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approximately 5 atm, and heating the furnace to 150 °C, followed by cooling to ambient<br />
temperature. During this activation step, samples were hydrided to some extent, if not<br />
completely. Therefore, these samples were heated up to 150 °C under a minimal flow of<br />
argon to ensure no hydrogen was left in the sample.<br />
2.2.2. U-Tube Reactor<br />
A 1 foot long, 1 inch O.D. seamless stainless steel pipe was bent into a U shape to<br />
hold up to 300 grams of sample. The reactor was fitted with 0.5 micron pore size inline<br />
filters and needle valves on each end, Figure 7. The compositional analysis of the effluent<br />
gas was done by a Buck Scientific type 910 gas chromatograph fitted with a Hayesep DB<br />
100/120, 30 ft, 1/8 inch O.D. stainless steel column obtained from Alltech. The GC<br />
utilized a TCD detector and the carrier gas was argon. Samples were taken from a three<br />
neck flask connected to the downstream. Sample injection was done with a gas tight 100<br />
µL syringe. The GC was connected to a Dell GX110 PC and the data was recorded using<br />
PeakSimple chromatography software.<br />
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