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纸质出版日期:2008-4-20,
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王庆国, 李小文, 程镕时. 混合溶剂作淋洗剂的体积排除色谱谱图中溶剂化高分子峰和溶剂峰之间内在关系的理论分析[J]. 高分子学报, 2008,(4):318-324.
WANG Qingguo, LI Xiaowen, CHENG Rongshi. Theoretical Analysis of the Relationship Between Solvated Polymer Peak and Solvent Peak in Chromatograms from Size-Exclusion Chromatography with Mixed Eluents[J]. Acta Polymerica Sinica, 2008,(4):318-324.
王庆国, 李小文, 程镕时. 混合溶剂作淋洗剂的体积排除色谱谱图中溶剂化高分子峰和溶剂峰之间内在关系的理论分析[J]. 高分子学报, 2008,(4):318-324. DOI: 10.3724/SP.J.1105.2008.00318.
WANG Qingguo, LI Xiaowen, CHENG Rongshi. Theoretical Analysis of the Relationship Between Solvated Polymer Peak and Solvent Peak in Chromatograms from Size-Exclusion Chromatography with Mixed Eluents[J]. Acta Polymerica Sinica, 2008,(4):318-324. DOI: 10.3724/SP.J.1105.2008.00318.
根据体积排除色谱(SEC)研究高分子溶质优先溶剂化的基本原理,证明在SEC色谱图中被束缚溶剂产生的面积与自由溶剂产生的面积大小相等方向相反,在研究优先溶剂化时从高分子峰入手和从自由溶剂峰入手在理论上具有等价性.分析表明,通过对溶剂化高分子峰的研究,还可以得到另一个重要物理参数——恒化学位时高分子溶液的折光指数增量.
Each size-exclusion chromatography (SEC) curve generally exhibits two peaks when a solvent mixture is employed as the eluent.The first peak is the solvated-polymer peak and the second is the freesolvent peak.The area of the solvated-polymer peak A eff3 can be regarded as the sum of contributions from the naked-polymer A3 and from the extra polymer-bound solvent A1.The free-solvent peak
however
is caused by deficiency of the same solvent that enriches itself around polymer chains.Theoretical analysis shows that the size of free-solvent peak A2 and that of the extra polymer-bound solvent A1 are equal in magnitude but opposite in sign.This relationship suggests that the preferential adsorption coefficient λV can also be determined from the nalysis of the polymer peak. Polystyrene(3)-benzene(1)-methanol(2) is the system taken to test the correctness of the theoretical analysis. The polystyrene (PS) sample was purchased from Krauer Company
with Mw=9.26×104
and Mw/Mn=1.1. Solvents (analytical grade purity) were purified before use.Benzene was purified by repeatedly shaking with concentrated sulphuric acid (15 vol% benzene) in a separating funnel until the acid phase remained colorless.The benzene phase was then washed with water
aqueous sodium hydroxide (10 wt%)
again with water
dried with anhydrous calcium chloride
and finally distilled. Methanol was fractionally distilled
and the middle cut was used.The eluents were benzene-methanol mixtures of different compositions at a flow rate of 0.4 cm3/min.The mixtures were made by volume and equilibrated in the reservoir of the GPC system.The injected sample solutions were prepared using solvent mixtures from the solvent reservoir.The range of volume fraction of benzene in the eluent U10 was from 1.00 to 0.80.All measurements were conducted at room temperature with a Waters Associates model 244DS liquid chromatograph
equipped with a model R401 differential refractometer and a model 730 microcomputer.A single column packed with Styragel (nominal porosity 50 nm
length 30 cm) was employed. When a solvent mixture is used as eluent
two measurements can be carried out
with and without column in place.When there is a column in place
the polymer-bound solvent will get separate from the free solvent.The selective binding of solvent to the polymer causes polymer-bound solvent signal and the polymer signal to merge.The measured peak area is Aeff3.In the experiment without column in place
there is a direct connection between the outlet of the injector and the detector. In this situation
the chromatographic system cannot separate the components.The free solvent
polymer-bound solvent
and the solute will elute at the same time.The composition deviations of polymer-bound solvent and free solvent to the original solvent mixture caused by preferential solvation can generate signals
but
since they elute at the same time
the contributions from them to the refractive index will cancel because of their opposite response signals.In this case the measured peak area is A3.When Aeff3 and A3 are available
the preferential adsorption coefficient λV can be obtained. For the system consisting polystyrene (3) plus benzene (1)-methanol (2) solvent mixtures
the values of λV from the present work are plotted against (1-u10),together with the results for the same system reported by Hert from measurements of dialysis equilibrium and light scattering technique.The agreement of the present results with those from previous work shows that the proposed method is valid.The advantages of studying the solvated polymer peak are discussed. This method provides an alternate way to determine specific refractive index increment at constant potential (dn/dc)μ for polymer/mixed solvent systems.
体积排除色谱优先吸附混合溶剂
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