Bicarbonate of Soda Wash Question

[triptatmos]

Hi guys,

So a while back some spice was extracted from Mimosa and after three pulls and a freeze precipitation 0.405mg of yellow-white crystals were left on a weighing scale.

These had some slight contamination: bits of pipette rubber were present, as well as some of the lye soup. So the plan then became to do a wash.

It was decided to not do Sodium Bicarbonate as it was gathered that shop bought Bicarbonate of Soda (Dr. Oetker) would do the trick. Bicarbonate of Soda was mixed in the room temp water until it became a saturated solution. The solution was then added to DMT dissolved in heated naphtha. Separation occurred and the dirty parts clearly stayed in the bicarb solution on the bottom. The naphtha was siphoned off from a measuring cylinder and into a dish for freeze precip. However, after this freeze precip there were now only 0.215mg of white spice left.

My question is why was almost half lost? Was the first pull just really dirty (it doesn't look it)? Is shop bought bicarb bad? Bubbles were noticed on the jar in which agitation occurred, were they crystals getting stuck?

I was just wondering how much everyone normally loses in a clean. This was the first process done after extraction there was no re-x or anything like that. Any ideas would be much appreciated.

 

[GLTASN]

a carb wash should only take a few seconds, paying close attn. to the ph. Ive read that if done longer or wrong ph they can eat into your supply.

I like Watcha's STB tek, not found here for some reason? it utilizes a carb wash but if memory serves saturation isn't nesc., just enough to get to the proper ph is needed. if you do a search its easy to find, step by step, with images.

 

[Loveall]

It sounds like you need to do some naphta pulls from the sodium bicarbonate water used for the wash (did you keep it?). I would increase the water pH and add salt (~20%) before doing so.

 

[Jees]

Hi T,

...it was gathered that shop bought Bicarbonate of Soda (Dr. Oetker) would do the trick...

I think the max pH of SodBicarb at 8.75 - 9 is a tad too low.
A theoretical calculator says potentially 50% of dmt stays in salt form at 8.75 and 33% at pH 9. This could confirm with your findings.
So far I've only heard of Sodium Carbonate washes, with only a small pinch in water you easily get pH 10 of which that calculator says only 5% will remain in salt form, so recovering 95% in freebase in the naphtha.
The washes are indeed done quick.
The item of losing yield by washes has been touched in some posts here, with not really conclusive tests but just be aware of that possibility.
But so far I bet on the too low pH.
Recovery of spice in that wash water is possible as Loveall said.
Happy trials :thumb_up:

 

[triptatmos]

Thanks for the replies guys. Sadly, this was a while back and I didn't keep the water was a bit too much of an eager beaver :d so no possibility of reclaiming it in salt form.

And yeah sorry, I realise now that I meant to say Sodium Carbonate. I had read somewhere on the Nexus that someone used Bicarb and they said it worked. I went for Bicarb cos it was easier to acquire. But yeah as you're helpful calculations show that and probably accounts for the loss. I knew I would lose some yield, but I hadn't read anywhere about a 50%. Seems that my laziness cost me some spice, but hey you learn from your mistakes!

 

[Jees]

...I had read somewhere on the Nexus that someone used Bicarb and they said it worked...

Actually there is a tek that uses plain water for a wash [1] but washing really very swift. So the pH becomes lesser of a point the swifter the wash is done, in that regard sodbicarb could be used as well but adapt washing style for it. It's just that sodcarb has that higher pH that offers more protection against yield loss and you need only very little of it.

[1] Vovin's tek - DMT-Nexus Wiki
in the second and third wash he used distilled water only.
I've no idea what the purpose is of the 2nd and 3rd water wash, maybe someone chime in.
He said after the 3rd wash the naphtha is clear as glass, maybe it's about that.