Simultaneous measurement of the molecular weight distribution and 5-ethylidene-2-norbornene content across the molecular weight distribution of ethylene-propylene-diene terpolymer via a new size exclusion chromatography-ultraviolet-refractive index method

被引:0
作者
Zhou, Z. [1 ]
Janco, M. [2 ]
Cong, R. [1 ]
Lee, D. [3 ]
Shan, C. Li Pi [1 ]
Boopalachandran, P. [1 ]
Shi, Z. [1 ]
Miller, M. D. [1 ]
Winniford, B. [1 ]
Huang, T. [1 ]
Herceg, E. [4 ]
Salazar, I. [1 ]
Pangburn, T. [3 ]
Sandlin, A. [1 ]
Fan, L. [1 ]
Wu, J. [2 ]
机构
[1] Dow Chem Co USA, Freeport, TX 77541 USA
[2] Dow Chem Co USA, Collegeville, PA 19426 USA
[3] Dow Chem Co USA, Midland, MI 48667 USA
[4] Dow Chem Co USA, Union, KY 41091 USA
关键词
copolymers; elastomers; polyolefins; properties and characterization; separation techniques; DIFFERENTIAL-OVERLAP TECHNIQUE; GEL-PERMEATION CHROMATOGRAPHY; TRANSITION-METAL-COMPLEXES; ABSORPTION CROSS-SECTIONS; ONLINE SEC-NMR; INTERMEDIATE NEGLECT; POLYPHENYLENE SULFIDE; DENSITY; SPECTROSCOPY; FRACTIONATION;
D O I
10.1002/APP.43911
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
A size exclusion chromatography (SEC)-UV-refractive index (RI) method was developed to measure the 5-ethylidene-2-norbornene (ENB) content across the molecular weight distribution (MWD) in ethylene-propylene-diene terpolymer (EPDM) at room temperature. The ratio of the UV and RI signals at the same effective elution volume was converted to ENB content. The feasibility of using this method to measure the ENB content across the MWD in EPDM at high temperature was also demonstrated. Prior understanding was that ENB had insufficient UV absorbance relative to high-temperature SEC solvents to allow for useful measurements. We demonstrated this by using high-boiling-point solvents, such as decalin, with a low UV absorbance in the UV wavelength range of interest for ENB. These solvents also gave rise to a high enough specific RI increment (dn/dc) for EPDM that a suitable RI detector response was obtained. Additionally, this methodology could be readily applied to other polymers soluble at high temperature as long as the polymers contained a UV chromophore. These include polymers containing vinyl, conjugated vinyl, aromatic ring, carbonyl, or halocarbon groups. This UV-absorption-based detection concept might also be extended to high-temperature thermalgradient interactive chromatography-UV, high-temperature solvent-gradient interactive chromatography-UV (high-temperature liquid chromatography-UV), temperature-rising elution fractionation-UV, crystallization analysis fractionation-UV, and crystallization elution fractionation-UV. (C) 2016 Wiley Periodicals, Inc.
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页数:11
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