Reactive pyrolysis is an exceedingly valuable tool (1) when attempting to fully characterize a complex matrix or (2) when the sample preparation itself begins to dominate the analytical method.
(1) There are many instances when the degradation products of the matrix prevent the determination of a given target compound. If the target compounds cannot be separated in time and yield overlapping ion fragments, they may be very difficult to identify and quantitate. When the target compounds can be derivatized, the derivatives can be detected and quantitated. This process can easily be implemented when using the Frontier multi-functional pyrolyzer. Microgram quantities of the untreated sample are placed in the sample cup. Microliters of the derivatizing agent (e.g., Tetramethylammonium hydroxide : TMAH) are added to the cup. The cup free falls into the furnace at an elevated temperature (ca. 350 – 425°C). The target compounds are immediately derivatized and the polymeric matrix remains in the sample cup. The resulting chromatogram is quite simple and the individual derivatives are easily quantitated.
(2) It is quite common for the sample preparation step to dominate the analytical method. Sample preparation takes the most time, requires the most resources, often is the largest source of error and clearly impedes laboratory productivity.Reactive pyrolysis eliminates the need for an extensive sample preparation step. The sample is placed in the sample cup, the reagent is added and the sample is ready for analysis. Using the Frontier pyrolyzer in combination with the Frontier auto-sampler, the process can be fully automated.
Reactive Pyrolysis (RxPY) uses an organic alkali, such as tetra methyl ammonium hydroxide (TMAH), and heat to hydrolyze and methylate ester linkages. RxPy is a useful technique for compounds with ester groups, some condensation polymers, heterocyclic N compounds.