Sodium Metabisulphite

[cheeseboy]

Cheeseboy's Vacuum is great for distilling safrole out of sassy oil, and helps get the water out in the epoxidation, but seems to be slightly weak as a vacuum for ketone distillation. So cheese is going to try and cryystalize the ketone into a precipitate using Sodium Metabisulphite. Heard that this is a great method, heard that it sucks. Who has used this method successfully? Cheese wants bees to answer who have TRIED this method, not bees who know of it from reading, although every bit of info helps. The ketone/crap oil is dark reddish, yellowy brown, almost black, and was derived from the Oxone>Isosafrol/--> H2SO4 treatment of epoxide route.
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[cheeseboy]

Right on, thanks for the info MaDMAx. 5 lbs of technical grade Na Metabisulphite costs $10 through a chem supplier, cheaper than the sodium bisulphite is. Heard it can be bought in the supermarket as a preservative. Is it commonly found at the Supermarket or just in some select places. Cheese would like to pick some up while waiting for the technical grade to arrive.
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[ChemicalSolution]

If you can distill safrole at a temperature of 130-135 or lower, you can distill the ketone...

Perhap's a lot of problems arise from not insulating/heating the distillation column..   This is not so much of a problem when distilling safrole-- a simple Al foil coat will work (although, not IDEAL).. With ketone, you might find yourself with an aim-n-flame running it over the Al-glass wool/coated column..

Don't use a column?? 

Do the bisulfite addition.

[cheeseboy]

Cheese's weak vacuum distilled the safrole out at around 168°C and the isosafrole came over at around 182°C . However the vacuum wasn't always on full untill the oil was less than half full in the flask (tendency to get sucked thrugh condensor into receiving flask). That's why the separation temps aren't statistically correct between Isosafrole and Safrole but they are close enough to know that they are 2 different alkenes. So with the ketone coming over 30° more than the precursing oil (2-alkene) that would make it's BP around 205°C. Cheese's heating mantle is broken and has no access to a stovetop for smelling reasons and cheese was trying to distill the MDP-2-P out with a french fry cooker, fryer, and found out AFTER setting up and waiting for 1 hour that the temperature of the fryer only went up to 200°C. So cheese needs another 10°C. A new hotplate stirrer is on the way, so patience and a freezer are cheesboy's friends right now. Fucking oil baths stink..arrg!!
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[ChemicalSolution]

Now that just ain't right!!

Are you using a water aspirator??  Fast mag-stirring??

You should go back and make sure your joints are lubed.. 

If that fails, go get one of those heavy duty water pumps.. Now, buy one of those coolers that have a water outlet switch at the bottom... Fill it full of ice water. and put the pump inside.. It should pull a much better vacuum..

[humidbeing]

Yeah cheese, I'm waititng as your problems are mine.

 I've been told that a good aspirator station is as good
as the oil pumps when the feet of head equals that of
psi 40 to 50 feet.
Swims still trying to decide wether to go for oil or
jet pump/driven aspirator.
Noj gets a high rating on his set-up illustrated on
rhods site.
 
nipples and buttocks and crotches with wings these are a few
of my favorite things

[Rhodium]

Max attainable vacuum with an aspirator is about 10 mmHg, while you would get down to 1 mmHg with an oil pump easily. That is a bigger difference than it sounds like.

[blaztoff]

You will end up losing around 40% if you try to extract with bisulfite and you will still have to distill your ketone after. Sodium Iodide works better if you dont want to distill your ketone after.
Use an aspirator. Make a aspirator station and use one of those jacuzzi pumps for circulating water. They can get your vacuum low enough to pull ketone over around 150-165C easilly. And if carefull you can distill ketone at higher temps. Swim has done so in 180-195C before. You just take your heat up very slowly and when first drops start to come over leave it-it takes a while but it works. Take your heatup to safrole dist henturn heat up in 2 degree increments till it startsto drip.
Deep friers and like will end up causing more probelems than thier worth. If you need heating and dont have a heater a nichrome wire strip will work. Connect it to a variable power switch and you have heating. You can put the wire directly into bath for easy heating. Just make sure your electrical connections dont touch it. It was used  quite often in old labs-they called it suicide wire cause of lack of safety. DO a search and you will come up with resisitance charts for nichrome wire telling you guage length required to heat to desrired temperature.

[ChemicalSolution]

Max attainable vacuum with an aspirator is about 10 mmHg, while you would get down to 1 mmHg with an oil pump easily. That is a bigger difference than it sounds like.

And according to Vogel, halfing your vacuum (30mm to 15mm for instance) will reduce the bp of the liquid by about 10C.

[cheeseboy]

So then the Na2SO2O5 is a 'Big Thumbs Down'? Cheese wanted to use it as a separating tool, but it will be a good indicator that ketone was actually made. The brown oil isn't too murky or dirty looking, it probably will mix into the metabisulphite and form a kind of oily cruddy mass instead of a crystal mass, that's what MaDMAs said. But it will be good to know that cheese actually has P2P not dark brown Isosafrole Epoxide or Glycol. What a time for a heating mantle to fizzle eh!?  Cheese tried using a water aspirator first, guess the pump wasn't strong enough or the aspirator plain sucked ass. Don't know and don't wanna try that set up again, the pump can be used for condensor hose pump.Not watsed. But a better vacuum is needed, cheese thought he got a good one but it ain't cutting the cheese.
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[blaztoff]

Instead of using a whole bunch to test if you have ketone take a little instead. You would probally have a hard time with bisulfite to tell if you have good ketone or not if its dirty. Try pouring out ketone into another container. There will usaully be a little left on sides of vessel one that is relativwlly clean compared to the rest of the mix. It will be enough to do a bulsulfite test-you only need about 1ml of ketone to do the test and you will have a much cleaner sample to test with than the rest of the rxn mix. Sodium Iodide will work with dirty ketone but its harder with Bisulfite. You might have to use a little alcohol to get the ketoneto crystallize if its dirty.

[cheeseboy]

Actually it's funny you say that, cause some was poured out of a vial and the vial smelled very much like ketone moreso after the shit was poured out. very creamy. So is the Sodium Iodide thing for cleaning up ketone that's already been subjected to the Sodium Metabisulphite, or is Sodium Iodide the same in the way that it forms a precipitate? How come noone ever mentioned Sodium Iodide before now it seems? Just the Sodium Bisulphite treatment.
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[blaztoff]

Sodium Iodide works the same way as bisulfite-it forms the precipitate. It seams to work better for extracting dirty ketone and you can use it without really distilling your ketone after even though Swim would recomend to distill it anyway. You can also store it.

[cheeseboy]

The crude ketone isn't too dirty, cheese figure's is not far from close but hasn't had a chance to distill it, it is sitting in deep freeze remaining liquid state. Smell is the only way to know without distilling and taking note of boiling temperature. #$%*%$#^*^%*@##%$^&*@#%@$&&%  Bah Humbug!
Cheeseboy- a whiteboy with soul, like a black guy without soul
May De Source Bee Wit Chu...Always

[blaztoff]

Good idea to store it. Even though the ketone might look clean it is not till you distill it. There is all sort of hidden nasties in there that will only come out upon distillation. But you can do a bisulfite test see if it is ketone or not now-may save you the trouble of distilling it later if it isnt. JUst take a test tube-add some water then put as much Bisulfite as it can hold shake repeatedlly. Once saturated just pour the solution out into another test tube so there is no more solids in it then add a drop of ketone into it-shake like mad maybe out in freezer but if it is ketone you will get little white crystals on top in  solution.