mass and distribution of copolyamide hot melt adhesive - Google Patents
Method for analyzing relative molecular mass and distribution of copolyamide hot melt adhesive Download PDFInfo
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- CN104950049A CN104950049A CN201410167005.3A CN201410167005A CN104950049A CN 104950049 A CN104950049 A CN 104950049A CN 201410167005 A CN201410167005 A CN 201410167005A CN 104950049 A CN104950049 A CN 104950049A
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Abstract
The invention relates to a method for analyzing relative molecular mass and distribution of a copolyamide hot melt adhesive. The method comprises the following steps: selecting PMMA as a standard substance, dissolving the substance into a standard sample with the mass concentration of 0.1-0.5 percent by using a trichloromethane-methanol mixed solution of which the volume percent of trichloromethane is 35-65 percent, with a WATERS gel permeation chromatograph, a differential refraction detector and a silica gel column, wherein the column length is 300mm, the inner diameter is 7.8mm, and the silica gel particle size is 5 microns, analyzing the standard sample one by one under the chromatographic conditions that the mobile phase refers to the trichloromethane-methanol mixed solution of which the volume percent of trichloromethane is 35-65 percent, the flow velocity is 0.2-1.0ml/min and the temperature of a thermostat is 30-45 DEG C, manufacturing a standard curve, and determining a standard curve equation; and accurately weighing a copolyamide hot melt adhesive sample, dissolving the sample to obtain a new sample with the mass concentration of 0.1-1.0 percent by using the trichloromethane-methanol mixed solution of which the volume percent of trichloromethane is 35-65 percent, and performing sample introduction analysis under the chromatographic conditions. The method disclosed by the invention has the advantages of simplicity in operation, high reproducibility and high precision.
Description
Technical field
The invention belongs to Analysis of Macromolecular Materials technical field, relate to a kind of method of gel osmoticing chromatogram analysis copolyamide hot melt adhesive relative molecular weight and its distribution.
Background technology
Copolyamide hot melt adhesive, as a kind of hot melt adhesive of high-performance high quality series, has been widely used in the every field such as dress lining cloth, auto industry, furniture and shoemaking.The molecular weight of polymkeric substance and distribution thereof are one of basic parameters weighing macromolecular material, but due to copolyamide hot melt adhesive self-characteristic, generally be insoluble to usual vehicle, so be difficult to analyze its molecular weight and distribution thereof, melting index is often adopted to go to replace, be unfavorable for the understanding of people to polymerization mechanism, thus affect the research and development process of new product.At present about the analytical approach of copolyamide hot melt adhesive molecular weight and distribution thereof still belongs to blank.
The object of the present invention is to provide a kind of method of gel osmoticing chromatogram analysis copolyamide hot melt adhesive relative molecular weight and its distribution.
Summary of the invention
An analytical approach for copolyamide hot melt adhesive relative molecular weight and its distribution, mainly comprises the following steps:
(1) the preparation of standard model solution
Choose respectively Mp=2825,4900,7500,11800,35000,122500, the PMMA standard model of 195000, and to be dissolved with a kind of mixed solution, make the mass concentration of standard model in this mixed solution be 0.1%-0.5%;
(2) the making of typical curve
Adopt WATERS 1515 gel permeation chromatograph, 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 is the chromatographic condition of 30 DEG C-45 DEG C, analyzes one by one the standard model solution of above-mentioned preparation, production standard curve, confirmed standard curvilinear equation;
(3) the analysis of copolyamide hot melt adhesive relative molecular mass and its distribution
By copolyamide hot melt adhesive sample, be dissolved in above-mentioned mixed solution, be mixed with the solution that mass concentration is 0.1%-1.0%, after waiting for system balance and stability, analyze with above-mentioned chromatographiccondition, obtain molecular weight and the distribution thereof of this sample;
Described mixed solution is methenyl choloride-methyl alcohol mixed solution, and wherein, methenyl choloride percent by volume is 35%-65%.
The number-average molecular weight scope of described copolyamide hot melt adhesive is 10000-150000, and fusion range is 95 DEG C-135 DEG C.
Innovation of the present invention is: provide a kind of mixed solvent, can be good at dissolving copolyamide hot melt adhesive, gel permeation chromatography can be adopted smoothly to carry out the mensuration of molecular weight and distribution thereof, method provided by the invention is easy and simple to handle, precision is high, favorable reproducibility.
Embodiment
The present invention is will be further understood that from following examples.
