Polymers are important materials for sensor, microfluidic, and other demanding applications. High-throughput screening methodology has been applied for the evaluation of the solvent resistance of a family of polycarbonate copolymers prepared from the reaction of bisphenol A (BPA), hydroquinone (HQ), and resorcinol (RS) in different solvents of practical importance, such as chloroform, tetrahydrofuran (THF), and methyl ethyl ketone (MEK). We employed a 24-channel acoustic-wave sensor system that provided previously unavailable capabilities for parallel evaluation of polymer solvent resistance. This high-throughput polymer evaluation approach assisted in construction of detailed solvent-resistance maps of polycarbonate copolymers and in determination of quantitative structure-property relationships. The best absolute solvent resistance of all studied copolymers was achieved in MEK, followed by chloroform and THF. A D-optimal mixture design was employed to explore the relationship between the copolymer compositions and their solvent resistance. The applied special cubic model for each solvent took into account the primary mixture terms such as BPA, HQ, and RS; binary interaction terms such as BPA-HQ, BPA-RS, and HQ-RS; and a ternary interaction term BPA-HQ-RS. A combination of the normal distribution of the model residuals and the very high values of adjusted R-2 (0.97-0.99) demonstrated a good quality of the model. At a HQ concentration of 40 mol %, the solvent resistance was the highest for all tested solvents, and different concentrations of BPA (40 and 60 mol %) and RS (0 and 20 mol %) did not affect the solvent resistance. Without HQ, solvent resistance was decreasing with an increase of RS and decrease of BPA. Overall, with an increase of HQ concentration from 0 to 40 mol %, the solvent resistance of BPA-HQ-RS copolymers was improved by up to 3 times in THF, by 21 times in chloroform, and by 32 times in MEK.

Phosphorus in different forms is used in a variety of applications (catalysts, thermal stabilizers, flame retardants) in polymeric formulations. It is important to be able to determine its concentration in raw materials, intermediates and final products. The challenge of measuring low concentrations of P, combined with the volatility of the organic phosphorus compounds, has been solved through a novel analytical procedure with a method detection limit of 0.4 µg g−1 P (10σ). The volatilization of organic P compounds was prevented by pre-oxidation with periodic acid, which allows ashing in the presence of magnesium acetate while maximizing the weight to final volume ratio. Using factorial design of experiments, experimental factors including ashing temperature, time, and the amount of the reagents were optimized with respect to accuracy and precision of the technique. The influence of Ti when present in the samples was eliminated by complexing it with H2O2. Additional pre-treatment with NH4OH was found to improve recovery for some reactive samples. Comparison with other established methods was carried out and is discussed.

Solvent-resistant polymers are important in numerous research, engineering, and consumer applications. To address the limitations of existing methods of evaluation of polymer solubility and solvent resistance, we developed and built a 6 x 4 array of resonant acoustic-wave sensors operating in the thickness shear mode (TSM). The application of this system makes possible analysis of nanogram quantities of polymers in small amounts of solvent and permits the simultaneous analysis of multiple samples, such as those produced in combinatorial polymerization reactions. These parallel determinations of polymer/solvent interactions eliminate errors associated with serial determinations. During the periodic exposure of the TSM crystals to polymer/solvent combinations, the mass increase of the crystal is determined, which is proportional to the amount of polymer dissolved and deposited onto the sensor from a polymer solution. We demonstrate our sensor system for reliable quantification of solubility of several types of polymers in various solvents. The high mass sensitivity of our resonant TSM sensors (10 ng), use of only a minute volume of a solvent (< 2 mL), and parallel operation (matching a layout of available 24 well plates) make this system a good fit with available polymer combinatorial synthesis equipment.