Small drops of basified mix in crystals

[dmt_awehhaea]

When SWIM was doing his first extraction, everything was going perfect. All up until the point where he had to use a cheap $1 turkey baster. It was awful, product spilled out and the mix was interrupted. Anyways, he managed to get most of the naphtha, but not all. (Figures, first pull is the most/best, and hardest if you never practiced before.)

The rest of the pulls went better, but SWIM had still sucked up tiny dots of the basified mix.

This is what it looks like,

Do you all recommend a re-x or will this be okay without a re-x?

Also, just a tip for any newbies. Invest in a proper tool or practice pulling before hand with something like oil/water, you don't want to screw up the most important pull!

 

[DmnStr8]

Do an re-x. It is an easy additional step. You don't want to be ingesting any lye as it is obviously bad for your health.

Invest in a seperatory funnel or a quality pipette to avoid this kind of thing in the future.

Happy extracting!!

 

[pete666]

Yeah, 50ml pipette with rubber bulb is the way to go. No need for sep funnel. I can't imagine doing the pulls with turkey baster. I tried but this is a real pain!

You can re-x or do sodium carbonate wash to remove the lye.

 

[dmt_awehhaea]

Update: Pull 2 was a total failure as well! There was at most .025g of product. The NPS was evaporated beforehand from 60g(Around 50ml) to about 20g, there was no cloudiness before freezing/after evap. After freezing, the NPS still remained clear with only very few crystals.

It seems the total is going to be around .2g, hopefully SWIM will do better next time

Thankfully someone talked SWIM out of a 100g extraction. I'm not too sure what's behind such low yields. The process was done just like cybs salt tek, (50g lye, 50g bark powder, ~35g salt, 60g/50ml naphtha, 60ml vinegar) The mixture turns dark maroon/black, NPS was separated 4 times in 40min. SWIM then added an extra evap step (reduce 1/2-3/4) when he noticed the NPS didn't look saturated. No luck!

 

[downwardsfromzero]

The trick is, if operating on the cheap, don't transfer straight from the extraction vessel into the freeze precipitation dish. Use a pyrex jug as an intermediate container for the naphtha. That way, any stray drops of base soup will be caught and your product will be a lot cleaner without needing to recrystallise.

0.2g from 50g bark isn't great but nor is it terrible. It could be that the bark is weak.

Thankfully someone talked SWIM out of a 100g extraction.

YW

 

[Randomness]

You might be able to wash the crystals with a bit of cold water containing a small amount of Bicarbonate or ammonia to clean up rather than doing a full re-x. It all depends on how pure a product you need.

If you still have the lye / mimosa soup you could try warming it up and doing another naphtha pull when it is fairly hot.

If you only got 0.2g then there should be way more in there. I would also be tempted to try adding another 10g of lye before pulling again.

 

[dmt_awehhaea]

You might be able to wash the crystals with a bit of cold water containing a small amount of Bicarbonate or ammonia to clean up rather than doing a full re-x. It all depends on how pure a product you need.

If you still have the lye / mimosa soup you could try warming it up and doing another naphtha pull when it is fairly hot.

If you only got 0.2g then there should be way more in there. I would also be tempted to try adding another 10g of lye before pulling again.

Total was exactly 0.2g. Second pull came out with absolutely no crystals, just some cold NPS with a tiny dot or two of basified mix, third and fourth also.

These were evapped and left to freeze for 6ish hours. (More than enough with the first)

I'm honestly not sure what's the cause of such sad results/yields. The basified mix looked almost exactly the same as Cybs. The only difference with the process was that the NPS separated fully in under 6 minutes (less for the second/third/fourth roll). I'm wondering if it was just the bark?

If anyone has any guesses, I'd happily like to hear from you!

 

[Randomness]

I used to always do my pulls whilst everything was fairly warm as naphtha cannot hold as much when cold, hence the reason freeze precipitation works.

Questions I would ask are.

Did you use any acid stage? If so there could have not been enough lye added.

How did you mix the NPS with the base/ mimosa soup? Was it adgitated enough to contact the spice? Remember that once you have added lye the spice is no longer soluble in the aqueous solution. Basically the nps has to come into contact with the precipitated freebase.

Did you recover all the NPS added or is some trapped within the bark as some kind of emulsion? I have had this happe before and got low yeild. Some of the solvent separated fully but the rest was trapped. It didn’t look like any was but I definitely got less solvent out than was added.

What was the temperature? As I mentioned above this can have a big impact.

How thick was the soup? I have had best results with at least 500ml of water to 100g of mimosa bark.

If it were me I would definitely try warming the solution and adding a bit more lye and possibly water if you have an especially thick soup and then doing another pull with everything at a higher temperature. I would be expecting at least 1g freebase from 50g bark.

I used to have a really good tek but it used magnetic stirring so I never bothered to post it on here.

