vacuum pumps are messy little things
i’m trying not to be so repetetive here, but these vacuum issues continue to slow things down. today we found out just how powerful our little vacuum was – it was able to suck the (taped on!) septum off of two round bottom flasks filled with solvent. we were trying to bring them into the box, and erroniously thought that they’d be fine under full vacuum. since we had to let some glassware (also inside the chamber) cool off from the oven, by the time we found out what had happened, half of the thf and some of the toluene had got sucked into the vacuum pump (which explained by the smell that stuck around). when we tried to re-evacuate the (empty) antechamber, a small explosion (for lack of a better description) happened, and vacuum pump oil (mixed with thf and who knows what else) flew out of the pump and sprayed everywhere, freaking us all out, but somehow managing to miss hitting any of us. thanks to our professor’s experience, we were able to easily clean up the mess with hexanes. the stuff worked wonders – i’d recommend it highly as a grease-cutting agent, but i’m guessing no one wants that stuff near their dishes). from there, we just had to call up the resident technology/mechanical go-to guy to help us replace the oil (which badly needed it…it was a brown color, like dark maple syrup, instead of the light golden-honey color it was supposed to be. draining the thing was another ordeal, in which the pressure of the liquid caused it to shoot out and miss the beaker we had set out. eventually we got the pump cleaned out, refilled, and it’s currently up-and-running.
besides that, and restarting the experiment from day one (since i killed the second step on wednesday), today was pretty much a bust as far as the experiments go. only other accomplishment was replacing the nitrogen tank (which we did all by ourselves!). as our professor says, if all research went according to plan and went right the first time, people would be able to get their phd’s in two years; these types of setbacks are what make the process take five years.
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