First extraction - Have a couple curious questions.

[parabowl]

Hey all, after lurking around I finally decided to get an account

My friend did the marsofold tek and had some questions after it, I could not answer his questions from searching or any of the FAQ's (which are a great help I might add :thumb_up: ) so I am going to throw them out there to see if any nexians can maybe help.

1. My friend tried a carbonate wash on the first pull and let it sit overnight to separate. I've read online that it should be separated within 5 minutes because you can lose yield to it if it sits too long. This doesn't make sense to me since if the carbonate solution is basic, then nothing should go into it. I am guessing that this is a myth, can anyone shed some insight into this? Of the 4 pulls done so far, they all have about equal yield so I dont think that he lost anything, but was just curious.

2. He tried 4 pulls total so far, the first pull done with the carbonate wash came out the yellowest. The 2nd and 3rd pulls had no carbonate wash and were done at room temp and came out a lighter yellow. The 4th pull also had no wash but was done with heated naptha and came out pure white. This seems to be the complete opposite as I would expect :surprised ! Could it be that the impurities were being pulled out in the early pulls and now there is just spice left? I was under the impression it would work the other way around.

3. Heating naptha to get more spice seems like a good idea but once you combine it with the rest of the solution, doesnt it just cool back off to normal temperature almost immediately as it is mixed throughout? My friend told me that the naptha was back to room temp again immediately after mixing. Should my friend be heating the whole container or just the naptha?

4. If my friend plans on recrystallizing anyways, is the carbonate wash just a waste of time?

I have been curious about some of these questions for my friend and have done a lot of searching/thinking about them. Any help is greatly appreciated!

 

[Kash]

Carbonate wash is pretty much useless/doesnt do a whole lot. It is used to 'supposedly' remove any excess base that somehow made its way into the naptha. If your aim is for pure white spice, make sure to defatt with naptha a few times a non-basic extract before you make basic and pull to the nonpolar solvent.

Acid/Base extraction with defatt gives purest product in my opinion.

 

[parabowl]

That was my thought after he did the carbonate wash too...useless haha.

 

[endlessness]

You mean 'sodium carbonate'. I know yu are abbreviating for simplicity but with chemistry and when asking for help/advice, its good to be exact, because a small mistake can make worlds of difference (for example if you use another carbonate and not sodium carbonate).

As for the losing yield during wash, you're right the DMT should not move to the water if the pH is high enough. A side by side with a quick vs long wash could answer this once and for all.

Regarding pulls, its hard to say because there are many variables appart from temperature. Unless you mix with a magnetic stirrer in the exact same amount of time, there will be other variables involved because you may mix more or less depending on the pull, etc. But I can say that, from experience after many extractions, first pulls tend to be whiter, later pulls tend to be yellower, heated pulls tend to be yellower, long-standing pulls tend to be yellower.

Heating pulls can be done to the solvent, or to the whole mix (please do it safely, FAQ has instructions). Its true that the whole thing will cool down if you mix warm solvent, but if its really warm, it may take a few seconds to cool down which could be enough to increase solubility and increase yields, and once it cools down the DMT wont move away from the naphtha, it will stay in it, and the naphtha will be saturated. Yu can mix the whole thing too, though, thats maybe overall more effective? You could do a side by side and let us know

I disagree with kash, washing is not useless, and defat is a wasteful unnecessary process IMO. Check the FAQ regarding if you should wash the spice. If you do a re-x, indeed a defat is not necessary, though, because the lye traces will go to the bottom goo which you decant the solvent from.

And regarding defatting, if you get yellow, you can easily recrystallize your product with minimal amount of solvent, instead of wasting tons of solvent for defat.

 

[parabowl]

Yes I meant sodium carbonate, I will remember to be more thorough in help threads in the future!

I have read threads with that debate too on the sodium carbonate wash. My friends yields were equal throughout getting 160 mg on the first pull, a combined 320 mg on the second and third pulls and 160 again on the 4th pull. I would have expected my friend to get much more spice at first and have it taper out, but it keeps being a consistent 160 mg for each pull. I am guessing that the naptha is reaching as much as it can hold. My friend was expecting to see 2.5 g according to the tek but he isn't complaining and will keep doing pulls then until he doesn't get as much.

Since my friend is seeing consistent results, for the 5th and 6th pull I will have him do just a hot naptha extraction for the 5th and I will tell him to immerse the whole container in a hot water bath for the 6th to compare the yields. Naturally one would expect the total immersion hot water bath to produce more spice so if the 6th pull has a greater yield than the 5th, one could be pretty sure that this is a more effective method. My friend will probably be doing these pulls in about 2 weeks and I will report back his findings.

My friend was hoping that he could just do a recrystallization instead of a defat (since it seems easier) so it is good to hear that you can interchange the two. He was also thinking of keeping a little bit of the light yellow spice from the 2nd and 3rd pulls to try out against the pure white spice since he hears that some people enjoy it better. It will be his first journey so he is very excited!!!

 

[parabowl]

Update:
My friend tried testing heating up the mimosa/naptha solution all together by putting it in a bucket of hot water from the tap. He did not think that it would be hot enough to create any serious pressure in the bottle...it broke and it all went out everywhere haha :shock: . So much for the experiment. My friend has started a new batch however so he is not too upset and will not make this mistake in the future.