 

[dmt_awehhaea]

I used to always do my pulls whilst everything was fairly warm as naphtha cannot hold as much when cold, hence the reason freeze precipitation works.

Questions I would ask are.

Did you use any acid stage? If so there could have not been enough lye added.

The acid stage was 60ml of vinegar dissolved in I believe 200g of water. 50g of lye was added in 200g water as well.

How did you mix the NPS with the base/ mimosa soup? Was it adgitated enough to contact the spice? Remember that once you have added lye the spice is no longer soluble in the aqueous solution. Basically the nps has to come into contact with the precipitated freebase.

The NPS was mixed with the mimosa soup by tilting upside down and upright slowly for 20-30s 4 times.

Did you recover all the NPS added or is some trapped within the bark as some kind of emulsion? I have had this happe before and got low yeild. Some of the solvent separated fully but the rest was trapped. It didn’t look like any was but I definitely got less solvent out than was added.

Recovering the NPS solution was difficult the first pull, SWIM had grabbed some of the mix and spilled some saturated NPS but recovered the majority, if not in the first pull, with later pulls. The NPS separation went fantastic, no emulsions, the NPS separated at the top in about 6 minutes as I said before.

What was the temperature? As I mentioned above this can have a big impact.

I placed the bottle in a heat bath of 125f.

How thick was the soup? I have had best results with at least 500ml of water to 100g of mimosa bark.

Soup was just like the one in cybs tek. Definitely not sludge, ~700ml liquid with 50g bark as instructed.

If it were me I would definitely try warming the solution and adding a bit more lye and possibly water if you have an especially thick soup and then doing another pull with everything at a higher temperature. I would be expecting at least 1g freebase from 50g bark.

I was definitely expecting the same. IIRC, it's been said the bottle shouldn't burn you when you pick it up, NPS only needs to be warm, not hot. SWIM assumed a heat bath of 120-130f was fine, (It also worked for the first pull, albeit .2g isn't much, it should be closer to .5-.6g.

Hopefully this is helpful troubleshooting information, do you have any suggestions for next time? Different bark? Different heat temps? SWIM can't exactly afford to lose any more product as MHRB/the rest is fairly expensive and time consuming.

 

[Asher7]

This is what I think I would do. For your dirty crystal I would just recreate an stb situation except throw crystal in instead of bark let it all get where it goes and then pull with solvent. I would try to get as much fat out as possible since it likes to sit right on the barrier of naphtha/lye water, which yours looks really white so that’s good. To do that I would just dissolve crystal in a shot glass with hot naphtha and let all the fat settle and pull saturated solvent with an eye dropper to freeze precip.

To figure out the bark I would do a simple stb with 100 grams of bark just to get an idea of what shows up with minimal steps that could potentially create loss. Just lye water soak, naphtha swirl and fan/precip/whatever you like. That’ll be your “control” if you want to think about it like that.

Anyone see flaws with that approach?

 

[Tony6Strings]

Thanks DmnStr8 and Pete666 for the recommend towards a pipette. I've been using a large plastic BD medical syringe, the solvent dries out the rubber and makes the plunger stick. It's a pain in the ass when it happens in the middle of a pull.

 

[Asher7]

You’re gonna smoke rubber I think.

 

[Tony6Strings]

You’re gonna smoke rubber I think.

Hash oil actually.

 

[Randomness]

I used to always do my pulls whilst everything was fairly warm as naphtha cannot hold as much when cold, hence the reason freeze precipitation works.

Questions I would ask are.

Did you use any acid stage? If so there could have not been enough lye added.

The acid stage was 60ml of vinegar dissolved in I believe 200g of water. 50g of lye was added in 200g water as well.

How did you mix the NPS with the base/ mimosa soup? Was it adgitated enough to contact the spice? Remember that once you have added lye the spice is no longer soluble in the aqueous solution. Basically the nps has to come into contact with the precipitated freebase.

The NPS was mixed with the mimosa soup by tilting upside down and upright slowly for 20-30s 4 times.

Did you recover all the NPS added or is some trapped within the bark as some kind of emulsion? I have had this happe before and got low yeild. Some of the solvent separated fully but the rest was trapped. It didn’t look like any was but I definitely got less solvent out than was added.

Recovering the NPS solution was difficult the first pull, SWIM had grabbed some of the mix and spilled some saturated NPS but recovered the majority, if not in the first pull, with later pulls. The NPS separation went fantastic, no emulsions, the NPS separated at the top in about 6 minutes as I said before.

What was the temperature? As I mentioned above this can have a big impact.

I placed the bottle in a heat bath of 125f.

How thick was the soup? I have had best results with at least 500ml of water to 100g of mimosa bark.

Soup was just like the one in cybs tek. Definitely not sludge, ~700ml liquid with 50g bark as instructed.

