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Synthesis and characterization of polystyrene standard for gel permeation chromatography using nitroxide mediated radical polymerization (NMRP)

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Author(s):
Caroline Paganucci dos Reis Malere
Total Authors: 1
Document type: Master's Dissertation
Press: Campinas, SP.
Institution: Universidade Estadual de Campinas (UNICAMP). Faculdade de Engenharia Química
Defense date:
Examining board members:
Liliane Maria Ferrareso Lona; Reinaldo Giudici; Paula Sbaite
Advisor: Liliane Maria Ferrareso Lona
Abstract

Gel Permeation Chromatography, also known as Size Exclusion Chromatography, is the most employed technique to characterize macromolecules such as proteins, copolymers, natural and synthetic polymers. It provides information such as molecular weight distribution (MWD), intrinsic viscosity (IV) and polydispersity (PDI). The importance of its response reflects in terms of polymer processability once the mechanic and chemicals properties are drastically affected by the polymer average molecular weight, chain size and distribution. The standards in the GPC technique have a great importance to obtain reliable results because they are employed in calibration curves needed to acquire the quantitative and qualitative data. Despite the wide use of GPC in Brazil at research centers, chemical and petrochemical industries, all the standards available are obtained outside the country through high importation costs. To change this paradigm, this work aims to develop a national product using the pseudo-living radical polymerization or living free radical polymerization (LFRP), which is a robust and innovative technique in the polymerization science area. The standard chosen was the polystyrene, which is the most used polymer in calibration curves of organic GPC analysis. Our challenge in this work was to obtain a controlled structure polymer with polydispersity index (PDI) between 1 and 1.10, narrow molecular weight distribution (MWD) and high purity degree, using to the best of our knowledge for the first time a mixture of initiators in a NMRP process. The NMRP is a robust and innovative technique compared with the ionic polymerization that is the currently employed process to obtain polymers with very low PDI. The advantages of NMRP process over ionic polymerization to produce controlled structure polymers are that no complicated purification steps are needed, controlled radical reactions require less stringent conditions for impurities and working temperatures, it is a simple and cheaper process, where the reactions can be carried out into glass ampoules (AU)

FAPESP's process: 09/03986-9 - Synthesis and Characterization of polystyrene produced by Living Free Radical Polymerization to be used as standard in Gel Permeation Chromatography Technique
Grantee:Caroline Paganucci dos Reis Malere
Support Opportunities: Scholarships in Brazil - Master