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xylene fasa - strange xtals
- Thread starter Phlux-
- Start date
This would definitely work. Also SWIM could use only a small amount of water to dissolve the crystals too. This would make the extraction with Naphtha easier and more efficient.
Exactly. a small-scale STB. the calcium hydroxide/sodium carbonate + fumarate salts watery paste is a modified STB, modified in the sense that it is dried before a solvent elective for the freebased alkaloids is used (acetone in this case)
In the "wet" stb, xylene or naphtha would be used simply because the latter are not miscible with water.
In the "wet" stb, xylene or naphtha would be used simply because the latter are not miscible with water.
this is after being cleaned once with acetone
okay so the method for converting bicarbonate of soda to calcium carbonate is to put it in the oven at 200 degrees for 1 hour ?
easy enough. its not that swim cant find it its just that the form it is found in - antacids - are always flavoured.
okay so the method for converting bicarbonate of soda to calcium carbonate is to put it in the oven at 200 degrees for 1 hour ?
easy enough. its not that swim cant find it its just that the form it is found in - antacids - are always flavoured.
Aye, almost. heating bicarbonate of soda (NaHCO3) in the oven will convert it to sodium carbonate (Na2CO3), not calcium carbonate.
The reaction is basically 2NaHCO3 ----> Na2CO3 + H2O + CO2
If you think about it, this is what baking soda as a raising agent does to the cooking... It decomposes to sodium carbonate and releases CO2 and H2O gases that raise the dough!
Mind that by heating bicarbonate of soda it will lose ~37% of the weight. If you cook 100g sodium bicarbonate you'll get 63g of sodium carbonate. It is a good measure to monitor complete conversion!
The reaction is basically 2NaHCO3 ----> Na2CO3 + H2O + CO2
If you think about it, this is what baking soda as a raising agent does to the cooking... It decomposes to sodium carbonate and releases CO2 and H2O gases that raise the dough!
Mind that by heating bicarbonate of soda it will lose ~37% of the weight. If you cook 100g sodium bicarbonate you'll get 63g of sodium carbonate. It is a good measure to monitor complete conversion!
Okay so swim asked me to ask you guys what he should do now. Here is what he did.
put the multi-fumarates in a bowl.
added an equal amount of sodium carbonate(he cooked bicarb in the oven at 200 for 1 hour - it did shrink and look different.)
mixed it with some water - a bit too much was added and swim thinks it would have been better if he had mixed the powders before adding the water.
Evaporated the water and ground it up - swim thinks it would have been better to really grind it up alot more than he did
packed it into a tubular vessel
and then added acetone - it was agitated alot, swim finds that by using a pippette with a squeezy bulb on the end to circulate the water by pulsing it, a good amount of agitation was achieved.
The acetone was left for a while for the particles settle. this raises the first question - how long should one leave it ?
The acetone was syphoned off and evaporated - more acetone was added and this step repeated a good few times - this raises the second question - how many pulls should one do - after pull 5 using about 12ml each time, the acetone is still comming off milky. should it be repeated until the acetone comes off clear ?
The last little bit is taking forever to evap, but all is looking good.
put the multi-fumarates in a bowl.
added an equal amount of sodium carbonate(he cooked bicarb in the oven at 200 for 1 hour - it did shrink and look different.)
mixed it with some water - a bit too much was added and swim thinks it would have been better if he had mixed the powders before adding the water.
Evaporated the water and ground it up - swim thinks it would have been better to really grind it up alot more than he did
packed it into a tubular vessel
and then added acetone - it was agitated alot, swim finds that by using a pippette with a squeezy bulb on the end to circulate the water by pulsing it, a good amount of agitation was achieved.
The acetone was left for a while for the particles settle. this raises the first question - how long should one leave it ?
The acetone was syphoned off and evaporated - more acetone was added and this step repeated a good few times - this raises the second question - how many pulls should one do - after pull 5 using about 12ml each time, the acetone is still comming off milky. should it be repeated until the acetone comes off clear ?
The last little bit is taking forever to evap, but all is looking good.
Hmm, SWIM's acetone tends to come off almost perfectly clear. SWIM is extremely careful to let the sodium carbonate settle completely when decanting. However, if SWIY is using an extremely small amount of acetone, it could possibly be supersaturated enough to appear milky. If at some point it comes off clear, try evaporating it on a clean dish to determine its possible content.
