High Throughput Characterization of Polyolefins by Differential Scanning Calorimetry

摘要

High throughput research (HTR) has become a key element in new product research. A wide variety ofchemical companies, including The Dow Chemical Company, have invested heavily in this technology. In HTRexperiments for polyolefin research, critical steps include making the polymer and then characterizing what hasbeen made. At The Dow Chemical Company, initial work on polyolefin characterization has been aimed atdetermining extent of conversion, molecular weight and composition. This has been successfully implemented.The next step is to include thermal analysis/characterization methods. Properties such as melting behavior, fractioncrystallinity and glass transition temperature are used to make decisions on polymer performance.In order to successfully implement a thermal method in an automated HTR experiment, four steps need tobe successful: (1) sample preparation and loading into test pans, (2) transferring the test pans to the instrument andinstrument set up, (3) performing the desired experiment including saving the data to a repository such as adatabase, and (4) automated data analysis in a manner that allows conclusions to be drawn. As part of the firstphase of characterization tools, a method for solution deposition of polymers was developed for performinginfrared spectroscopy on the samples. The method involves solution deposition into wells of a 48 cell array. Aslight modification of these arrays made them appropriate for holding DSC pans. When the samples are preparedit is necessary to transfer the sample to the DSC and set up the experiment. The robotics can easily handle loadingthe DSC autosampler. However, setting up the run sequence is still a time consuming, error-prone, manualprocedure. A commercial DSC with auto sampler and cooler is used for performing the experiments. A computerprogram developed in-house automatically performs data analysis (ex. Tg determination) as well as saves the rawdata and calculated results to a database.In this talk we will discuss our work developing procedures for HTR DSC.