What's the material of this container? Is it compatible with chemicals you use?

The volume of the pipette is just practical, you can do it with 3ml, it's just annoying.

The material is glass, probably not borosilicate but enough to withstand high(er) temps such as boiling, but would most likely shatter if exposed to a rapid cool-down. For reference the type of container pictured in the TEK would be the same, if not extremely similar material to the one I plan to use.

I hear you on the inconvenience side, though I had a heap of the 3mL handy so I'll just use that until they're gone and then up to 50mL.

Yeah, soda–lime glass is not bad at all. It can be used for many extractions, but i would change it after some time, just for the safety, especially if working with heat and lye. But not earlier than after about 10-15 extrations, which is enough for most people.

And the problem with sudden changes of temperature is really serious. One of my bottles cracked full of basic water after unwanted contact with cold water when warm. Fortunately I do everything above the sink, so this saved me from serious problems.
But this was because I was not cautious enough, so just ... don't do the same mistake or at least keep the same safety precautions.

In this instance it would be a temporary/disposable container, and as long as it does the job (sealing and shaking) then it's a very easy solution than trying to get something more expensive.

It does make me think that the heat bath has another purpose; which is to allow the glass to cool-down slower thus minimising the risk of thermal contraction/expansion and subsequent shattering.

Got another question - at the naphtha stage, 50mL is rising and leaving a very THIN layer on the top, that itself isn't a bad thing except that the container is very wide before narrowing, so with that in mind, would adding 100, 200 or even 300mL to the container cause an issue with regards to the separation or would it be considered a waste of naphtha? the idea being that if the naphtha is merely a carrier for the DMT, then it would require more extraction but not necessarily dilute the end result yes?

And another one (sorry about this). Reading through the TEK there were a few things that didn't make sense to me (with the way it was written it could be interpreted a few different ways):



Based on that there are a few ways I'm reading it:

1) Add naphtha, shake and leave for 60 mins, then shake and leave for 45mins x 4 times = 4 hours in total for 1 pull, then repeated for however long before the MHRB is exhausted, which after 5 pulls is 20 hours elapsed

OR

2) Add naphtha, shake and leave for 60mins, then shake and leave for 45mins THEN pull = 1.75hrs per pull. so after 5 pulls is 8.75hrs.

Or is it something different completely?

Yes, it may be tricky to suck out the most of the solvent. You can't get all the solvent for first pulls, there always will be remainder. Only the last pull allows getting 99%. For non-last pulls there always will be 10-20% reminders.

There are 2 ways how to get the most of solvent out...
First is the shape of the vessel. You can use erlenmeyer flask, which helps to keep the solvent column high.
Second you can use more solvent. This is not problem for the extraction, in fact it is even better to use more, because more dmt will get out each pull. The only problem is it is not saturated, so can't be used directly for freeze-precipitation. This can be solved by evaporation of the solvent or by back-salting.
Yes, evaporation may be considered as wasting naptha, I always do back-salting.


sorry, I don't understand this

Sorry I explained poorly, you answered the question perfectly with your explanation around more naphtha equals requirements for back salting and not as good for freeze precipitation.

Or (again),

Add naphtha, leave for 60mins then pull

THEN

add naphtha, leave for 45mins, then pull.

I am not using this TEK. I can just tell you what I do. I mix like crazy for one or two minutes. Then I wait for full separation. Once fully separated, I repeat this cycle again. I do 3 cycles for first pull, 6 for second pull, 10 for third pull. I don't know your solvent, so can't say how many pulls you need. It can be anything between 2 and 10 I would say. But it depends on the solvent you use, its volume, temperature. It is good idea to freeze-precipitate or back-salt your last pull, so you know how much is there. This can tell you whether you need next pull

I guess what I'm trying to understand is how long to leave the mix separate for, the more I try to understand the TEK the more I'm wondering what to make of it.

I totally appreciate that you're not using this TEK, so I can't say how grateful I am for your advice so far. when I looked at the results from the first pull I'm still scratching my head as to why it came out clear, have left it sitting in pure 100% hydrocarbon (shellite) for about 1.5hrs before pulling, really just wondering if I should have waited another 5 hours before commencing the first pull or not. At this point I'm just trying to cement that this MHRB is a bad batch or if I'm not doing it right.

BTW - I can't reply to PM's just in case.

The more contact and movement between layers, the more the dmt transfers. The best is shaking without break, but this is not very practical. So shake just two minutes, so everything mixes up. Then wait till full separation. This is working for you too, as the tiny drops of solvent are moving upwards through the water. Once the layers are separated, there is not gain in leaving it like that. So shake again and separate again. The more cycles you do, the better. Pull immediately after full separation of last cycle.

Right there, that's what I'm missing I think, pic inbound.

I'm guessing this is what I'm waiting to clear?

Not dmt, but the principle is the same...

https://www.youtube.com/watch?v=QhC1QeJsWqk

You aim for two clearly separated layers. Anything in between is an emulsion.

I've been trying to get rid of this emulsion but it's not happening. So far I've tried a technique with siphoning the emulsion then slowly releasing in the RB mix below the emulsion, and noticed the pH was 9.6 so I've added more lye to get it to +11

Any other ideas as far as removing emulsion from a STB tek?

What's the total mhrb/water/lye ratio you used?

it was a 1:1:15 of MHRB/lye/water respectively. I added extra lye and the emulsion seemed to dissipate somewhat.


Also I've seen a result of the freeze-precip; the naphtha drain was then put into a collection jar and back into the freezer and then BOOM....crystals started forming. So possibly too much naphtha (unlikely) OR the naphtha wasn't saturated enough and as a result, the gradual evaporation of the naphtha (via freezing or atmosphere exposure) got the ratio between dmt and naphtha low enough for crystals to form......is that a regular thing? Is that a sign that maybe the steps before pulling wasn't done long enough? Can't stress enough how I'm more asking for for what your opinion/experience says - I know you're not doing the same tek process.

You never know how much dmt is in the bark. So you don't know how saturated it is. It has to be evaporated to cloudiness before freeze-precip.

Check faq about emulsion. I would use more salt then heat and vibrations. Careful stirring would be the last resort for me if you won't be able to find proper procedure for your bark.

Thank you for that, I actually didn't get to that part of the guide *facepalming myself now*, up until recently I was reading more through chapters 1-3.