Combinatorial Science - Polymer Screening
The polymer screening step in the workflow involves testing products of polymerization experiments to determine if reactions occurred as expected and characterize polymer properties that may impact final product performance.
Symyx Rapid GPCTM is a high throughput method for characterizing polymer molecular weight and molecular weight distribution. This system includes a sample preparation system that is used to dilute the polymer samples and inject the samples into the GPC system. The sample preparation system has heated liquid dispensing pipettes for handling viscous polymers. The GPC system uses high-speed columns and an evaporative light scattering detector. Samples can be analyzed in as little as 10 minutes.
The system can identify the molecular weight of a compound based on its retention volume and has a molecular weight range from 162 – 15,000,000 depending on columns and standards used.
The Bruker Optics' Vertex 70TM FTIR spectrometer with HTS accessory rapidly analyzes polymer compositions. Samples are deposited on a 96-position silicon wafer for mid-IR transmission experiments or onto an aluminum substrate for diffuse reflection experiments.
The detector used in diffuse reflectance experiments is liquid nitrogen cooled to maximize the sensitivity. The cabinet is also purged with dry nitrogen to minimize water and CO2 interference.
In addition to the standard substrates, the autosampler tray and software can be modified to receive almost any array format. The HTS autosampler allows for many coating samples to be analyzed in a single experiment.
OPUSTM and OPUSLabTM software from Bruker allow for easy data workup and experiment control with many options available to manipulate the spectra.
The TA Instruments Q1000 modulated DSC, with autosampler, characterizes polymer samples for thermal properties such as glass transition temperature (Tg) and crystalline melting point (Tm).
The Agilent GCMS characterizes products of polymerization reactions. For instance, unreacted monomer content can be measured to determine polymerization kinetics. The mass spectrometer is equipped with Electron ionization (EI) and has a mass range of 1.6 to 800 amu. This system is also equipped with a 100 sample autosampler for automated sample introduction and an automated data system for instrument control, data acquisition and analysis. It also contains an electronic library for unknown compound searching and identification.
An Agilent HPLC is used to characterize the products of polymerization reactions. The system contains a 100 vial autosampler, pumping system, differential refractive index, ultraviolet, and fluorescence detection. A fraction collector is also available for concentrating reaction products for further characterization. The Agilent 1100 HPLC is an automated liquid chromatography system and is equipped with solvent degasser, quaternary pump, and temperature controlled column compartment. This system can also be used to purify synthesis products with its fraction collection module.
A 400 MHz NMR equipped with an autosampler is used to characterize polymer systems for their chemical structure.