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Synthesis and Characterization of polystyrene produced by Living Free Radical Polymerization to be used as standard in Gel Permeation Chromatography Technique

Grant number: 09/03986-9
Support type:Scholarships in Brazil - Master
Effective date (Start): August 01, 2009
Effective date (End): July 31, 2011
Field of knowledge:Engineering - Chemical Engineering - Chemical Process Industries
Principal researcher:Liliane Maria Ferrareso Lona
Grantee:Caroline Paganucci dos Reis Malere
Home Institution: Faculdade de Engenharia Química (FEQ). Universidade Estadual de Campinas (UNICAMP). Campinas , SP, Brazil


Gel Permeation Chromatography (GPC) as know as Size Exclusion Chromatography (SEC) is one of the most used techniques to separation e characterization of natural and synthetic polymers, copolymers and proteins, providing information about molecular weights and molecular weights distribution. In the GPC technique the standards used are of critical importance, because they are used to build the calibration curves. Spites of the intense utilization of GPC technique in Brazil, the standards commercially available are all obtained from out of the country, involving importation at high costs. In order to change this paradigm, this project proposes to develop a national product using an innovative and robust technique. As case study the polystyrene is considered, because it is one of the most used standards in organic GPC.One of the challenges involved in obtaining standards for GPC is to obtain polymers with polydispersity (PDI) very close to one, with narrow molecular weight distribution and high pureness. In this project the living free radical polymerization as known as controlled free radical polymerization will be used to produce the polystyrene. As controller it will be used TEMPO (2,2,66- tetrametil-1-piperidinoxil) and as initiator it can be used either TBEC (tert-butilperóxido-2-etihexil carbonato) or BPO (Peróxido de Benzoíla). In previous work developed by our group it was observed that TBEC is able to produce controlled polymers at higher velocity, however, the BPO initiator usually produces polymers with PDI closer to one.It will be produced polymers with different molecular weights (from 10.000 to 500.000), in order to build a calibration curve (12 points). The characterization of the produced polymer will be performed by using a triple detector GPC, with refraction index, light scattering and viscosimetric. After the characterization, the analytical method will be validated, in order to check the quality of the measurements in terms of selectivity, linearity, operation range, detection limit, quantification limit, precision and robustness.

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Academic Publications
(References retrieved automatically from State of São Paulo Research Institutions)
MALERE, Caroline Paganucci dos Reis. Synthesis and characterization of polystyrene standard for gel permeation chromatography using nitroxide mediated radical polymerization (NMRP). 2011. Master's Dissertation - Universidade Estadual de Campinas (UNICAMP). Faculdade de Engenharia Química.

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Filed patent(s) as a result of this research project

KIT DE PADRÕES DE POLIESTIRENO PARA CALIBRAÇÃO DE CROMATOGRAFIA DE PERMEAÇÃO EM GEL (GPC), PROCESSO DE OBTENÇÃO E USO DO BENEFÍCIO KIT PI1103568-4 - Universidade Estadual de Campinas (UNICAMP) . Liliane Maria Ferrareso Lona; Caroline Paganucci dos Reis Malere - July 2011, 29