Emulsion using Max Ion Tek (that was Orionized)

[primordium]

Hi and thank you for reading this!

I followed Cyb's "MAX ION" tek (Cybs 'MAX ION' tek - STB - Welcome to the DMT-Nexus). I used 100g of ACRB and and made one modification--i.e., I used 130g of NaOH as a twist from Orion's tek (TEK: Boil n Base V1.2 updated - A/B - Welcome to the DMT-Nexus).

I knew that additional base was not a problem from the FAQ ( "One does not need to worry about over-basifying, there's no such thing." ). So, I figured it could only help prevent an emulsion from developing. [By the way, a solid definition of "emulsion" (as it relates to these extractions--e.g., why it forms, how to remedy it, etc.) on the FAQ or wiki would be greatly appreciated!]

After my first pull, an emulsion developed. Even worse: it never went away. It remained there for all of the rest of my pulls.

On chat, someone recommended adding salt. I threw a bit in. No help. I figured more lye and water couldn't hurt, so I threw more in. No help. The emulsion remained, taunting me with its disc-like immutability. Once I realized my glass turkey baster could dip past the emulsion, I made quick pulls that didn't recover all of the solvent, but they were clear (which was good to me). Before I actually made the pull, I put the glass bottle in a heat bath, which seemed to clarify the solvent a bit more.

I used small mason jars for the pulls. So, thanks to that emulsion, a few of them are either very murky now (not in the way it should be!) and some have reddish sediment at the bottom. How can I clean this up (if I even can)?

Right now, all of the small jars are in the freezer. I didn't get a chance to pre-evap at all, so they are probably all 1/4 or 1/5 full of liquid. A few seem reasonably clean, but half or more are certainly contaminated.

Any suggestions or even admonishments ( "Why the f*#$ did you...?" ) would be helpful.

 

[Purges]

The issue I had with 'emulsion' using Orions TEK was that the bark would float to the top and poke into the solvent layer. I found a bit of prodding with the baster and a few gentle rolls of the bottle helped reposition the bark clump. You may also find that if you just leave the container for a couple of days that everything will break down of its own accord.

As for the sediment, use a tall thin container for your pulls, then add some water to that container. A test tube would be ideal. It will dilute any gunk that you don't want and make it easier to decant. You can then suck off either the water or naptha. I wouldn't bother sticking any naptha in the freezer until you know it's clean. This will just create headaches later on.

 

[cyb]

Once I realized my glass turkey baster could dip past the emulsion, I made quick pulls that didn't recover all of the solvent

This is strange...
An emulsion is a layer of fine bubbles/foam and will sit on top of the base mix and under the solvent layer. How are you 'dipping past' it?

Most emulsions are to result of excessive agitation and can be broken up with heat/salt/lye/time. Some can be gently stirred to 'pop' the bubbles.

 

[Entheogenerator]

Any suggestions or even admonishments ( "Why the f*#$ did you...?" ) would be helpful.

Why the f*#$ did you go ahead and put the jars in the freezer?

Just kidding. But seriously, it is almost always best to ask questions and voice concerns before moving forward with the process. You may have crystals in your jars tomorrow, you might not if you didn't reduce your NPS pulls. But if your pulls were "murky" or contained "reddish sediment", there's a good chance that they also contained lye, which could now very well be inside those crystals. You have kind of created more work for yourself by moving forward with freeze-precipitation. The way I see it, you have two options to clean up those crystals and remove any undesirable and potentially hazardous impurities. You could recrystallize, which many people do anyways even if their pulls aren't contaminated. Or, you could filter/dry your crystals, redissolve in room-temperature NPS, perform a sodium carbonate wash followed by a couple of distilled H20 washes, reduce DMT-containing NPS so it is more concentrated, and freeze-precipitate again.

I am also confused as to how you "dipped past" the emulsion? I'm not entirely sure that the problem you are dealing with is an emulsion. Disc-like immutability? Pictures would be very helpful.

 

[primordium]

Once I realized my glass turkey baster could dip past the emulsion, I made quick pulls that didn't recover all of the solvent

This is strange...
An emulsion is a layer of fine bubbles/foam and will sit on top of the base mix and under the solvent layer. How are you 'dipping past' it?

Most emulsions are to result of excessive agitation and can be broken up with heat/salt/lye/time. Some can be gently stirred to 'pop' the bubbles.

Okay, so I must have been confused with what an emulsion is and was dealing with two distinct problems.

