back in the game

first “official” day of lab research today. winter break wasn’t all too productive…i hadn’t counted on non-reaction supplies running out while the stock room was closed, so i didn’t really have an alternate system of cooling in place for when the liquid nitrogen tank ran dry.

so, i was able to do the final workup step of my first catalyst last thursday, right before classes (a nice, off-white powder, and ~80% yeild, which is nice). today was cleanup and prep day (in between classes), along with a meeting with my advisor. thf was dried/distilled, many nmr tubes were cleaned (aqua regia, 5x water, 2x sodium bicarb, 5x water, then 2x acetone…in other words, long and involved), and the lab in general was worked on. the thf distillation surprised me today – the reflux step, which usually runs overnight, was finished in under an hour. this actually ended up throwing off my schedule for the day (i had planned on setting up and leaving the reflux, and saving the distillation/bubbling/purge-in steps for tomorrow’s lab-day. i need to just resign myself to long days of labwork this semester, especially if i want to finish this project in time.

hopefully later i’ll be able to upload the pictures i took today in the lab; the experiments were being particularly photogenic, and i got some good shots.

here’s the aforementioned photos. sorry for no funny art comments/embelishments…i don’t have my tablet with me.

first, the sodium bicarb. crystals that were growing out of the washbottle:

now, the thf distillation that kept me in lab all day:

lab days are here again…

and so, with the end of the first biochem lab (’twas a long one!), i have time once again to breathe life into my research project. sure, i’d been doing small jobs before now (distilling and drying solvents, getting glassware ready, etc), but not really getting my feet wet (so to speak).

jumped in today and already i’m a bit rusty at synthesis, after a few months away. didn’t realize that, though i had two 100ml flasks in there, i was supposed to use them in a certain order. i must have made a mental note and then promptly forgotten about it. so, at the end of it, i had a solution that needed the volitiles removed, but no readily available vacuum adapter. gotta wait until tomorrow to get that going (too late today to do so). ah, if we but had adapters of all sizes, this problem would not be an issue. 19/22, however, is the (only!) size we lack for such an adapter.

as for the experiment; i can only hope it’s going well; didn’t get far enough today to get an idea, yet. all the reagents were fresh, though (with wax seal, too!…those things are nigh impossible to open with gloved hands, though…grumblegrumble)

update later when there’s real news to report, i guess.

getting back into the game

as of today, the glovebox is (nearly) up and running again. it ran out of nitrogen since it hadn’t been used since the summer, so today was spent purging it down. it’s a very finicky piece of equipment; it spiked from 80 to 500 ppm O₂ when i just started thinking about changing out the tank before i went home.

i have a feeling it’s gonna be difficult this semester to get my research done; though i only have two other classes and a semenar class, one of those classes is biochemistry, the lab of which is currently sucking up any and all free time i have. i hope i’ll be able to give my glovebox and pretty chemicals the attention they deserve…

in other news, my poster was printed out today (by the campus print shop). it’s legible and all, but i’m not sure it’s of a quality i was expecting – there are lots of jpg artifacts and pixellation going on.

back to beginnings

spent yesterday remaking the product i did the first week of research, so i can have more to work with in the fall. it’s a very nice reaction, gives good amounts of a cheerful, yellow, fluffy-powder product. easy too – just three chemicals, a solvent, stirring overnight, then filtering. not air or water sensitive, which is a welcome change.

also had to continue with my catalyst in the box, removing the solvent by vacuum. ran into a snag in the morning, however, and took the time to clean out the dewar used for the solvent trap:

turns out a lot of ice (which condenses on everything near it) ends up falling into the dewar. it surprised me that such large chunks lasted overnight, when i know the liquid nitrogen didn’t stick around that long.

my product (which i isolated this morning) wasn’t as spectacular as the yellow fluff. despite using larger quantities, i still only have a 5% yield…very disappointing. it might be one of the chemicals that went bad, which would doom the reaction from the start…my advisor said she’d procure a new bottle for me in the fall.

hard to believe it’s the last day of summer research. i’ve been working hard all day trying to get these last few reactions to finish up, and had to fight the glovebox’s fridge to start putting some of the more sensitive chemicals away (like my tiny yield of catalyst)…found out (for future reference) that if you turn the door to the fridge counterclockwise, it loosens it up so that it will close easier. of course, that discovery was only made after i had spent 15 minutes arm-wrestling with the box…the hardest tasks seem to be in the most awkward locations.

housekeeping

finally got most everything cleaned up today, now that my two labmates are gone. i’ll have the whole lab to myself for the rest of the week, as well as the fall semester. it’ll be odd. it’s quiet, which is nice (well, as quiet as it can be with so many vacuum pumps running…), but a bit eerie. i’m most looking forward to only having to clean up after myself, and to not having to worry about all of the glassware and items i’ve painstakingly cleaned out being used up before i can start my experiment (especially the filter frits, which have to be left in the oven for a few hours before going into the glovebox).

