Strange pulls... {pics}

[jbark]

So I have been walking 6 friends through an extraction from 333g of MHRB. Why 333? 1/3 of a kilo, which is the total of what we have, and 333 is the simplest fraction to extract given the size of the container I have.

Everything proceeded perfectly, and I freeze precipitated the first two pulls, and then pulls 3 and 4 separately. I separate them in order to see the progress, and in twos so that my final 5th pull is also separate so that I can evaluate if more pulls are necessary (they never have been). This time, however, each pull batch was very different:

The first (pulls 1 & 2) left a thin white crispy film (photos 1 & 2 below) and made me a little nervous - really didn't look like much product, and no visible crystallization.

The second (pulls 3 & 4) was replete with fluffy white crystals and seemed to have a much higher yield than pulls 1 & 2... (pics 3 & 4)

The third little bowl (pics 5 & 6) I put on the stove (not on, of course!) so that I could use the hood fan to ventilate the fumes (as I did with all the pulls as I decanted and collected them in the final pyrex dish) and within 10 minutes it had gone the milky yellow you can see in the pic! (I must note that this pull was from the recycled naptha from pulls 1 & 2, so may have had some prior saturation). When I freeze precipitated this bowl (in the same freezer, same temp), yellowish crystals crusted the bottom of the bowl, giving by visual estimation maybe half to two-thirds the yield from pulls 3 & 4, and quite a bit more than pulls 1 & 2! The yellow colour may be normal from a later pull, or from the reused NPS I suppose...

Of course, now I am going to do at LEAST a 6th pull, which I have never needed to do before. And maybe even a 7th!

So the mysteries are:

-why did pulls 1 & 2 yield a thin powdery crust, with very little yield?
-why were pulls 3 & 4 (and 5) superior yields (by eye, of course, nothing has been scraped and weighed yet) to the first two pulls? I have never seen this...
-why did pull 5 go milky so fast, with very little solution lost to evaporation? (there was no temperature change either...)
-why the yellow in only pull 5? The reused NPS? Is it pulling more alkoloids now in the later pulls? I suspect it may be for both these reasons.

I don't know if anyone has any cogent answers, but if not, this thread will at the very least be a curiosity for others!

Cheers,

JBArk

EDIT: I should note the pulls were all done with 175 mls of naptha, scaled up to compensate for the large amount of MHRB and the volume of solution (roughly 4-5 litres); and that all pulls were done at room temp, with NPS at room temp.

 

[DoingKermit]

I can't answer all your questions, J.... however, I can say that I have had the milky white film (shown in first pic) many times. I can assure you, although not pretty clumps of crystals, it is still just as potent. I think it has to do with putting the NPS in the freezer while it is still fairly warm.... that's merely an educated guess though and could easily be wrong.

 

[jbark]

I can't answer all your questions, J.... however, I can say that I have had the milky white film (shown in first pic) many times. I can assure you, although not pretty clumps of crystals, it is still just as potent. I think it has to do with putting the NPS in the freezer while it is still fairly warm.... that's merely an educated guess though and could easily be wrong.

Maybe, but I never heat my naptha. I have never needed to and my yields have always been 1.7-2.1%. Everything was room temp... (I just added this info to the edit section of the OP)

JBArk

 

[jbark]

No other ideas out there? Chemist-folk?

Cheers,

JBArk

 

[User1911]

Although I can not say why it happens but it't normal, remember DMT is a molecule which means its extremely small. So although your eye sees it as film there really just dmt molecules. Looks like film but when scraped it turns to xtals. You may even notice amber goo which is also normal. Every extraction and pull will be different but in the end its the same result.

So don't try racking your brain over looks, A lot of factors come into play just enjoy it..

Nice work.

 

[Spiritofspice]

How olds your bark.

 

[Entheogenerator]

So the mysteries are:

-why did pulls 1 & 2 yield a thin powdery crust, with very little yield?
-why were pulls 3 & 4 (and 5) superior yields (by eye, of course, nothing has been scraped and weighed yet) to the first two pulls? I have never seen this...
-why did pull 5 go milky so fast, with very little solution lost to evaporation? (there was no temperature change either...)
-why the yellow in only pull 5? The reused NPS? Is it pulling more alkoloids now in the later pulls? I suspect it may be for both these reasons.

