Polymer samples, characterization

The terminal groups of a polymer chain are different in some way from the repeat units that characterize the rest of the molecule. If some technique of analytical chemistry can be applied to determine the number of these end groups in a polymer sample, then the average molecular weight of the polymer is readily evaluated. In essence, the concept is no different than the equivalent procedure applied to low molecular weight compounds. The latter is often included as an experiment in general chemistry laboratory classes. The following steps outline the experimental and computational essence of this procedure ... 

When a dilute solution of a polymer (c << c ) is equilibrated with a porous medium, some polymer chains are partitioned to the pore channels. The partition coefficient K, defined as the ratio of the polymer concentration in the pore to the one in the exterior solution, decreases with increasing MW of the polymer (7). This size exclusion principle has been used successfully in SEC to characterize the MW distribution of polymer samples (8). 

We have recently initiated our investigation of blends by examining the compatibility between our modified polymer sample 4 and poly(methyl methacrylate). Mixtures with a composition of between 10% and 30% of sample 4 yield compatible blends which are transparent under a polarized light microscope, and are characterized by a single Tg. Mixtures richer than 60% of 4 undergo complete phase separation. 

Table III. Conditions for Polymer Preparation and Sample Characterization"...

A given sample of polymer is characterized by a distribution of molecular weights arising from the interaction of the network of reactions shown in equation 9.3.17 (and possibly equation 9.3.18), and the mixing processes taking place in the reactor in which the polymer sample was prepared. 

Table 1. Molecular Weight Characterization of Polymer Sample...

Flocculation is indeed dependent on polymer adsorption, and there are hypotheses correlating the two phenomena, but often these have been put forth without detailed measurement of the two phenomena simultaneously (10-13). In this paper, flocculation is investigated as a function of polymer and solution properties and hydrodynamic conditions by measuring different properties of the system, including adsorption, using well characterized kaolinite and polymer samples prepared specifically for this purpose. Also, the role of concentration and charge density of polyacrylamide and polyacrylamide-polyacrylic acid co-polymers in determining kaolinite flocculation is examined under controlled hydrodynamic conditions. 

Catalyst efficiency, estimated by polymer yield, eliminated several of the potential CSAs due to their inhibition of polymerization. For those combinations that produced a sufficient amount of polymer for characterization, the molecular weights and molecular weight distributions of the polyethylene samples were then compared to control polymers prepared with no added CS A. A reduction in the Mn in combination with a narrowing of the MJMn indicated a hit for chain shuttling behavior. 

The choice of a matrix tailored for a particular kind of polymer sample is cmcial for successful characterization of the sample. Therefore, it is useful to discuss the properties of some common matrices [4—6], 3-Amino-4-hydroxybenzoic acid and POPOP need high laser power, since they possess a high threshold. Alpha-cyanocynnamic acid is... 

An example can best explain the procedure. A poly(bisphenolA carbonate) sample characterized by a broad-MMD was injected in an SEC apparatus, about 100 fractions were collected, and 24 of them were analyzed by MALDI [7]. Figure 15.2 reports the SEC trace of the PC sample. The trace covers a quite broad range of elution volumes and it is centered at about 30 ml. The polymer starts eluting at about 26 ml and ends at about 38 ml. The MALDI spectra yielded MP values (see above). Using this information, the SEC trace in Fig. 15.2 is calibrated and the average molar masses turn out to be Mw = 55,800, Mn = 23,600. 

The above flame retardants, HMPN and TMP, along with another commercially available alkyl phosphate, triethyl phosphate (TEP), were systematically characterized by Xu et al. To quantify the flammability of the electrolytes so that the effectiveness of these flame retardants could be compared on a more reliable basis, these authors modified a standard test UL 94 HB, intended for solid polymer samples, and measured the self-extinguishing time (SET) instead of the universally used flame propagation rate. Compared with the UL 94 HB, this new quantity is more appropriate for the evaluation of the electrolytes of low flammability, since the electrolytes that are determined to be retarded or nonflammable by this method all showed zero flame propa-... 

Vith the procedure outlined above, simple programs of programmable calculator (TI 59) and microprocessor (ZoO) for finding M(Vh) and <>o(%) were vrritten. The mean elution volume and total variance of the experimental chromatograms of well characterized polymer samples are first calculated according to... 

One approach to preparing polymer samples for a combinatorial study could involve using conventional laboratory synthesis methods to prepare the desired polymers one at a time. There are many studies reported in the literature where a series of polymers having some systematic variation in composition or other property were prepared and characterized. However, this approach has limitations in time and resources and becomes unattractive when the synthesis of large numbers of polymers is required. 

The polymer samples studied here fall into three distinct categories. Data from two sample populations have been combined in the SAN copolymer study. A group of SAN materials having compositions ranging from 42 (wt)% AN to 82% AN were polymerized and characterized quite some time ago (1972), with intrinsic viscosities determined only in DMF. Very recently, a second group of SAN s with compositions from 5 (wt)% to 48% AN, as well as one sample of polystyrene (0% AN), were polymerized and characterized, with intrinsic viscosities determined in DMF, THF, and MEK. These two populations are differentiated in the Results section by the designations "old data" and "new data". The third category of samples is that of S/MA copolymers and S/MA/MM terpolymers, with intrinsic viscosities measured only in MEK. 

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