MDSC parameter optimization for the determination of glass transitions using a Design of Experiments approach

Optimum experimental parameters for modulated differential scanning calorimetry were determined using a Design of Experiments approach. Two different strategies were tested, an isothermal method only varying modulation period and amplitude and a non-isothermal method including an underlying linear heating ramp. Three different test compounds were investigated including a blank of NaCl, a small pharmaceutically active molecule (Valsartan) and a polymer (PVP-VA 64).Obtained optimum values were found to be identical for each compound tested and shown to be statistically robust for repeated daily experimentation. Optimized signals showed lower glass transition values Tg paired with higher changes in isobaric heat capacity Δcp. Measured glass transition signals exhibited minimal variation during repeat analysis, and showed significantly better signal-to-noise ratios in comparison to literature data.

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