This could indicate moisture contamination within the acetone, which would likely dissolve some of the sodium-carbonate. SWIM prefers to use anhydrous magnesium sulfate to chemically dry the paste due to this possibility. SWIM doubts this possibility, however, as the mixture appeared quite dry, and SWIM assumes the acetone was properly dried of water contamination as well.
Thanks for trying this method! Pretty handy, eh?
This could indicate moisture contamination within the acetone, which would likely dissolve some of the sodium-carbonate. SWIM prefers to use anhydrous magnesium sulfate to chemically dry the paste due to this possibility. SWIM doubts this possibility, however, as the mixture appeared quite dry, and SWIM assumes the acetone was properly dried of water contamination as well.
Thanks for trying this method! Pretty handy, eh?
very handy - the same acetone was used for the fasa step - when evapping it looked like there was a pile of water caus the last bit is taking forever - is anhydrous magnesium a dessicant - can i use silica gel - also how can i be sure my acetone has no water - i remember reading somewhere about adding oven baked epsom salts ?
Ethnochemist
Rising Star
Yeah, swiy would want to take epsom salts and bake them in the oven. 400F for a few hours.
SWIY then adds that to the acetone.
E.C.
SWIY then adds that to the acetone.
E.C.
Yes, that's the anhydrous magnesium sulfate. One would do well to add that to the acetone as well as the paste. Silica gel wouldn't work well in the paste, but SWIM's heard of using it in column chromatography to dry acetone.
as in use cooked epson salts instead of cooked bicarb in the paste ? is there any benefit to this ?
from this same bottle of acetone swim has evapped a lot of it with no water problems - only now its giving me problems - the last bit just wont evap. and looks watery - no idea where it came from unless the condensation on the outside of the jar sneaked in while the acetone was evapping - the evap process was going so fast it was cooling its self.
from this same bottle of acetone swim has evapped a lot of it with no water problems - only now its giving me problems - the last bit just wont evap. and looks watery - no idea where it came from unless the condensation on the outside of the jar sneaked in while the acetone was evapping - the evap process was going so fast it was cooling its self.
SWIM get's that almost every time, it will evaporate eventually. SWIM's usually only takes a day or two. He keeps his process fairly dry so the moisture content is fairly minimal and probably attributable to ambient moisture.
But no the epsom salt is not a replacement for the base (sodium carbonate). To use it, just make the paste as per usual, but rather than air drying the paste, stir in the anhydrous epsom until thoroughly dry.
But no the epsom salt is not a replacement for the base (sodium carbonate). To use it, just make the paste as per usual, but rather than air drying the paste, stir in the anhydrous epsom until thoroughly dry.
what SWIM does to keep the acetone from causing water precipitation is to use either a little mini coffee hotplate or a mini crock pot with water in it...this keeps the acetone and jar from getting cold enough for water to form on it..and it helps evaporation..just make sure it doesnt get too hot
Swim took the xylene he had added the fasa from and pulled - the empty xylene and washed it with water - as soon as the water was added it became like milk and is slowly separating - is this normal ?
swim was also wondering - with how successfull stb and fasa is, why do ppl still do a/b extractions - ?
swim was also wondering - with how successfull stb and fasa is, why do ppl still do a/b extractions - ?
Most of those people have been striving to perfect that technique for years. Some have adopted the FASA method though, and SWIM has a feeling that once they've converted enough fumarate to freebase, they'll see the simplicity of sodium carbonate and acetone. These methods were only developed this last Summer if SWIM recalls correctly.
SWIM's only concerned that the new blood takes to the FASA approach and dry techniques right off the bat so that they can forgo the purchase of such toxic meth-related chemicals. To be fair, acetone is meth-related, but buying one can every few months with cash isn't so risky as buying a plethora of solvents and strong acids and bases. Plus its cheaper and much more wholesome.
SWIM's only concerned that the new blood takes to the FASA approach and dry techniques right off the bat so that they can forgo the purchase of such toxic meth-related chemicals. To be fair, acetone is meth-related, but buying one can every few months with cash isn't so risky as buying a plethora of solvents and strong acids and bases. Plus its cheaper and much more wholesome.