Physical Sciences Laboratory (PSL)
Catalyst formulation and materials processing: synthesis of heterogeneous catalysts on metal oxide or carbon supports; synthesis involves examples of both base metal and precious metal catalysts with both single metal and bimetallic catalysts; processing of carbon materials for improved supports; fume hoods for preliminary chemical synthesis experiments. The catalyst materials produced in this laboratory are then used in processing tests, usually first in batch reactors at CEL or EMSL and then continuous-flow reactors at CEL or CPDL.
This state-of-the-art integrated system for high-throughput experimentation allows both preparing catalytic materials and performing primary screening tests of heterogeneous catalysts (combinatorial catalysis). With it we can test in aqueous phase conditions with gas addition for development of new processes for conversion of biomass to fuels and chemical products in support of our DOE-EE Office of the Biomass Program customer. It is a complete "flow" parallel processing catalyst evaluation system designed and built by the leaders in the field, Symyx Technologies, Inc.
The processing components include:
- three robotic systems for heterogeneous catalyst synthesis using 96-well plates (approximately 1 milliliter volume each), one each for
- solids loading,
- solution impregnation and feedstock addition, and
- solution makeup and product recovery for analysis;
- calcining and reduction furnaces and the processing vessels, and
- a 4 x 96-well high-pressure reactor (HIP).
The HIP design allows operating conditions at up to 1500 psig @ 200°C. The reactor will have gas feeding capability and have the vortex agitating system for good liquid-solid mixing and gas dispersion.
Lab-scale reaction engineering and chemical analytical support: two gas chromatographs with flame ionization detector and electron capture detector; fume hoods with reactor systems. Low-pressure process tests can be performed in this lab. The gas chromatographs support process development in the analysis of volatile organic products.
Materials Characterization Lab
Chemical analysis support: 3 liquid chromatographs with refractive index detectors and evaporative solids light scattering detector; FT-IR spectrophotometer unit with temperature controlled and flow-through cells. The liquid chromatographs support process development in the analysis of non-volatile products. The FT-IR is particularly useful for chemical functional group analysis for process monitoring.
Chemical process development and chemical analytical support: UV-Vis spectrophotometer unit; fume hoods for preliminary chemical synthesis experiments and homogeneous catalysis. Low-pressure process development work can be done in this lab. The UV-Vis is also useful for organic chemical bonding analysis for process monitoring.
Nuclear magnetic resonance laboratory: Three systems with tunable probes for multiple nucleus analysis and solid state analytical capability. The three units are a Varian 300S, a Chemagnetics 300, and a Chemagnetics100 system. We have developed our analytical expertise with these systems particularly in the area of monitoring individual sugar monomer types and specialty vegetable lipid compounds.
Bioprocessing development: including the establishment of standard methods and performing experiments in the 1.25-liter and 2.5-liter computer-controlled New Brunswick fermentors.
The installation of additional capacity is ongoing, including a 30-liter B.Braun fermentor.
To model airlift processes, a bubble column was acquired and validated, and the initial process design established for an A. niger citric process. Other experimental equipment includes a multi-well plate reader, an enviromental-controlled shaker, and an ambient shaker. All of this equipment allows process development in bioprocessing systems from initial organism characterization to continuous fermentation process development, optimization, and scale-up.
Two autoclave systems for disinfecting bioprocessing equipment and a walk-in refrigerator for storage of samples.