What was the time-frame of your pulls?
Like:
T+ 0:00 hr - Basified
T+ ? hr - Pull #1
T+ ? hr - Pull #2
T+ ? hr - Pull #3
etc.

If you were going the STB route (which to me seems likely due to the large volume of solution), I believe the lye may take some time to break down the bark and release the DMT. I have noticed in past STB extractions that if I do my first pull immediately after basifying, it yields less than the next few pulls. But if I wait an hour after basifying before adding NPS, a la Noman's suggestion, my first pull picks up >1/2 of the total yield.

I think the same goes for the impurities that cause the yellow coloration, but it takes longer for them to be released. Typically if I do my first 3 pulls all in a row an hour after basifying the first is the whitest, the second is just slightly yellow-tinted, and the third is just slightly more yellow-tinted than the second. But the times that I have done the first pull the same night as basifying and then one pull a day from there on out, each pull is significantly more yellow than the last.

The used naphtha may have also had something to do with it, as you suggested.

I'm not sure why the one pull became cloudy so quickly, it does seem odd... :?:

 

[jbark]

So the mysteries are:

-why did pulls 1 & 2 yield a thin powdery crust, with very little yield?
-why were pulls 3 & 4 (and 5) superior yields (by eye, of course, nothing has been scraped and weighed yet) to the first two pulls? I have never seen this...
-why did pull 5 go milky so fast, with very little solution lost to evaporation? (there was no temperature change either...)
-why the yellow in only pull 5? The reused NPS? Is it pulling more alkoloids now in the later pulls? I suspect it may be for both these reasons.

What was the time-frame of your pulls?
Like:
T+ 0:00 hr - Basified
T+ ? hr - Pull #1
T+ ? hr - Pull #2
T+ ? hr - Pull #3
etc.

If you were going the STB route (which to me seems likely due to the large volume of solution), I believe the lye may take some time to break down the bark and release the DMT. I have noticed in past STB extractions that if I do my first pull immediately after basifying, it yields less than the next few pulls. But if I wait an hour after basifying before adding NPS, a la Noman's suggestion, my first pull picks up >1/2 of the total yield.

I think the same goes for the impurities that cause the yellow coloration, but it takes longer for them to be released. Typically if I do my first 3 pulls all in a row an hour after basifying the first is the whitest, the second is just slightly yellow-tinted, and the third is just slightly more yellow-tinted than the second. But the times that I have done the first pull the same night as basifying and then one pull a day from there on out, each pull is significantly more yellow than the last.

The used naphtha may have also had something to do with it, as you suggested.

I'm not sure why the one pull became cloudy so quickly, it does seem odd... :?:

Good guess but nope - A/B:

In acid 36 hrs before filtering, basified, then base solution readjusted to break emulsion with more lye then salt. 1st pull and 2nd within an hour of each other. Pulls 3 & 4 two days later, pull 5 three days after that.

I will do another pull in the next few days and report back. Thanks for the feedback - the 5th pull may be a combination of time between pulls and the used naptha factor. I should have noted in the OP that it was an A/B and not an STB...

Cheers,

JBArk

 

[jbark]

Although I can not say why it happens but it't normal, remember DMT is a molecule which means its extremely small. So although your eye sees it as film there really just dmt molecules. Looks like film but when scraped it turns to xtals. You may even notice amber goo which is also normal. Every extraction and pull will be different but in the end its the same result.

So don't try racking your brain over looks, A lot of factors come into play just enjoy it..

Nice work.

Yes, but getting a higher yield with later pulls is fishy... and I have never had a thin powdery film type pull before...

@Spiritofspice: bark was one week old from acquisition, and where I acquired it from was local and they had acquired it direct from source (Brazil) one week earlier. Without knowing its full history, I suspect it is probably the freshest bark I have ever put my hands on. Quality will be revealed when I tally the yield. (my yields are usually in the 1.7-2.1% range) 8)

Cheers,
JBArk

 

[Du57mi73]

Maybe the surface area of the pan was too big for the amount of dmt that was in the naptha so that when it dropped out it didnt form crystals, but instead a small thin layer. Ive had a similar situation but from different circumstances. When i dry my naptha to completion(after re-x), i always tilt it on its side. By doing this it assures that a very small % of dmt is always going to be deposited as the naptha slowly evaporates down the pan. This is what causes a powdery film for me. So i thats why i think that.

Have you scraped it up? Was it active? What was the consistancy after scraping?

