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The development of reliable sample preparation methods has been critical to the success of matrix-assisted laser desorption/ionization (MALDI) mass spectrometry experiments. Good MALDI sample preparation for polymers involves choosing the solvent system, the matrix, and the ionization agent correctly, and combining them in a manner that will lead to a sample that will produce the desired ions. The vast diversity of chemistry available in industrial polymers has challenged our ability to design reliable sample preparation methods. In the experiments reported here, we show that matrix-enhanced secondary ion mass spectrometry (MESIMS) is an effective analytical technique to explore sample segregation in solid phase MALDI samples. Qualitative comparison of MESIMS and MALDI results for polymer samples prepared with multiple matrices aids our investigation of the solid-phase solubility of a variety of low molecular weight polymer materials. Including the solid-phase solubility with the liquid-phase solubility of the polymer samples and the matrices enables the construction of a relative solubility chart, which shows the best solubility matches between the polymer and matrix materials for MALDI experiments

Using MESIMS to analyze polymer MALDI matrix solubility