Material characterization using a Tandem micro-Reactor – GC–MS

• A novel tandem reactor GC–MS analytical technique for the rapid characterization of biomass and polymeric materials is described in this paper.
• Use Evolved Gas Analysis-MS to rapidly measure the thermal profile of a complex material.
• Using the tandem reactor GC–MS to re-generate catalytic activity in situ underscores the versatility of the tandem reactor GC–MS system.

This work illustrates how the Tandem micro-Reactor (TMR), when interfaced to a GC–MS, facilitates the rapid characterization of virtually any material: gases, liquids and solids. A TMR has two independently controlled micro-reactors in series. Each micro-reactor has three heating modes: isothermal (up to 900 °C), multi-linear (e.g., 100–400 °C at 20 °C/min) and distinct temperature steps (e.g., 100 °C, 200 °C, etc.). The TMR can be used for both Evolved Gas Analysis (EGA) and detailed component analysis. Three examples illustrate how the TMR-GC–MS can be configured to differentiate or identify virtually any material. (1) Lignin, oak, bagasse and cellulose are easily differentiated using EGA–MS – each material is analyzed directly by simply weighing the sample (<75 mesh) into the sample cup. (2,3) The temperature dependence of ethanol and methanol transformations to ethylene and propylene, respectively, are presented using an online, real-time configuration. The ethylene transformation is also performed using a series of ethanol injections at distinct catalyst temperatures. Lastly, regeneration of the catalyst’s surface is performed in-situ, which improves laboratory productive as well as elevating the precision of the data.