Laptop troubles

once again, i’ve managed to kill off my laptop. the poor thing has been through so much with me. this time it’s virus(es). it must have been the email i opened, but that’s besides the point.

i have two and a half days to talk about, but not too much has happened of note. time has mostly been spent trying to distil some thf so that the next experiment will run smoothly. used the sodium+ benzophenone under nitrogen method, then had to start over due to a leak in the distillation setup that allowed air (and therefore moisture) to enter the system, probably overnight. hopefully the rest of this goes off smoothly, and we can start up a second batch before the end of the day – i really don’t feel like bringing in the two batches of solvent separately, when we have to use the large antechamber. it’s annoying to use, and i like to use it (for solvents especially) as little as possible.

other than that, i’ve been running some control tests for temperature, to make sure that the substances i’m working with don’t spontaneously react without the catalyst.

spiking the glove box

had to bring a lot of stuff into the box yesterday (including solvents that i probably won’t end up using…), which ended up spiking the oxygen count on the box…i still don’t like messing with the large antechamber. today i’m gonna end up purifying the thf we’re gonna use to get all the water out of it (in theory). i hope the professor stays with while i do the first one…i don’t like trying to figure out these things on my own – things tend to explode around me.

i did learn how to pump-thaw-freeze a solvent yesterday (to get rid of air). did it on the deuterated benzene to bring it into the box. it was actually pretty fun, and not too much chance of exploding.

i’m ready for the long weekend coming up, though.

wash wash wash

mostly spent the day filtering and washing products…took some nmr spectra, also (at the very end of the day). hadn’t had a chance to look it over yet. i feel like i’m falling behind a bit, like i was supposed to have this step finished a week ago or so. i can’t help but feel slightly unrushed, as i know i have the fall semester to work on this project as well. though i know this isn’t likely to happen, i don’t wanna run out of stuff to do before i finish out the fall semester.

not much eventful happened today, not looking forward to tomorrow (working in the box, involving bringing in solvent).

schlenk line, decoded

so…condensed version:

found out that i was using the line improperly, and that there was a difference between which side of the knob was up (which makes sense since you can choose for either vacuum or nitrogen). so the snafu earlier this week which i thought involved crazy nitrogen pressure things actually involved me turning on the vacuum.

anyhow, yesterday…yesterday involved drying the redone first step, and moving both that and the thing i made last week (the bright yellow stuff) to the next step. it’s insanely titchy stuff, those addition funnels. couldn’t manage to get them to drip as slowly as i’d like. just when i’d get it nice, something would happen and it’d slow down and stop.

by the end of the day, the other two people in the lab headed off to dinner (the chamber had to repurge after we brought in some solvent), and i was left to continue the dripping. ended up staying after by two and a half hours, since i had to deal with the nitrogen tank running out (and the connected problem of finding the teflon tape, when all the rooms were closed up…i got lucky with some i found in the professor’s side laboratory). i felt accomplished, but tired. i think i’m gonna try to head out a bit early today to meet up with a friend i haven’t seen in a while. i think i’ll spend the day drying the products from yesterday.

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.

more exploits with vacuums

learned not to pull a full vacuum on any closed container today, after making a bit of a mess with a round bottom flask filled with drying agent and capped with a septum…i’ve learned now how to deal with bringing it into the glovebox.

still haven’t gotten the hang of the schlenk line, though. need to ask about it. seems like trial and error at the moment, plugging things up and turning things until the desired output happens.

mostly, though, spent the day drying out the disaster of a product from yesterday’s experiment. i’ve yet to do an nmr of it (that’s for tomorrow), so i’ve no idea whether it’s good or not (i’m leaning towards not, as it’s brown, and it’s supposed to be a light tan color). tomorrow’ll probably be spent remaking the precursor to the disaster, and bringing forward the second compound (hopefully both will be okay to react over the weekend, as they’re supposed to be overnight reactions…).

catastrophy strikes!

