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a zephyr in time skip to main skip to sidebar a zephyr in time an experiment in progress saturday march 20 2010 might as well not be here blah this thing might as well go on indefinite hiatus lots of work at the lab not so much time to blog and anyway most things that happen are unbloggable i d say one thing though life is very sad when the diffractometer is down boo my crystals are dying of old age as we speak boo too continue posted by echiral at 5 28 pm 0 remark s labels at work v thursday march 4 2010 liveblogging my crystals are up for xrd today runs around in circles what if they don t diffract what if they are too twinned to collect data on what if they are existing compounds gahh also nobody else is in the lab at the moment noooooo where s everyone i need all the help i can get continue posted by echiral at 9 33 am 1 remark s labels at work v thursday february 25 2010 3 second rant at self 2 laboriously prepared reagents 1 mistake 1 sad echiral dammit i added the deprotonated form of my reagent instead of the protonated form sigh wasted a clean dry flask of the right size 100 mg of crazy sensitive and limited reagent 113 mg of clean deprotonated compound and 2 hours of time an in situ protonation won t work boo hiss on the bright side although no reaction should happen to the current mess there might ve been a slight colour change maybe or maybe my eyes are playing tricks on me after i reset this reaction i think it s time to go home continue posted by echiral at 1 21 am 0 remark s labels at work v saturday february 13 2010 reading week reading week is coming up naturally work goes on reading week or no i m just relieved that there ll be no classes for a week so that i can get more work done funny how i don t really like classes any more however interesting they may be they just get in the way of experiments if the scheduling is a bit less awkward i won t mind it so much but right now every other morning is pretty much wasted with an awkward mid morning hour that s not quite long enough to set up a reaction grump plans for the week finish two mini projects and maybe just maybe one major project too reaction marathon i forgot to dry a 100 ml schlenk flask before i left for the weekend oops other than that i think i m good to go crystallography final project which is due unnaturally early in february measure theory assignment we re going to start fourier analysis after reading week oh to those who celebrate happy chinese new year tonight s the 30th it s traditionally a time for the entire family to gather together kind of like thanksgiving too much food expires on chair twitching continue posted by echiral at 7 58 pm 1 remark s labels at work v university life saturday january 23 2010 diction y know how one s vocabulary rapidly degenerates in the presence of a kitty it turns out that in my case this happens with coloured crystals too see the typical organic colourless crystals one sees during lab class aren t particularly interesting eh as long as i actually have a yield and decent spectra it s all good when the crystals are deeply coloured and large enough to glitter in the recrystallization solvent however it s sparkly and red and inside a large rbf squee looking at it makes me happy actually i think everyone who successfully made this compound has experienced this it s a long and annoying prep but the product is attractive enough to make up for it sadly the first crop is the prettiest one subsequent crops have an unfortunately tendency to become microcrystalline powdery less shiny now please let my nmr match the literature fingers crossed continue posted by echiral at 9 10 pm 1 remark s labels at work v sunday january 17 2010 right i have this thing called a blog as i said work takes up a lot of time really i hardly had time to read any blogs let alone write anything two weeks in i m still doing workup for one single freaking reaction to get a decent amount of pure product when recrystallization crops come in i also got away with calling my microcrystalline product fluffy in front of the pi sure i can say flocculent but come on most of us would just think of it as fluffy and leave it at that continue posted by echiral at 12 34 am 2 remark s labels at work v friday january 8 2010 so that s why synthetikers pull long hours i ran my first reaction of the term in the workplace lab today it was an easy reaction but took much longer than i thought it would the reality is that unless one plans experimental timing very well and is fortunate enough to have everything working available the first time around any experiment will always take longer than the procedure suggests furthermore most syntheses are more or less serial make an intermediate react it to get another intermediate and so on and i m not even in total synthesis whew so in result driven labs a student must pull long hours to get all the requisite work done finish one reaction step perhaps work it up and start the next with me add newbie idiocy and there s a recipe for 16 hour days right there frankly i have no idea how some of the other lab members who have full course loads on top of full time lab work can do it all notes to self 1 turn on the vacuum pump and let it run a bit before adding ln2 to the cold trap always always always evacuate first no blowing up the newly assembled vacuum line with liquid oxygen or even worse blowing up someone else s vacuum line 2 the right tool for the job usually does exist in the lab the only problem is that its location tends to be unknown so go find it 3 filtration through celite is very similar to column chromatography in the sense that a one can pack it dry or pack it wet but do pack it well and bubble free b never ever let it run dry until after the filtration 4 filtration in a glove box is no fun but easier than alternative one can t run the vacuum too long it starts stripping solvent and sucking glove box inert atmosphere so most of the time the vacuum is static meaning reallly slow filtration and hope really hard that the frit doesn t get clogged 5 assemble glassware hot and under inert gas flow 6 enough grease makes for airtight stopcocks even without the teflon backing gasket nut oh and rubber bands work as backing substitutes kind of depends on application 7 don t get grease into the sample 8 don t bump solvent up the vacuum line don t leave a sample under vacuum line unless it s dry 9 for overnight drying empty the cold trap and fill the trap dewar full of coolant right before leaving 10 people have long memories do something really wrong and your name will be part of the lab lore forever and ever not in a good way continue posted by echiral at 2 18 am 1 remark s labels at work v older posts home subscribe to posts atom about me echiral canada claim one can be a mathematician and a chemist too without being a physicist view my complete profile chemists carbon based curiosities chemical forums blog chemical quantum images chemistry world curly arrow entropic musings everyday scientist fetzthechemist hdreioplus de in the pipeline lamentations on chemistry liquid carbon molecule of the day my chemical journey the chem blog the sceptical chymist equivalence classes and in academia dr jekyll mrs hyde dr shellie femalescienceprofessor i blame the patriarchy lecturer notes post doc ergo propter doc professor in training thus spake zuska youngfemalescientist coffee theorem operators ars mathematica fermat s last theorem god plays dice learning curves life and then some me or my maths not even wrong shtetl optimized the unapologetic mathematician zero divides int dq t enginerdiness rate your students snark scribe the angry pharmacist