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Dual Detection High-Performance Size-Exclusion Chromatography System as an Aid in Copolymer Characterization

机译:双重检测高性能尺寸排阻色谱系统有助于共聚物的表征

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Compositional heterogeneity is one of the essential factors controlling the physical and physico-chemical properties of copolymers; its determination is in most cases a rather difficult and challenging scientific task. The overall composition of a copolymer comprising two kinds of repeating units can be determined as a function of molecular mass by the dual detector high performance size exclusion chromatography (HPSEC) technique. The common combination of the refractive index (RI) detector with the UV spectrophotometer can be applied if at least one of the monomer units absorbs at a suitable wavelength and if the UV-spectra of both components are sufficiently different. In this paper, synthesized random copolymers of styrene and methyl methacrylate were dissolved in tetrahydrofuran and characterized by the RI-UV HPSEC technique, at the UV wavelength of 254 nm. Home made software and a corresponding hardware interface were used for the equipment control, data acquisition, data processing and calculation. The obtained results show that the technique is capable for fast, routine determination of average copotymer composition. There is no significant variation of chemical composition with molecular mass for investigated copolymers with Lower polystyrene content. For copolymers rich in polystyrene, chemical composition varies with molecular mass. In this case, calculated apparent mass fractions of styrene may exceed 100%, and this is explained by the presence of small quantities of low-molecular-mass styrene homopolymer.
机译:组成异质性是控制共聚物的物理和物理化学性质的重要因素之一。在大多数情况下,其确定是一项相当困难和具有挑战性的科学任务。包含两种重复单元的共聚物的整体组成可以通过双检测器高性能尺寸排阻色谱(HPSEC)技术确定为分子量的函数。如果至少一个单体单元在合适的波长下吸收并且两种组分的紫外线光谱足够不同,则可以使用折射率(RI)检测器与紫外线分光光度计的通用组合。本文将合成的苯乙烯和甲基丙烯酸甲酯的无规共聚物溶解在四氢呋喃中,并通过RI-UV HPSEC技术进行表征,紫外波长为254 nm。自制软件和相应的硬件接口用于设备控制,数据采集,数据处理和计算。获得的结果表明,该技术能够快速,常规地测定平均共聚物的组成。对于具有较低聚苯乙烯含量的所研究的共聚物,化学组成随分子量没有明显变化。对于富含聚苯乙烯的共聚物,化学组成随分子量而变化。在这种情况下,计算出的苯乙烯表观质量分数可能超过100%,这可以通过少量的低分子质量苯乙烯均聚物的存在来解释。

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