(1) the preparation of standard model solution
Choose respectively the Mp=2825 of APSC company, 4900,7500,11800,35000,122500, the PMMA standard model of 195000, and dissolved with a kind of mixed solution, make the mass concentration of standard model in this mixed solution be 0.1%, described mixed solution to be methenyl choloride percent by volume be 40% methenyl choloride-methyl alcohol mixed solution;
(2) the making of typical curve
Adopt WATERS gel permeation chromatograph, 2414 Composition distribution, silica gel chromatographic column: column length 300mm, internal diameter 7.8mm, silica gel particle diameter: 5 μm, mobile phase to be methenyl choloride percent by volume be 40% methenyl choloride-methyl alcohol mixed solution, HPLC level, flow velocity 1.0ml/min, calorstat temperature is the chromatographic condition of 35 DEG C, the standard model solution of above-mentioned preparation is analyzed one by one, take elution volume as horizontal ordinate, the logarithmic function of Mw is ordinate, produces typical curve, obtain correlate equation LogMw=8.5599-0.2871V, wherein M-Mw molecular weight; V-elution volume; Linearly dependent coefficient is 0.9994.
(3) the analysis of copolyamide hot melt adhesive relative molecular mass and its distribution
Take appropriate copolyamide hot melt adhesive sample, be dissolved in methenyl choloride-methyl alcohol mixed solution that methenyl choloride percent by volume is 40%, be mixed with the testing sample solution that mass concentration is 0.3%, after wait system balance and stability, measure with above-mentioned chromatographiccondition, obtain the number-average molecular weight Mn=16647 of copolyamide hot melt adhesive, weight-average molecular weight Mw=22529, polydispersity coefficient PD=1.3533.
(4) reappearance experiment
Take copolyamide hot melt adhesive sample, be dissolved in methenyl choloride-methyl alcohol mixed solution that methenyl choloride percent by volume is 40%, be mixed with the testing sample solution that mass concentration is 0.3%, treat that sample dissolves completely, be placed in five sample bottles respectively, after wait system balance and stability, measure with above-mentioned chromatographiccondition.Concrete determination data is in table 1.
Table 1 copolyamide hot melt adhesive sample repeatability experimental result
The data measured by table 1 are found out, the relative standard deviation RSD of the copolyamide hot melt adhesive sample recorded, is far smaller than require in gel permeation chromatograph test specification 5%, illustrates that analytical approach of the present invention is reproducible, precision is high.
Claims (2)
1. an analytical approach for copolyamide hot melt adhesive relative molecular weight and its distribution, mainly comprises the following steps:
(1) the preparation of standard model solution
Choose respectively Mp=2825,4900,7500,11800,35000,122500, the PMMA standard model of 195000, and to be dissolved with a kind of mixed solution, make the mass concentration of standard model in this mixed solution be 0.1%-0.5%;
(2) the making of typical curve
Adopt WATERS gel permeation chromatograph, 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 is the chromatographic condition of 30 DEG C-45 DEG C, analyzes one by one the standard model solution of above-mentioned preparation, production standard curve, confirmed standard curvilinear equation;
(3) the analysis of copolyamide hot melt adhesive relative molecular mass and its distribution
By copolyamide hot melt adhesive sample, be dissolved in above-mentioned mixed solution, be mixed with the solution that mass concentration is 0.1%-1.0%, after waiting for system balance and stability, analyze with above-mentioned chromatographiccondition, obtain molecular weight and the distribution thereof of this sample;
Described mixed solution is methenyl choloride-methyl alcohol mixed solution, and wherein, the percent by volume of methenyl choloride is 35%-65%.
2. the analytical approach of a kind of copolyamide hot melt adhesive relative molecular weight and its distribution as claimed in claim 1, is characterized in that, the number-average molecular weight scope of described copolyamide hot melt adhesive is 10000-150000, and fusion range is 95-135 DEG C.
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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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220986A (en) * | 2019-05-27 | 2019-09-10 | 浙江巨化技术中心有限公司 | A kind of analysis method of perfluorinated sulfonic acid relative molecular weight and its distribution |
| CN112798693A (en) * | 2019-11-13 | 2021-05-14 | 浙江圣兆药物科技股份有限公司 | Method for accurately monitoring molecular weight change of PLG in microsphere preparation process |
Citations (1)
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| CN102159620A (en) * | 2008-09-18 | 2011-08-17 | 三菱瓦斯化学株式会社 | Polyamide resin |
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Patent Citations (1)
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| CN102159620A (en) * | 2008-09-18 | 2011-08-17 | 三菱瓦斯化学株式会社 | Polyamide resin |
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| MARTIN B. HOCKING等: "Water-Soluble Acrylamide Copolymers. VI. Preparation and Characterization of Poly[N,N-dimethylacrylamide-co-acrylamide] and Control Polyacrylamide", 《JOURNAL OF POLYMER SCIENCE PART A POLYMER CHEMISTRY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220986A (en) * | 2019-05-27 | 2019-09-10 | 浙江巨化技术中心有限公司 | A kind of analysis method of perfluorinated sulfonic acid relative molecular weight and its distribution |
| 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 |
| CN112798693A (en) * | 2019-11-13 | 2021-05-14 | 浙江圣兆药物科技股份有限公司 | Method for accurately monitoring molecular weight change of PLG in microsphere preparation process |
| 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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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 |