so…bringing the compounds forward one step took a turn for the worse today. still not sure what happened. i guess i don’t understand the schlenk line after all. some sort of pressure build-up happened, and the solution in my round bottom ended up getting sucked into the addition funnel. suffice it to say, the solution was not supposed to turn black. i’m trying to continue the experiment, but i’m pretty sure i’ll have to restart that part of it (thankfully, the first step was pretty easy).

really tired today, so i’m just gonna head off to bed now.

not all vacuums were created equal

feeling pretty tired…gotta get used to full days in lab again – walking around, standing a lot, and focusing on the experiments.

today wasn’t too busy as far as experiments go…we’re still getting started on stuff. only really managed to filter and dry (mostly) the precipitates from yesterday. i had two runs going at the same time, so i ended up taking over the analytical lab to use the water aspirators. turns out the one i used for my first compound wasn’t all that powerful, or maybe i used too much methanol to wash with, because even though it dried for way longer than my second compound, the nmr scan showed a lot of methanol still in the sample (that, and the over 100 percent yield clued me in to my problem). it’s sitting in the vacuum antechamber at the moment, overnight, to get rid of any leftover solvent. seemed to be working when we checked a while after we put it in – it looked noticibly fluffier, and was lighter in color. i probably should have put my other compound in too, for good measure, but there wasn’t any indication of methanol on the nmr scan.

tomorrow will be a fight over who gets to use the new thermo-controlled hotplate…and will test my patience, since i’m uneasy around heat. i just need to learn how to deal with it.

other notibles: learned how the schlenk line worked (and actually understood it this time), learned how the nmr-tube cleaner worked (sort of…as long as it’s already hooked up to whatever the hose runs off to), prepped stuff for tomorrow by cleaning and putting in the oven

first day

managed to jump straight in today…

cleaned out the glovebox (or rather, watched the two (relative) tyros do so, though i ended up being the one to switch out the nitrogen tank on the thing (twice!) since it went empty…probably will end up doing it again tomorrow…we go through so much nitrogen.

most of the experiment leftovers from last summer got dumped into a waste bottle, which after a while ended up bubbling, then smoking violently (brown nastiness which made us close it up in the hood with the blash shield down).

i got to make aqua regia today (3 parts nitric acid, 1 part hydrochloric acid, for future reference…okay, according to wiki and a few other sources, it’s 1 nitric to 3 hydrochloric…need to double check this), was nice and dark red, and a bit foamy.

spent lunch in the chemlounge watching tv, which was lazy of me.

got my smart key updated to include many of the rooms on the floor that i’ll need access to during the summer…don’t know if they’ll let me renew it for the fall (i probably won’t need it, though, come to think of it).

hmmm…what else…

started the first experiment today, making one of the precursors to the ligands, which is the precursor to the catalyst. it was pretty simple experimentally; just adding stuff together and stirring overnight. i had to do a double batch, as i’m making both catalyst types…one’s bright yellow, and the other is bright goldenrod (more towards orange, but still pretty yellow). left them on a couple of stirring plates in the professor’s side lab. hoping they’ll still be stirring tomorrow, and not a big hunk of mess at the bottom of the round bottom. i added extra solvent at the end to help out, not sure if it was enough.

tomorrow should be interesting. at least we have a concrete plan of action this summer, which is refreshing and wonderful.

introduction…lit review…

so, starting out with the researching…and the reading…and the writing…

and, let’s face it, the boring. messing around in lab is fun, reading about stuff…not so much.

i guess, to be fair, this stuff is pretty interesting; it just doesn’t cut it on a relativistic scale. like they keep saying – independent study is the easiest thing in the world to blow off. i gotta force myself to sit down to read/write about it, and it seems that the smallest things can distract me (especially with how dense some of these articles are – it seems like the fewer the pages, the more work it takes to get through them). i got most of my work done today in the few hours before my tutoring job (in the tutoring center)…seems like the only place i could concentrate the slightest bit today.

anyway….more topic-oriented. gonna meet with my sponsor(?) tomorrow to talk about what i’ve written so far (which amounts to an embarassingly small incomplete first draft)….hopefully won’t take too long…too much other stuff to work on.