the fume hood is finally cleared out (which makes me feel better… i had to avoid looking at it because it brought out my ocd side), we have a new empty glass disposal box, the filter frits are finally starting to shape up, and i’m finally starting to get things back to an orderly state i like. got some new (and improved?) aqua regia bubbling away in the fume hood as well, a half-batch, to finish up the cleaning efforts for the summer (hopefully we won’t have too much leftover when we’re done). it’s looking nice and bright red. made it about an hour ago, and it’s still evolving chlorine(?) gas. got the sash pulled down just in case.

run of bad luck

so, things aren’t going so well recently…

the nitrogen tank we replaced tuesday(?) is already almost gone, and we haven’t done much with it. we purged in a lot of solvents yesterday, but that wasn’t what killed it. it’s taken an unexpectedly large amount of the tank to purge the box down from 50-ish ppm oxygen, and it doesn’t want to stay down this time. it’s currently hovering near 15, but it keeps going up when we aren’t purging. i don’t like how it’s behaving, and it’s making me hesitant to do the next step in my reaction. my catalyst (so pretty!) is super-air sensitive, and i don’t want it going off as soon as i uncap it because of some personal problems the box is going through at the moment.

also, yesterday saw me in a long run of broken glassware. i managed to kill off a 1000 mL round bottom flask, a 50 mL round bottom flask, and a bottle. i have a theory that it’s because they were wet when i flame-dried them, but i’ve never had that problem before. it’s so crazy.

i’m glad i only have a week and a day left. i think i’m starting to get frustrated with this stuff.

counting chickens?

ok, this may be me celebrating too early, but i think i finally did an experiment that worked today! my product actually looks as described – pale tan colored solid. that hasn’t happened much recently, so i’m stoked (does anyone use that term anymore?). they’re actually pretty; spikey little crystals. i tried to get a few pictures, but it’s super hard to do that with it in the glovebox – i gotta shoot through two layers of glass. i might make a photopost of it later if they turn out, or just add to this post later.

in other news, had to change out the nitrogen tank (finally!) today. it’s been worrying me that it’d run out overnight, but we managed to catch it pretty much the moment it ran out (a first…we always seem to only notice it’s finally out when the oxygen count on the box starts to go up alarmingly quickly). i’m pretty proud of us for that.

in other news… also, found out that the product of the next step i’m set to do only keeps for a week (and is light, air, and moisture sensitive…great for sunny, humid, summertime florida!). as i’m only here for one more week this summer, i’m thinking i’ll just focus on making more of my spikey crystals, and stockpile them for the fall, when i have more/less time.

watching paint (thinner) dry

so, i’m at a ’sit and wait’ step in my experiment at the moment. all i have to do is keep an eye on the solvent trap and refill with liquid nitrogen as needed (and it doesn’t need a top-up often…it’s been fine for the past 2 hours or so). thankfully i only have to evaporate half of the toluene that’s in the round bottom flask, before adding some hexanes to precipitate out my product. unfortunately, i’m not sure how pure my product is; it’s still got a green color to it even after a second filtration through celite, when it should be clear. i’ll just wait for the nmr, i guess.

oxygen spike

my group has never been as happy to see an oxygen spike on the glove-box as we were yesterday. usually, we like to keep the count down to 15 ppm oxygen or less, but sometimes when we bring things into the box the number skyrockets (once to 700…not fun to fix – purging can take hours).

lately, we’ve had a run of good luck, and the count has stayed extremely low (hovering at and below 1 ppm). in fact, we’ve lately started to worry that the box was lying to us and the oxygen analyzer was actually broken (chemists: suspicious of labs going well). yesterday, though, when we brought in a slew of things from the large antechamber, the count spiked to around 50 ppm – to much rejoicing. i’m just glad i made sure to cap off my experiment. though it’s a color it isn’t supposed to be, i’d rather not corrupt it any more than it already is.

been a while…

so, my laptop bit the big one a while back (as in it got virus-ed to death) and had to be re-imaged, thus leading me to completely forget about the blog for about 3 weeks or so (i’m not sure, and i’m too lazy to check). i’ve now two and a half weeks left in my summer research, and have only just started actually working with the metal that was to be the focus of the project. it’s an odd color, but my advisor assures me that the color will come out when i filter it through celite.

nothing too exciting has happened, other than afternoon thunderstorms for the past two weeks or so. one time the power in the building actually went out for about an hour (but after the storm had ended, oddly enough. it was crazy, and i was getting paranoid about the glovebox getting compromised (it was okay). didn’t help that it happened during the week when our advisor was away at a conference.

i’m procrastinating now on filtering the reaction i have going. i guess i can filter now, and let it evaporate while i go to lunch (and probably for the rest of the day).

Edit (06.19.08, 3:24pm):

ok, filtered it and started evaporating off the toluene a few hours ago. no dice – the color stayed. as we don’t have any more frits of the right size inside the box, and the frits can’t be flame-dried, i have to wait several hours (i’m gonna save it for tomorrow to make sure the things are water-free) in order to bring the frits into the box so i can re-filter the solution. in the meanwhile, i’m trying to reduce the volume so it’s easier to work with later – less solvent to get rid of after filtration.

i have a feeling that the toluene we’re using has been compromised somehow…all of my experiments have gone wonky whenever we use it. i think my next step tomorrow will be to distill some to bring into the box… just gotta clean out the distillation set-up already in the hood so i can get ready tomorrow.