Author Topic: end of titration but sans acetone  (Read 3202 times)

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aztec

  • Guest
end of titration but sans acetone
« on: August 07, 2004, 04:52:00 PM »
she does not have access to acetone at this time. however, she does have 99% alky.

may she go straight to re-crystallization without the acetone? usually, she rinses with acetone upon titration, then she performs the dual solvent re-crystallization(acetone/alky combo a la geeze).

there will be no access to acetone for several days yet. your comments appreciated.

aztec


CharlieBigpotato

  • Guest
assuming the acetone was used for:
« Reply #1 on: August 07, 2004, 09:31:00 PM »
removing over-zealous acidification?
if so, in aqueous solution, ph could bee brought back up with (drop-wise) base; evapped; re-solvated w/ dry alcohol; filtered to remove NaCl (assuming Hcl and NaOH were used) and a final evap w/ another solvent.
going too far basic would bee the next problem; shoot for 7

ChemoSabe

  • Guest
Room Temp dH20
« Reply #2 on: August 08, 2004, 12:18:00 AM »
The room temp dH20 evap technique might still be OK with this.

If not then eat it as opposed to whiffing or vaporizing. But mix it with something to eat or drink of course.

Swim's buddy once overdid it when spicing up a bottle of cold coke on a very long drive.

PS. Check out (try) VE's EZ gassing technique. Someone coaxed swim's buddy into it and he then said "bye bye" to titration. Quicker and more thorough.


number427948

  • Guest
I hope Im reading your question properly,but I
« Reply #3 on: August 08, 2004, 12:19:00 AM »
I hope Im reading your question properly,but I think M.E.K. could be substituted, perhaps I will check the solubility characteristics. If indeed your wanting to re- XTALL.MAybe some1 else will know


abominator

  • Guest
Stick with a simple iso crystallization
« Reply #4 on: August 08, 2004, 02:59:00 PM »
Stick with an iso rextal for now on a small portion of your gear and when you get access to tone or MEK, then do the proper rextaling techinique.

I imagine the product would still be a little dirty, but if it came from a LWR, then chances are it has few by-products in it anyhow(as opposed to hot dry cooks).


aztec

  • Guest
thanks!
« Reply #5 on: August 08, 2004, 06:47:00 PM »
she had always used acetone as a staple and was amazed to find herself without it not a clue as to what to do. thank you.

zib, even when she hasn't over-acidified, she has the habit of an acetone rinse before re-xtl. is it completely unnecessary? she kind of got addicted to the way the crystals just slid off the dish upon splashing it with acetone... like cookies off of a well greased cookie sheet.


CharlieBigpotato

  • Guest
yes, it is sweet
« Reply #6 on: August 09, 2004, 04:40:00 AM »
the only times i found it redundant, or even a a furthar pollutant, was in dreams of negative pressure.. in those dreams, one is faced with wondering just what it is they are removing; and if acetone might furthar pollute something that is already shiny. if you aren't using lab-grade regents, at some point, cleaning efforts are suspects for more pollution.

solvent pollutants, otc, can soon bee a consideration on the road to purity.
you will know if and when this occurs, assuming a pristine reference point.

much as i should bee want to diss osmium;
the post rxn; pre-based , aqueous solution NP wash is the oft missed step in this show.
get rid of the shit earlier down the road, when it easy.

why do it later on?

still, water alone will do all you hope for. and water will wash crud off the re-chrystalized funky go-go.

you don't need anything else.

geezmeister

  • Guest
careful titration, no heat evap
« Reply #7 on: August 09, 2004, 04:43:00 AM »
Be very thorough washing your solvent. Then do your titration very carefully, drop by drop, checking the pH carefully, and evap with no heat, fan only. It does take a while. It also gives very very clean, glass like meth you can smoke right out of the evap dish. Use less acid than you are used to, shake more than you are used to shaking, and do an additional pull or two if you don't have the yield you think you should have.

I was skeptical when Ici_Rhi said she could evap without acetone, but after I saw her titrate a batch and watched the clear meth form under fan, I became a believer.


ChemoSabe

  • Guest
Relevance of Old Monkees Song
« Reply #8 on: August 09, 2004, 11:37:00 AM »
Geez,

When I read your closing comment I couldn't help but replace the lyrics in that old Monkees song that would now go....

then I saw her meth
now I'm a beleiver

Swims buddy saves old tone and eventually redistills it. It seems to him that acetone that is heavily laden with I2 byproducts can often still somewhat reek of IO after one distillation. Swim's buddy wonders if the IO smell might just be of a "ghost" quality from recently having whiffed it elsewhere or if a second distillation is really necessary to get it purer. He uses this restilled tone only for somewhat dirty (non final product or precursor) purposes because he's never been certain enough of it's overall cleanliness.


abominator

  • Guest
Slow evaps
« Reply #9 on: August 09, 2004, 03:25:00 PM »
The way Geezmeister decribes how Rhi evaps is exactly how this bee learned to evap his gear.  No heat, just a fan and maybe under a bright light sometimes.  Swim says he always gets better yeilds this way, but it does require much patience.

Swim has always been an advocate of many solvent washings, in fact he remembers a gakk quite a while back that could be washed out of the post-rxn fluid.