Tips to increase yield?

[Starman]

I've done a couple of extractions so far, but my field seems to be significantly less than what others are getting. Any tips for things I can do to increase yield would be extremely appreciated!

Here's my process:
1. Portioned out 100g of fine-powdered MHRB
2. Cantelmo's method of freezing and heating of the MHRB water to break down the cells (repeated 3x)
3. Separated the liquid into 2 mason jars with around 50g MHRB each
4. Slowly adding lab-grade Sodium Hydroxide pellets (about 20g to each jar) then left to cool to around room temp
5. Added around 200mL VM&P Naptha to each jar, circular motion "shake" until Naptha layer is no longer visible
6. Wait for clear layer separation, then repeated "stirring" step again a couple of times
7. Extract Naptha layer into a measuring cup
8. Pour extracted Naptha into a wide glass Pyrex dish
9. Left to freeze-precipitate for around 36 hours

Here is a photo of the yield I'm getting:

 

[Transform]

The likeliest explanation is that you have weak bark - but how many pulls are you doing? From your description it looks as though you only did a single pull. At room temperature you should be doing about 5 or maybe even more. That's 5 separate batches of fresh solvent, or at least re-used solvent that's had the DMT freeze-precipitated out of it.

 

[Starman]

The likeliest explanation is that you have weak bark - but how many pulls are you doing? From your description it looks as though you only did a single pull. At room temperature you should be doing about 5 or maybe even more. That's 5 separate batches of fresh solvent, or at least re-used solvent that's had the DMT freeze-precipitated out of it.

The one shown in the photo was the 2nd pull, but the first pull was pretty weak. I hadn't added enough base to raise the pH.

Are we able to talk about suppliers of bark on here?

 

[Transform]

Are we able to talk about suppliers of bark on here?

No we are not.

It could be that room temperature is too cold for your solvent to pull very much, which is possibly an effect of the exact composition of the solvent. You can try any of the following:

• slightly more naphtha per pull
• warmer pulls (with a warm water bath - no naked flames!)
• more pulls

The increase in yield between the first and second pulls could be considered a good sign - maybe a third pull would be better as well, in which case you can carry on pulling until the yield drops off.

 

[Ruffles]

Do FASA then convert to freebase in a mini A/B with minimal solvent. FASA at least let's you know when the solvent has been depleted by the lack of clouds. Plus you get all of the nonpolar back.

As I understand it, freeze precipitation of freebase is more efficient when you have very high concentrations which is best done by evaping some of the nonpolar.

 

[Brickwall_55]

I was going to post this but thought it wasn't of relevance but guess it might be now.
You want to evaporate enough that it goes cloudy when blowing on it then you know its saturated enough yea ?

Kinda like this

 

[MrGuano]

I used same technique, I got 0.7g from the first pull, what did you get? That's a big old dish.
I did a lot more rolling/stirring than Chris appeared to do, like every half hour over a few days.

 

[fractals4life]

If the second pull is always larger than the first then it sounds like a few more agitate / let it clear cycles are called for. Generally not enough time spent letting DMT dissolve into the NPS, and possibly the bark needs to be dissolved by the lye a bit more before first pull is made.

I keep pulling until the freeze yield is down to 30mg or less.

 

[Starman]

If the second pull is always larger than the first then it sounds like a few more agitate / let it clear cycles are called for. Generally not enough time spent letting DMT dissolve into the NPS, and possibly the bark needs to be dissolved by the lye a bit more before first pull is made.

I keep pulling until the freeze yield is down to 30mg or less.

I think the second pull was only greater yield because I had a better pH level in the soup. I added something like 7g more NaOH after the first pull. I was testing to see what the minimum amount necessary would be, to save on supplies. Turns out I should have been more generous.

I used same technique, I got 0.7g from the first pull, what did you get? That's a big old dish.
I did a lot more rolling/stirring than Chris appeared to do, like every half hour over a few days.

With 100g MHRB, correct? How much Naptha are you adding to your flask?

Do FASA then convert to freebase in a mini A/B with minimal solvent. FASA at least let's you know when the solvent has been depleted by the lack of clouds. Plus you get all of the nonpolar back.

As I understand it, freeze precipitation of freebase is more efficient when you have very high concentrations which is best done by evaping some of the nonpolar.

Not sure how to execute this process. Are there any good resources you can link to so I can check it out? Much appreciated!

 

[Transform]

Not sure how to execute this process. Are there any good resources you can link to so I can check it out?

The FASA Method - DMT-Nexus Wiki

wiki.dmt-nexus.me

 

[MrGuano]

With 100g MHRB, correct? How much Naptha are you adding to your flask?

Yes correct, I added 100ml.

