not all of our posts have actual content!
March 24th, 2008 by Ψ*ΨAs awesome as it was to see some actual, relevant discussion–on a device post!–by people who know much more than I do…I’m out of energy, so shiny pictures will have to suffice. Better pretty colors than no post at all, right?
As very few readers know, several hoods in my lab are broken. Mine is no longer one of them–it was actually fixed–but the 2×4 OF SCIENCE is, sadly, still in rotation. If only we could get these things repaired within a reasonable time frame![1] Until then, they’re cleared out and waiting. Unfortunately, clearing them out meant taking everything out of them and finding new homes for whatever happened to be occupying that space. And one of the things occupying that space–surprise!–was our ether still.
It has found a new home. In my hood. This wouldn’t faze me too much, except…
1) ether stills can go KABLOOIE, and
2) dude, where’s my nitrogen…? Or…what? another electrical outage? No telling when that could happen again.
As my labmates happily informed me, “You weren’t there to protest.”[2]
On a happier note, here’s some green stuff I found below the columnator. I have an inkling as to whose it is and maybe, sorta, kinda what it might be, but…no telling for sure.
[1] …Oh, wait, we’re not in the College of Medicine. Damnit!
[2] They couldn’t have known that for certain. We ninjas are invisible when we so choose, after all.
Everyone should run their reactions under ambient conditions no matter what!
what
I mean that I’d prefer a reaction that does not require absolute solvents over the one that does.
Was that a still that was out of use for a long time? You might want to test it for peroxides…since it’s in your hood!
Well atleast you aren’t like the postdoc I knew who was rotavapping really old THF which exploded embedding shards of glass in the ceiling and breaking the stone lab bench!
You could always use your ninja powers to ensure safety.
i wantz a purple ether still!! blue is suspect imo.
if it has benzophenone ketyl color there then there are no peroxides. Ketyls gobble up your peroxides and oxygen and moisture. Even your mother in law is no match for them/
That stir-plate is sexy.
From this and all of the other lab pictures you have posted, your labs look like a lab ghetto. How many elements were on the periodic table when your labs were built?
I too have spent many years working in labs that required “2×4 of science” type of modifications. I wonder what I’m going to die of. Cancer? Heavy metal poisoning? Hood sash decapitation?
Little known fact…our labs actually pre-date Mendeleev.
And how ’bout some pictures from this weekend? Hmmmm?
Look, what happens not on the internet stays not on the internet.
unless it’s on facebook. just saying. they will be facebooked at some point but no wai i’m putting them up here.
IAWTC
Our building is most definitely ghetto. I wish I could still get into the biomedical research building–it would be quite informative to show photos from there beside some from the chemistry building.
I should mention that the broken hoods got fixed today! Much sooner than we thought it would happen.
For the record, the hood walls were like that when I got here. The CEILING…yeah, that’s my fault, but I’m definitely not tall enough to reach and clean it. One super-angry large-scale Grignard quench is all it takes to understand the meaning of “dropwise.” Anyone else out there use PEG for oil baths? Does it turn brown after you use it for a while?
I have two stills in my hood….one is for THF or dioxane, and the other is rotating, DMF, DMAc, DCM or, when times are tough, acetone recycling. But, at least I can see what colour the walls of my hood are, and if I have a flask in the oil bath.
While still on the topic of lab safety..read this Yahoo news report.
I understand construction workers being on top, but where the hell are the researchers i.e chemists, biologists, medchem people?!!!
” strain injuries from typing as well as illnesses from inhaling toxic printing inks and other substances.”!!
What about dying from cancer from working with toxic chemicals all day (876341 billion hours a week if you’re a grad sudent)?
Or having this happen. There are worse fates than cancer…
LOL, organics.
BTW, I’m going to be done with my 395 research on Friday.
Wanna try to grow some crystals?
Well…I kinda did that already. They just didn’t get along so well with the x-rays, for various reasons. I just wish I knew why the last ones didn’t diffract.
How do you get a purple ether still like that? I keep loading benzophenone into mine after refills and I can never quite get the same purple color as I once got. it just turns kinda greenish or something. Keep adding more benzophenone? The still def. has sodium in it…. I can see the metal float around while it refluxes.
greenish? yikes!
“can never quite get the same purple color as i once got.” umm…how old is the still and how many times have you had to refill it?
btw, the still in the pic is NOT purple. i’ve seen purple stills…so beautiful.
