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Mesc HCL Cleanup with Pics Options
 
futura
#1 Posted : 9/5/2010 11:33:26 AM

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OK here is the clean-up report.

Started with 450 Grams P.Torch

If you like you can go to this thread https://www.dmt-nexus.me...aspx?g=posts&t=15022
and scroll down to the first post by me with pics to see how I got to the point before clean-up.

I took the 4.1 Grams from the first picture below(All three piles) and divided among 4 shot glasses.

I added 20ml Freezing Cold Anhydrous Acetone to each shot glass,chopped up crystals with a butter knife,swirled around,covered glasses with foil and put back in freezer for five minutes. I then removed from freezer and sucked off Acetone with eye dropper. I did this twice and discarded acetone.

I added 20ml Freezing Cold Anhydrous(91%IPA which I dried with Baked Epsom Salts) Isopropyl Alchohol to each shot glass,chopped up crystals with a butter knife,swirled around,covered glasses with foil and put back in freezer for fifteen minutes. I then removed from freezer and sucked off IPA with eye dropper. I did this twice and discarded the first wash but saved the second.

I then filled the first shot glass with distilled water till crystals dissolved then added that water to second shot glass and swirled till crystals dissolved then dumped contents into Pyrex Pie plate,I did the same with shot glasses 3 and 4 and dumped that into pie plate as well. I placed fan blowing into pie plate and let evaporate for 12 hours till dry. I then scraped up crystals into center of pie plate,chopped them up and put pie plate into tupperware container filled with damp-rid and sealed lid and let further dry for 24 hours.

The second picture shows these washed crystals after 24 hours in the tupperware.

Total yield of this was 2.6 Grams

I lost about 37% total weight to the 4 washes.

I took the combined second IPA washes and put them on a plate and evaporated it in front of a fan for 12 hours and then scraped and chopped and into tupperware as above.

The third picture shows the evaporated crystals from the combined second IPA washes.

Total yield of this was was 350 mg

Also note:

I had problems recovering all the D-Limo as my french press broke.

I recovered 900ml out of 1350ml d-limo from my first 24 hour soak. I then added 1350ml more d-limo,soaked for 24 hours and only recovered 600ml. I then added 1350 more d-limo soaked for 12 hours and only recovered 100 ml as by then the powder had turned to paste!!

So my yield was low due to the fact I only recovered a portion of the total of D-limo used.

I think my initial salting pull was so large(Large Brown Pile in first and last pic) because I followed ron69s tek and the acid level I salted at was so low it pulled so much non-mesc alkaloids out...thats why it was so brown!!!

I think in the future I will salt as I did the second pull(Medium and Small piles in first pic)using 9 drops 10% Hcl to 200 ml water which gave me a starting hcl water ph of 3.00 and after adding to d-limo gave me a salting PH of 6.00 and salt at least 4 to 6 times per pull.

As you can see from the first pic(Small and Medium Piles) a PH of 6.00 salting pull gave me almost the same color mesc I got after I washed the nasty brown stuff(First Pic-Large Pile)I got from using ron69s teks suggestion of 5ml 10% hcl to 25ml water.

Ron69s Tek gave me a starting hcl water PH of 0.50 and after I added it to the limo it was a salting ph of 1.5...way too low for clean mesc..however if you are seeking a full-spectrum cactus experience that would be good for you cause it seemed to pull everything from the torch powder.

I was hoping to get White Powder from so much cleaning up but from reading posts on here that seems only possible with a Boiling MEK/Freeze Precipitation Recrystalization.

I have also read that the IPA wash pulls some stimulating,euphoric alks out of the Mesc HCL so I am going to try the washed stuff and then compare the effects with the IPA evaped stuff mixed back in to the washed stuff at the same ratio it was before the second IPA wash(260mg washed stuff compared to 260mg washed+35mg IPA evap stuff.)

I understand the Acetone pulls all the sedating alks which I really dont want...Im hoping the Acetone got the nauseating alks out as well as i really dont want that!!

The fourth pic shows the twice Acetone and twice IPA washed pile in the same dish with the evaporated IPA second wash pile so as to compare colors of each.

The fifth pic shows a close up of the medium unwashed pile from the first pic which was the PH 6.00 salted pile scraped from the outer edges of evaporation dish,it weighed 640mg.

