1st gassing attempt

[Armbarian]

okay swim tried to gas some np/meth for the first time. All went as expected (cept the was a bit more gas than anticipated). Swim put the tip of the tube in and letthegas flow, at first everything seemed to go well. A nice jar of crystals seemed to form. Then swim had to run to answer the phone came back to a jar of milky liquid with sludge at the bottom. Swim has decided to evap the sludge and see what happens. Where did swim go wrong? Swim used VE's damp rid/ muratic acid gassing method. Could someone tell a noob what to do after gassing?
Thank you for tollerating my stupidity.

[Bandil]

Did you gass while talking on the phone? In that case it's overgassing...

Basify, extract the goodies with some NP, and try again.

[wareami]

But if overgassing is the case, wouldn't a bee still be able to collect the sludge(it's still meth) and treat with acetone to remove excess HCL and then recrytalize?
Just thinking that rebasing may be overkill re-getting what was already got!
One would need a very fine filtration setup to collect AWE the sludge though.
Most suggest vacuum filtration for this I beelieve!

[Bandil]

Come on folks! Have some pride please  

Sludge does not equal quality drugs. If you engage in a lengthy and expensive synthesis of a compound, do it properly. It's very little extra work really!

Instead of gassing, I'd suggest you do it as described here:

Post 513755

(Bandil: "Easy preparation of HCl salt w/o gassing", Newbee Forum)

You simply need to basify, extract with toluene (or similar) and follow the writeup. You'll have a very minimal decline in yeild and wont have to worry about over acidifying etc!

Have a nice weekend,
Regards Bandil

[ChemoSabe]

The time this happened to swims buddy he added 20 ml of DH20 to the NP in a sep funnel swirled a few times until the NP cleared up. Sepped off and evaporated the water (which turned pink). Acetone wash and reXed the goods.

Top notch product.

The first acetone wash had the stuff bright white with no pink remaining. But reX the stuff for numero uno grade caca.

And not any attempt to hedge over Bandils ideas. His are rock solid good advice but I gave my own 'cause at this point in your chem endeavors it might be a simpler way to go which should still get you good results. From an all around viewpoint though Bandil is quite correct in all he sais.

[dextro]

how can "overgassing" arise?
swid is thinking: when the last trace of FB is consumed by the HCL Gas, then there will be no further crystal creation. Is this not true?

2nd. question: after the steam distilled FB is dissolved in NP, is there still a "water-wash" of the NP necessary?

thx

[ChemoSabe]

The non polar solvent will continue to take on HCl even after all the crystal has formed turning it pink or orange. And stinking.

[NaXen]

2nd. question: after the steam distilled FB is dissolved in NP, is there sill a "water-wash" of the NP necessary?

SWIM has always done washes of the NP post-steam distilling, its not a whole lotta extra work, and could facilitate the cleanup procedure greatly    but SWIM is not sure if it is absolutely necessesary....

[Rhodium]

Instead of washing with water, it is advantageous to wash the non-polar with brine (concentrated table salt solution).

See

Post 394075 (missing)

(pHarmacist: "Washing with brine", Newbee Forum)

[dextro]

thx rhod. for the link!

so it seems the best workup after steam distilling is:

1.) one water wash
2.) one brine wash
3.) dry over Mg Sulfate
4.) gas

previous washing with NaOH seems to be an overkill, right?

videoeditor is his "steam and clean" post called "it will be the cleanest FB on the planet" so why should someone do this much washings?

So there is a little bit of confusion