The Tulane Center for Polymer Reaction Monitoring and ... - PSS

The Tulane Center for Polymer Reaction Monitoring and Characterization
Tulane University New Orleans, LA 70118 phone: (504)865-5087 email: areed2@tulane.edu
Website: http://tulane.edu/sse/polyRMC
The GPC course is aimed principally at current GPC users who have at least some
experience in the field and who would like to broaden and deepen their knowledge in
fundamentals of polymer characterization, detection and analysis methods, and practical issues
and applications. There will also be some instruction on polymer characterization methods that
are complementary to GPC. The first part is the 2-day class instruction outline. The second part
is the hands-on component.
The course will be given by several GPC experts and widely experienced users from both
PolyRMC at Tulane University and PSS.
Tentative PolyRMC GPC course outline.
The topics will not necessarily be presented in this order and content may change.
I. Background on polymer characterization, detection, and GPC principles
1. Polymer characterization; When is GPC the method of choice and when is it not?
Quick overview of GPC
Equilibrium vs. non-equilibrium solutions
Solutions containing microgels and other large particles
Polymers too big to be usefully separated by GPC
2. Important Polymer Characteristics
Molecular weight distributions and averages
Polymer conformations, static and dynamic dimensions
Intrinsic Viscosity
Branching
Charged polymers
Dilute and semi-dilute polymer solutions
3. Methods of measuring polymer characteristics
Concentration detectors; RI, UV/visible
Multi-angle static light scattering
Dynamic light scattering
Measurement of intrinsic viscosity
Other detectors; conductivity, fluorescence, FTIR, Mie scattering, Mass spectrometry
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4. Physical principles of GPC (SEC) separation.
II. Practical Aspects and Issues in GPC
5. GPC columns
* Column packing types and technologies
* Practical aspects on column resolution
* Column selection, use of multiple columns
* Solvents and other considerations
Multi-detector GPC demonstration I. (Topic TBA)
6. Obtaining molecular weight distributions from GPC data
* Column calibration using molecular weight standards and a concentration detector
* ‘Universal calibration’ using a concentration detector and either a known viscositymass
(Mark Houwink) relationship or a viscometer
* Light scattering detection, ‘calibration-free’ GPC.
* Comparison of the three methods, strengths and weaknesses of each, value of
combining and comparing results of the different methods.
7. Practical aspects of detectors and instruments, pros and cons:
* Refractometers, determining dn/dc
* single, dual wavelength, and diode array spectrophotometers
* single capillary and bridge viscometers
* single and multiple angle static light scattering
* Pumps, autosamplers, autoinjectors, degassers, and other hardware.
III. Special topics and applications in GPC (to be determined)
The following are possible topics, which can be omitted and added according to participant
preferences. Please fill out the questionnaire!
GPC of polyelectrolytes
GPC of natural products
Topics in aqueous GPC
Error analysis in GPC
High Temperature GPC
Branching characterization using mutli-detector GPC
GPC of specific products; polysaccharides, proteins, polyolefins, elastomers,
polyurethanes, additives
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High molecular weight polymers
Multi-detector GPC Demonstration II. (Topic TBA)
IV. Complementary and alternative methods to GPC
Automatic Continuous Mixing (ACM); Determining characteristics of multicomponent
polymer systems, polymer solutions not amenable to GPC, measuring
important auxiliary characteristics, measuring polymer dissolution kinetics.
High throughput methods.
Automatic Continuous Online Monitoring of Polymerization reactions (ACOMP).
GPC course outline hands-on outline
The hands on component of the course will focus on data analysis and interpretation, and will
also include practice in sample preparation and running GPC. Attendees will learn to distinguish
good data from bad, spot frequent GPC problems (e.g. overloaded columns, limits of column
resolution), encounter different scenarios (e.g. narrow, broad and multimodal polymer
distributions), and fully analyze data by three distinct methods; i) column calibration by polymer
standards, ii) universal calibration using viscosity detection, and iii) absolute molecular weight
determination by light scattering. The training is general and applicable to any type of modern
GPC apparatus. To facilitate the training, ParSEC software from Brookhaven Instruments and/or
other software will be used, and each attendee will have access to a computer with this software
in order to carry out all of the exercises. In addition to the intensive data analysis and
interpretation portion, PolyRMC personnel will demonstrate GPC procedures and attendees will
prepare and inject ‘mystery samples’ on their own, with their subsequent data analysis being
graded against the samples’ known characteristics.
I. GPC experimental procedure demonstrations
II.
III.
IV.
Data analysis and interpretation demonstrations
Portions III and IV are ‘self-paced’ and concurrent, with course instructors
available for questions and help
Attendee data analysis of various GPC scenarios
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