If it were me I would definitely try warming the solution and adding a bit more lye and possibly water if you have an especially thick soup and then doing another pull with everything at a higher temperature. I would be expecting at least 1g freebase from 50g bark.

I was definitely expecting the same. IIRC, it's been said the bottle shouldn't burn you when you pick it up, NPS only needs to be warm, not hot. SWIM assumed a heat bath of 120-130f was fine, (It also worked for the first pull, albeit .2g isn't much, it should be closer to .5-.6g.

Hopefully this is helpful troubleshooting information, do you have any suggestions for next time? Different bark? Different heat temps? SWIM can't exactly afford to lose any more product as MHRB/the rest is fairly expensive and time consuming.

Sounds like you did everything correctly, would have thought you should have ended up with a proper yield.

Only thing I can suggest is adding a bit more lye. Personally I never weighed mine I used to slowly add until I could no longer see any kind of reaction or colour change happening. That was with a magnetic stirrer though.

Was the bark powdered?

 

[dmt_awehhaea]

Thanks DmnStr8 and Pete666 for the recommend towards a pipette. I've been using a large plastic BD medical syringe, the solvent dries out the rubber and makes the plunger stick. It's a pain in the ass when it happens in the middle of a pull.

I won’t lie, SWIM did this with his rubber syringe used for ink too. Even without directly touching the rubber, It simply stopped moving and broke off, definitely a great way to ruin your syringe at the very least.

 

[dmt_awehhaea]

This is what I think I would do. For your dirty crystal I would just recreate an stb situation except throw crystal in instead of bark let it all get where it goes and then pull with solvent. I would try to get as much fat out as possible since it likes to sit right on the barrier of naphtha/lye water, which yours looks really white so that’s good. To do that I would just dissolve crystal in a shot glass with hot naphtha and let all the fat settle and pull saturated solvent with an eye dropper to freeze precip.

To figure out the bark I would do a simple stb with 100 grams of bark just to get an idea of what shows up with minimal steps that could potentially create loss. Just lye water soak, naphtha swirl and fan/precip/whatever you like. That’ll be your “control” if you want to think about it like that.

Anyone see flaws with that approach?

Cybs tek is essentially a STB with the salt/vinegar step added?

Unless temperatures weren’t high enough with the NPS, I don’t think the methodology was what screwed it up. All parts were measured carefully (even the naphtha, using 60g which is about equal to 50ml) and followed completely. SWIM is good at following directions, given they are informative enough.

I’m starting to think 120-130F wasn’t enough to pull the DMT. The first pull was done shortly after adding the lye, that certainly provided a heat boost the other pulls didnt have.

Even if that’s the case, why would the first pull have had such a low yield anyways? Assuming 5-10g lost of the 62ish g of Naphtha, the yield should have been higher? Very confusing!

 

[dmt_awehhaea]

Sounds like you did everything correctly, would have thought you should have ended up with a proper yield.

Only thing I can suggest is adding a bit more lye. Personally I never weighed mine I used to slowly add until I could no longer see any kind of reaction or colour change happening. That was with a magnetic stirrer though.

Was the bark powdered?

The only alterations or parts done that weren’t clarified was heat bath temperatures, evap, and freeze time (4-5hours rather than 12h)

The bark was indeed powdered finely with a nice dull purple/pink.

The evap step was done simply due to how unsaturated the NPS was. After pull 2, the third pull was evap from 60g to 20g, with the fourth going from 50g to 35ish g

Not one pull was cloudy until they were just taken out of the freezer (just temperatures I assume)

TL;DR: A sad SWIM ended up with just .200g of lye tainted product from 50g of bark.

 

[Tony6Strings]

@dmt_awehhea, I would stick to what you've been doing and just be a little more careful when separating the layers. You're already working with a solid tek and pulling some decent looking spice, your first picture looks just fine excepting the tiny bit of base you can see got through. Regarding yeild, in my own personal experience with the Cybs my first is never my largest yield. Usually my third is. Is this because the base takes a little time to work the magic out of the bark?

 

[dmt_awehhaea]

@dmt_awehhea, I would stick to what you've been doing and just be a little more careful when separating the layers. You're already working with a solid tek and pulling some decent looking spice, your first picture looks just fine excepting the tiny bit of base you can see got through. Regarding yeild, in my own personal experience with the Cybs my first is never my largest yield. Usually my third is. Is this because the base takes a little time to work the magic out of the bark?

Do you have any recommendations regarding heat breath temperatures? Is 120-130F enough? I wish I could hear from Cyb himself. Like you, I’m relatively stumped on what’s the issue.

 

[Tony6Strings]

"The mix throughout this tek should be warm not hot, a cycle of warming and leaving to room temp is best, NOT a constant hot temp". -Cybs Hybrid Salt Tek

My extraction is usually done over a few days. I get it going in the hot water bath before each pull, heat it not past the point where I can hold the extraction vessel and roll solvent without burning myself.