We has a THF still that’s right next to my hood (DO NOT WANT) but it’s always nice and blue and bone-dry. (We know this due to the lab’s Karl Fisher titrator- frankly, we’ve found that purple is overkill. Dark blue is good. It’ll be dry enough for synthesis and if you need it really air-free, then you’ll end up having to freeze-pump-thaw it anyway)
i didn’t say it wasn’t overkill…i said it was beautiful
your point about air-free reactions is valid. the impression i always had is that blue is definitely dry and purple is definitely oxygen free. still, i can’t imagine anyone can truly keep it oxygen-free between the time they syringe it out and take it to their reaction.
i’m at an undergrad institution right now, and i don’t think we have any sodium, much less a still. even bone-dry stills seem like overkill to me now, but i miss the security of them at times..
still, that still is not purple!! if you’ve seen the purple, you know.
Ours was a perfect dark blue when it was first set up. A little green isn’t as frightening as the ugly tan color our THF still used to turn.
There is difference between color of ketyl in ether and ketyl in THF. If I remember correcty the ether is more purplish whereas THF is blue. It can turn more greenish as yellow brown gunk accumulates.
A smart guy who was in charge of stils in the group (Mike Grogan) found out that he could buy ready-made sodium dispersion in parrafin wax which does not catch on fire on moist air and is easy to cut like chocolate – and the ketyl color turns on immediately because of the huge metal area. Parrafin from the dispersion does not contaminate the distillate and the leftovers in the stills are actually safer to quench
Our group’s used the paraffined Na for years- works great. At my undergrad we used potassium instead of sodium… and I was in charge of the THF still. Seems that nowadays, I’m not scared of much in lab, compared to how terrified I was of the impending fireball of doom that was my recharging the THF still. (And sodium works better anyway, I think- the still seems to stay dry much longer. I mean, this was in Arizona, dry as a bone, and we still had to add potassium quite frequently.)
He was smart. Have you talked to Mike since you left?
no I have not – I admired the guy though he was always reserved
He was kind of quiet, but smart (he finished his cumes before everyone else, though I don’t know his research). I just hadn’t heard much about him (surprise).
If I remember correctly his thesis was on cyclic guanidine organocatalyst, for asym Strecker. This work was done long before Jacobsen
I have found that when the ether or THF is predried over solid KOH makes the difference in whether the blue/purple color lasts at least a week (often much longer) or a couple days. Make sure that the solid doesn’t start to break down in the holding container or else it inreases the nice coating of whatever the yellow shit is that builds up on the wall of the flask once it is added. Our sodium comes in big chunks in mineral oil as well, cut it thin and rinse off the excess oil with hexanes. Haven’t had a problem yet. The best route is for one person to add the essentials and turn it off and on everyday.
the still has been up for a solid year or so without a quench. There is a fatty piece of sodium floating around in it that I can see. I have been maintaining and setting up all the stills in our lab(which is crazy considering there is no supervision). Mine is usually a nasty tan color (the thf still) and after a couple days it goes green. When it got low on solvent once there was this nasty sludge that covered the bottom. My guess is that a lot of the benzophenone ends up there, as well as new pieces of sodium. The other problem I frequently have is the god damn sodium clumps up into a big ass ball over time.
Every lab in our department has one of the solvent dispensing systems from here http://www.glasscontoursolventsystems.com/index.php
)
Seriously, it’s a piece of art. The (20 L) kegs are easy to refill. We have 4 solvents on tap…super dry and anything we don’t have, some other lab probably has (except dioxane
yes, but those require money. gobs of money.
“We have enjoyed much success with customers such as Harvard University, Yale University, Scripps Research, Boston College and many more.”
haha. Yeah, well if I went to a liberal arts institution where I had more than a 1000 dollar budget for research(thats for 2 years of work) maybe I would just get me one of those. But until then I am stuck with a tan color thf still that I don’t really trust. Most of the time I am forced to distill onto 3A sieves and allow to sit overnight. That usually works pretty well.
Tom, are you sure that you are drying your THF under stroxygen-free atmosphere? You know, a little oxygen and the ketyl color is gone.
Yeah I got it back to a nice purp color now. I just had to add some small pieces of sodium and some fresh benzophenone. Looks great now.