 

[Entheogenerator]

Good guess but nope - A/B:

In acid 36 hrs before filtering, basified, then base solution readjusted to break emulsion with more lye then salt. 1st pull and 2nd within an hour of each other. Pulls 3 & 4 two days later, pull 5 three days after that.

I will do another pull in the next few days and report back. Thanks for the feedback - the 5th pull may be a combination of time between pulls and the used naptha factor. I should have noted in the OP that it was an A/B and not an STB...

Cheers,

JBArk

Well that's what I get for assuming things!

So, something similar to one of cyb's teks? Was heat used for the acid soaks?

I think the ideas about the thin film related to the surface area of the pan sound like solid theories, and I have seen something similar in the past. If crystalline particles are small enough, they look like a powder to the naked eye.

 

[jbark]

So, something similar to one of cyb's teks? Was heat used for the acid soaks?

I think the ideas about the thin film related to the surface area of the pan sound like solid theories, and I have seen something similar in the past. If crystalline particles are small enough, they look like a powder to the naked eye.

My own tek, A/B (basically a conglomerate of a bunch of other teks) No heat for acid soaks or for NPS - as stated above, I have never felt the need to complicate things with seemingly unnecessary steps as my yields have always been in the 1.7-2.2% range.

The pyrex dish for pulls 1 & 2 was identical to that used for pulls 3 & 4 so the surface area should be identical. Exactly the same conditions were present for all pulls and subsequent freeze precipitation - the only difference being that they were done several days apart. And 1 & 2 is a fine powder and 3 & 4 white, fluffy semi-spherical crystals...

Mysterious, I know!

Cheers,
JBArk

 

[Du57mi73]

What was the weight of pulls 1/2 vs pull 3/4?

 

[jbark]

What was the weight of pulls 1/2 vs pull 3/4?

I'll have to get back to you on that one. I am walking 6 people through the steps (teaching them to fish 8) ) and co-ordinating schedules has been tricky, so the pyrex dishes are covered in a cool dry place until we can all find the time and get together for a razor scrape and weigh fest. Hopefully within the next week...

Cheers,

JBArk

 

[Du57mi73]

They must see the xtal porn. it truely is beautiful.

 

[jbark]

So I got most of the gang together last night for a crystal scrapefest. The results:

Pulls 1 & 2: 1.7g

Pulls 3 & 4: 1.5g

Pull 5: 0.8g

total: 4g

There is definitely more DMT in the MHRB base soup, so I will do at least one more pull. The strange thing is that Pulls 1 & 2 (the thin powdery like film one) scraped up in flakes and did not smell like DMT. Perhaps traces of DMT odour, but nothing compared to the other pulls. Its smell was decidedly neutral...

I kept The yield from 1 & 2 separate and will re-x it to see what I get...

If I get another 0.5g out of the soup and then re-x the whole batch I will be likely just over 4g of product from 333g MHRB (1.4 %)- probably my worst yield ever. I have 2 x 333g of the same MHRB left which I will do in 2 batches and compare to se if my yields are consistent.

I still don't know what could possibly have happened to the first two pulls...

Cheers,

JBArk

 

[cyb]

Throw a pile of Salt in the mix JB...you could get lucky on the next pull.:thumb_up:

 

[jbark]

Throw a pile of Salt in the mix JB...you could get lucky on the next pull.:thumb_up:

A pile was thrown in early on. Will more salt basify more of the DMT for subsequent pulls? I have never heard of this, but I'll try it!

thanks!

JBArk

 

[DoingKermit]

The strange thing is that Pulls 1 & 2 (the thin powdery like film one) scraped up in flakes and did not smell like DMT. Perhaps traces of DMT odour, but nothing compared to the other pulls. Its smell was decidedly neutral...

I know I mentioned that I too have had the "white film" occur in the past. I also remember it not having much odour to it... however... my goodness was it potent! Not sure why it smells less than clumps, but I can confirm it is just as powerful (that's if we indeed had the same issue).

 

[Du57mi73]

Throw a pile of Salt in the mix JB...you could get lucky on the next pull.:thumb_up:

A pile was thrown in early on. Will more salt basify more of the DMT for subsequent pulls? I have never heard of this, but I'll try it!

thanks!

JBArk

Salt will not basify anything. Salt just makes it so that your dmt is more attracted to the naptha.