 

[DancinDog]

I've done a couple of extractions so far, but my field seems to be significantly less than what others are getting. Any tips for things I can do to increase yield would be extremely appreciated!

Here's my process:
1. Portioned out 100g of fine-powdered MHRB
2. Cantelmo's method of freezing and heating of the MHRB water to break down the cells (repeated 3x)
3. Separated the liquid into 2 mason jars with around 50g MHRB each
4. Slowly adding lab-grade Sodium Hydroxide pellets (about 20g to each jar) then left to cool to around room temp
5. Added around 200mL VM&P Naptha to each jar, circular motion "shake" until Naptha layer is no longer visible
6. Wait for clear layer separation, then repeated "stirring" step again a couple of times
7. Extract Naptha layer into a measuring cup
8. Pour extracted Naptha into a wide glass Pyrex dish
9. Left to freeze-precipitate for around 36 hours

Here is a photo of the yield I'm getting:
View attachment 101235

I'm only a newbie too, but I had very good results using Cyb's Hybrid ATB "Salt" Tek. It uses vinegar, salt, lye, & naphtha. Maybe the vinegar & salt would improve your yields.

Here's the link:

Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki

wiki.dmt-nexus.me

 

[dustyforge]

I'm only a newbie too, but I had very good results using Cyb's Hybrid ATB "Salt" Tek. It uses vinegar, salt, lye, & naphtha. Maybe the vinegar & salt would improve your yields.

Here's the link:

Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki

wiki.dmt-nexus.me

Hi mate. I tried this yesterday and I got quite a few crystals and they were very white and grainy and look more like salt grains. Do you know if some of the salt used in the tek can re crystalise and end up in the end product?

 

[fractals4life]

Table Salt ( NaCl ) will not dissolve in NPS, so unless you're sprinkling it into your dish before putting it into the freezer then it shouldn't be salt.

A quick test would be to take a grain and see if it dissolves in a drop of water. DMT freebase will not noticably dissolve in water, salt or lye will.

 

[dustyforge]

Table Salt ( NaCl ) will not dissolve in NPS, so unless you're sprinkling it into your dish before putting it into the freezer then it shouldn't be salt.

A quick test would be to take a grain and see if it dissolves in a drop of water. DMT freebase will not noticably dissolve in water, salt or lye will.

Thank you mate ill try it when I get home later

 

[DancinDog]

I've done a few more extractions and tried recrystalizing. Since I have chosen to perform freeze cycles to the MHRB I realized that I could utilize 1-quart zip-loc freezer bags to simplify the freeze-thaw cycles.

My glass extraction vessels are 1-liter borosilicate cylinder-shaped water bottles, which will accommodate 100g of MHRB. Although they can handle the freeze-thaw cycles okay I realized that zip-loc bags, being thin & flexible, would make it quicker and easier to accomplish the multiple freeze-thaw cycles. The cycling is much faster because you can pull them from the freezer & place them directly into a warm water bath & the MHRB mass is surrounded by warm water. Then, they chill quickly by laying them out float on a cool countertop or placing them into a cool water bath before refreezing.

I just filled each bag with 100g of MHRB & 300ml of water & soaked them in a warm water bath. They can then be freeze-cycled as quickly as you want, or stored long-term in the freezer until needed. That frees up your glassware for extractions & also saves freezer space.

While reading through various threads here I learned about 50ml all-glass syringes that don't have rubber or plastic seals. They used SS blunt needles & are immune to acid, bases, solvents, and high temps. Someone also mentioned utilizing an inverted glass funnel with the syringe to collect solvent pulls. The mouth of my 1-liter bottle is 55mm, so I'll order a 50mm diameter funnel. That seems a lot simpler than a separatory funnel setup.

I've learned to deposit my NPS pulls into a small jar to aid in settling out any soup droplets that happen to get sucked up during the pulls. It settles out almost immediately, and then I transfer the NPS to a glass baking pan for freeze precipitating.

 

[razer420]

Heya lets resurrect this thread. Not getting crsytals. Not sure why. Did the stuff the way, you know man? Where's my christals? My ph.meter broke but its black. Added naptha.

 

[Transform]

Heya lets resurrect this thread. Not getting crsytals. Not sure why. Did the stuff the way, you know man? Where's my christals? My ph.meter broke but its black. Added naptha.

You might have to go into a bit more detail than that. Not to mention, try writing in coherent sentences (as highlighted in bold, no, I don't know what "did the stuff the way" is even supposed to mean!)

There's a goo thread in the FAQ section - and goo doesn't necessarily equate with poor yield. For a more rigorous treatment,there's the Minimum Polymer thread.

Getting a bit more systematic should help you with your extraction process, and maybe a few other things.