One problem I had was a thin layer of base at the very top (I thought this "third layer" was what others had called an emulsion, but I was apparently wrong). I dipped past this layer with my turkey baster.

I did have a legitimate emulsion, though. Beneath the solvent was what looked like a liquified choreboy of base--curly and foamy, just like you described. That was the emulsion for sure. Since this is beneath the solvent, what is the problem? Just the fact that you might not withdraw as much of the solvent as you might like?

When we say it can be broken up with "heat/salt/lye/time," does that mean to literally just add salt and lye and then stick the bottle in a heat bath for a while?

 

[primordium]

Any suggestions or even admonishments ( "Why the f*#$ did you...?" ) would be helpful.

Why the f*#$ did you go ahead and put the jars in the freezer?

:d It was nearing midnight and I figured waiting around would complicate the process more. Clearly, I was wrong!

Just kidding. But seriously, it is almost always best to ask questions and voice concerns before moving forward with the process.

I'll remember this next time (if there is a next time!).

You may have crystals in your jars tomorrow, you might not if you didn't reduce your NPS pulls

I peeked at them (about 8 hours later now). The "clean" jars have clumpy white in them.

But if your pulls were "murky" or contained "reddish sediment", there's a good chance that they also contained lye, which could now very well be inside those crystals. You have kind of created more work for yourself by moving forward with freeze-precipitation. The way I see it, you have two options to clean up those crystals and remove any undesirable and potentially hazardous impurities. You could recrystallize, which many people do anyways even if their pulls aren't contaminated.

Since this option seems much easier than the other, is there a greater risk of retaining impurities?

Or, you could filter/dry your crystals, redissolve in room-temperature NPS, perform a sodium carbonate wash followed by a couple of distilled H20 washes, reduce DMT-containing NPS so it is more concentrated, and freeze-precipitate again.

Thank you for the systematic advice! I'll be sure to research more on this (i.e., UTFSE).

For moving ahead, I have these jars now with too much naptha and clumpy, still floating white clumps ("floating" in the sense that they are not stuck to the walls of the jar). Can I go ahead and move them out of the freezer and use a cold fan on them to evap a bit, then throw them back into the freezer? Or is there something else I should do?

 

[cyb]

When we say it can be broken up with "heat/salt/lye/time," does that mean to literally just add salt and lye and then stick the bottle in a heat bath for a while?

Yes...If you have an emulsion and the solvent is already in the jar, just sprinkle some salt over the top of the lot, add lye (but only if you think you don't have enough) then heat bath to warm up the mix.
Some slight agitation should reduce it over time.

No idea what could be floating on top of the solvent.

 

[primordium]

When we say it can be broken up with "heat/salt/lye/time," does that mean to literally just add salt and lye and then stick the bottle in a heat bath for a while?

Yes...If you have an emulsion and the solvent is already in the jar, just sprinkle some salt over the top of the lot, add lye (but only if you think you don't have enough) then heat bath to warm up the mix.
Some slight agitation should reduce it over time.

No idea what could be floating on top of the solvent.

Thanks! Is it okay to pull out during the freezing process to evap more? I just have white clumps now.

 

[cyb]

Is it okay to pull out during the freezing process to evap more? I just have white clumps now.

Yeah, that's fine :thumb_up:
You really only need 100ml max (depending how much you extracted from...)
fyi. 30ml warm solvent will hold around 1g spice

 

[primordium]

Thanks for the help!

I poured the solvent into more jars, so now I have 11 altogether (which lowered the overall volume in each). I'm evaporating at room temperature now to lower the amount even more (Vovin's tek - DMT-Nexus Wiki).

Anyone have a guess at how long this evaporation might take? Imagine hand-sized jars like 1/5 of naphtha in them.

 

[primordium]

With much of the white solids not sticking to the walls of the jars, I am not sure how to decant. That is, if I pour out the NPS, I will also be pouring out much of the white material. In other words, I can't just pour out, fan out, and scrape.

What do I do?

 

[Entheogenerator]

I would recommend you use the sodium carbonate wash method that I described above on all of your pulls before freeze-precipitating or evaporating, unless you plan on recrystallizing them all. Recrystallization will work for the pulls that you put in the freezer when they were contaminated.

Anyone have a guess at how long this evaporation might take? Imagine hand-sized jars like 1/5 of naphtha in them.

This isn't really enough information to estimate how much solvent you have. What does hand-sized mean? Like half-pint mason jars? The naphtha will evaporate faster if it has more surface area. I would recommend combining them and putting them in a large glass baking dish to speed the process up significantly. Naphtha evaporates faster than water, but not as fast as say acetone or IPA.

