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Evaporation with Low Yield :-\ Options
 
Angel_Above
#1 Posted : 11/19/2009 4:50:13 AM
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Second pull being evaporated right now.

The first pull I had gotten over 2.5 grams of DMT using 250 grams powdered MHRB.

I seem to have about only 50 mg in the dish that's being evaporated right now, and all the naphtha is pretty much gone (evaporated down 400 ml of yellow naphtha after doing a sodium carbonate wash).

If I turn the dish upside down in the freezer and leave it there for, let's say, a week, will it crystalize more and will I end up with more product?

Just wondering what my next step is.

Also, what is a good way to store 2.3 grams of DMT? I currently have it in a pill jar in my fridge, but I don't know how effective that is for storage.

Should I switch it over to a baggie, put the baggie in the pill jar, then jar in the freezer for better protection?
 

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jamie
#2 Posted : 11/19/2009 4:52:24 AM

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Oncewas
#3 Posted : 11/19/2009 4:52:59 AM
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I thought 2.5 grams was good for a 250 gram mhrb? that's 1% Very happy
 
Angel_Above
#4 Posted : 11/19/2009 4:53:56 AM
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Well ya, but I though I would be able to do subsequent pulls.
 
cashewman1
#5 Posted : 11/19/2009 5:32:43 AM

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To further help you should post:
The tek your using
The portions you used



Ideally you should be able to do subsequent pulls, but it can vary depending on the volume you used to pull the spice. Either way there is a point when the amount of DMT in the solvent reaches a saturation peak, at this point you have the most DMT you can get in the solvent, and it is an equilibrium between free base DMT and Dissolved DMT in the Solvent then you remove and freeze precipitate it.
Now if you managed to pull 2.3 to 2.5 grams of of DMT from a freeze precip of your NP solvent, then you already have some great yields of close to 1% on MHRB. This either means you have some impurities(excess lye/plant material) and may want to consider washing it and recrystalizing, or you did a damn good job.
When you remove the fully saturated solvent and replace it with new solvent you can establish a new equillibrium between the amount of DMT in the basified solution and the amount of DMT dissolved in your NP solvent. Think of it as diffusion, when solvent lacking solute enters the container the DMT will naturally move towards the area of lower concentration (NP Solvent) from the area of higher concentration (Basified bark solution), but there is less DMT available due to removing it from the extraction jar with your first pull. This means your subsequent pulls should be substantially smaller and smaller. 50 mg from second pull after 2.3-5 grams first pull sounds fine.
turning it upside down should not effect the yield precipitate but rather it helps drip fats and excess contaminates off of the crystals for full drying, and storing in a pill jar in freezer is plenty fine, my friend likes to use microcentrifuge tubes.
Sorry long winding and possibly convoluted post, over tired from studying for exams tomorrow, maybe will try and clean it up tomorrow
Need sleep
Hope it helped
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Angel_Above
#6 Posted : 11/19/2009 6:24:49 AM
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Yes it helped.

And my plan was to originally evaporate the first pull down to a much smaller amount (like 50 mL) but when I checked on the evaporation plate a few hours later (I had class) I saw tons of crystals on the plate. I turned it upside down in the freezer for a night to try to make it a cleaner product, and that's when I scraped 2.5 grams.

I used an HDPE2 bottle with 250g lye/250 g powdered MHRB, and the rest distilled water.

I would add naphtha and mix it around a few times daily for 3 days (this used on the first pull) and I took the naphtha off and put it in a mason jar. I did the same thing with 350 mL of additional naphtha and reached my 600 mL. At this point, I did a sodium carbonate wash (pinch of NaCO3 and 75 ml distilled water) and after that did two more 50 mL distilled water washes without sodium carbonate.

I then moved on to evaporating, and you know the rest.

I have some of those centrifuge tubes. I saw a picture of DMT in one before, and it made me want to get some Very happy

 
furley
#7 Posted : 11/19/2009 9:18:42 PM
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3 days seems like an enormous amount of time for just 1 pull, you likely got all the DMT out in that 1 go. Also couldn't there be problems with condensation if you left a plat uncovered upside down in the freezer?
 
Angel_Above
#8 Posted : 11/20/2009 6:21:50 PM
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There would be condensation problems if I had it right side up with a cover, not upside down.

But yeah, I just checked on my plate and it's all goo that's on the bottom of the dish that smells liek DMT, with some other random shit in there (attributing that to plant fats).

Not worth scraping/smoking, right?
 
 
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