Why are you freezing and then evaporating? You only need to do one or the other. I rarely evaporate my solvent when extracting DMT. Once you have reduced it to the point that it is super concentrated, you can just freeze-precipitate for 24 hours or so and get the same yield without wasting a bunch of naphtha. Freeze-precipitation often yields a final product of a higher purity as well.

With much of the white solids not sticking to the walls of the jars, I am not sure how to decant. That is, if I pour out the NPS, I will also be pouring out much of the white material. In other words, I can't just pour out, fan out, and scrape.

What do I do?

Coffee filters. Put a filter in a funnel, pour the naphtha into the filter, and stick it all in the freezer while it drains through. I like the brown ones because the spice is easier to see.

 

[cyb]

IMO: Don't use coffee filters to catch floaters...they will just melt back into the solvent soaked fabric as the temperature rises and be lost.
If you get floaters, the best way it to either freeze longer or pour off very carefully and slowly. Use a baster if necessary or hold them back with some fine mesh (stockings?).
Even if a couple escape you can reuse the solvent for the next pull and get them back.

Cold Fan evapping naphtha takes very little time.

 

[Entheogenerator]

IMO: Don't use coffee filters to catch floaters...they will just melt back into the solvent soaked fabric as the temperature rises and be lost.
If you get floaters, the best way it to either freeze longer or pour off very carefully and slowly. Use a baster if necessary or hold them back with some fine mesh (stockings?).
Even if a couple escape you can reuse the solvent for the next pull and get them back.

Cold Fan evapping naphtha takes very little time.

This is also good advice, to each their own.

I use coffee filters when there is a large number of floaters, like if most or all of the crystals are free from the walls of the container. I just pre-freeze the filter and the funnel I put it in, then pour the naphtha quickly and put the filter, funnel, and drainage vessel back in the freezer for a few minutes while it drains, to minimize spice meltage. But I also freeze-precipitate in a glass baking dish, which makes decanting the naphtha difficult.

 

[primordium]

All good advice! Thank you both!

I have a large number of floaters in some of my jars, so pre-freezing the filter and funnel seems worth a try. With 11 small mason jars, I'll probably use this time to experiment and see what works.

 

[primordium]

Coffee filters. Put a filter in a funnel, pour the naphtha into the filter, and stick it all in the freezer while it drains through. I like the brown ones because the spice is easier to see.

IMO: Don't use coffee filters to catch floaters...they will just melt back into the solvent soaked fabric as the temperature rises and be lost.

I use coffee filters when there is a large number of floaters, like if most or all of the crystals are free from the walls of the container. I just pre-freeze the filter and the funnel I put it in, then pour the naphtha quickly and put the filter, funnel, and drainage vessel back in the freezer for a few minutes while it drains, to minimize spice meltage. But I also freeze-precipitate in a glass baking dish, which makes decanting the naphtha difficult.

I went ahead and used a coffee filter for one of my jars. I poured the naphtha through (both the filter and the other jar were stored in freezing temperatures for over 12 hours). I put the filter and the jar it was attached to back into the freezer. When most/all of the naphtha appeared to have dropped through, I removed the filter and had a fan on it for several hours.

Unfortunately, all I was left with was a yellowish sticky coating to the filter, which was unusable.

Thanks for all of the suggestions! I was eager to experiment since I know there is more of an "art" to some of these steps, with some procedures working better for some than others.

If you're still feeling generous with advice, head on over to my other thread! It's here: Clear Goo, Re-Crystallization, and a Hair Dryer. - A/B - Welcome to the DMT-Nexus

 

[Entheogenerator]

Unfortunately, all I was left with was a yellowish sticky coating to the filter, which was unusable.

I hope you didn't throw that out... It sounds like it could very well be The Legendary ACRB Goo.

 

[primordium]

Unfortunately, all I was left with was a yellowish sticky coating to the filter, which was unusable.

I hope you didn't throw that out... It sounds like it could very well be The Legendary ACRB Goo.

I did throw it out. I'm sure it was valuable, but when I tried to use a razor to slice it off, the filter was inseparable from it (it was, more or less, melted into it).

I bet there was some way to re-dissolve and gain it back, but I'm already asking so many questions that I didn't want to bother anyone with an additional one!

 

[Purges]

You can always go on chat if you need some advice. Also, you could have just soaked the filter in some warm solvent to retrieve your goodies, I'm sure most of us have wasted a fair amount of Spice learning the ropes. I know I have *hangs head*