The sixth pic shows a close up of the small unwashed pile from the first pic which was the PH 6.00 salted pile scraped from the center of the evaporation dish,it weighed 160mg

The last pic shows a closeup of the large unwashed pile from the first pic which was the PH 1.50 salted pile,it weighed 3.3 grams

Any comments welcome...
futura attached the following image(s):
P1010004.JPG (59kb) downloaded 499 time(s).
P1010008.JPG (60kb) downloaded 500 time(s).
P1010002.JPG (59kb) downloaded 499 time(s).
P1010011.JPG (59kb) downloaded 499 time(s).
Unwashed 4.JPG (58kb) downloaded 488 time(s).
Unwashed 5.JPG (58kb) downloaded 488 time(s).
Unwashed 3.JPG (60kb) downloaded 486 time(s).
 

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dg
#2 Posted : 9/5/2010 4:15:08 PM
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i think clean ups should be much simpler...
An easy re crystalization of hydrocloric or sulfuric:
add dried crystals to hot acetone or mek, add drops of water until all the crystals are totally dissolved, simmer on low heat to reduce a bit
pop back in freezer
bam- forced precip- now filter perfect needled of mescaline
 
futura
#3 Posted : 9/5/2010 10:12:21 PM

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dg wrote:
i think clean ups should be much simpler...
An easy re crystalization of hydrocloric or sulfuric:
add dried crystals to hot acetone or mek, add drops of water until all the crystals are totally dissolved, simmer on low heat to reduce a bit
pop back in freezer
bam- forced precip- now filter perfect needled of mescaline


Would only the mesc crash out or would any of the non-mesc alkaloids crash out as well??

Wouldnt the water added freeze solid in the freezer or would the acetone or mek keep it liquid??

Should the acetone or mek be dried first to allow as little water as possible to freeze, or is that a waste of time since water is added later??
 
dg
#4 Posted : 9/6/2010 4:16:41 AM
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futura wrote:
dg wrote:
i think clean ups should be much simpler...
An easy re crystalization of hydrocloric or sulfuric:
add dried crystals to hot acetone or mek, add drops of water until all the crystals are totally dissolved, simmer on low heat to reduce a bit
pop back in freezer
bam- forced precip- now filter perfect needled of mescaline


Would only the mesc crash out or would any of the non-mesc alkaloids crash out as well??

Wouldnt the water added freeze solid in the freezer or would the acetone or mek keep it liquid??

Should the acetone or mek be dried first to allow as little water as possible to freeze, or is that a waste of time since water is added later??


only uniform needles form, yes jest mesc forms,

if more water vs tone is used, it can freeze, but usually no
no need to dry tone or mekSmile
but save the resulting liquid, add to next extraction, in my tests about 2-5% losses otherwise
 
Virola78
#5 Posted : 9/6/2010 5:11:47 PM

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Nice pics. Looks like your in for some fun : )
also nice and detailed write-up..

I was wondering, if the pH should be higher to prevent unwanted alkaloids to be pulled, wouldnt that (higher pH) also limit the amount of mesc that is pulled? I mean would the resulting unwashed product be better quality (more pure) but less quantity?

Can somebody with solid knowledge of chemistry pls say this will not be the case?? : )

Also, i would like to point out a common mistake:
> 5ml 10% HCl + 25ml water will not provide 2% HCl.
I think the original 69ron tek suggests adding water to 5ml 10% HCl until a total volume of 25ml is reached --> 2%

btw i usually weigh my solutions (weigh 5g of 10% HCl. then add water until 25g) edit: ofc bigger volumes will be measured (weighed) for doing multiple saltings.

“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
futura
#6 Posted : 9/7/2010 4:07:37 AM

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Virola78 wrote:
Nic

I was wondering, if the pH should be higher to prevent unwanted alkaloids to be pulled, wouldnt that (higher pH) also limit the amount of mesc that is pulled? I mean would the resulting unwashed product be better quality (more pure) but less quantity?



At a PH of 5.4 100% of all Mesc alkaloids are pulled...however you also pull non-mesc alkaloids

At a PH of 6.00 95% of all Mesc alkaloids are pulled and approx 5% non-mesc alkaloids are pulled.

At a PH of 7.00 approx 80% of all Mesc alkaloids are pulled and aprox 0% non-mesc alkaloids are pulled.

So there is a trade off...

at 5.4 you get all the mesc but it must be cleaned a lot leading to yield loss...

at 7.0 you get almost 0% non-mesc alkaloids but alot of the mesc alkaloids are not pulled...

at 6.0 you get virtualy all the mesc alkaloids and almost no non mesc so it only needs minimal clean-up

So in conclusion I think 6.0 is best...as it leads to most yield even after minimal clean-up.

Unless you are going to do a boiling MEK/Freeze precipitation I would go with a ph of 6.00 for maximum yield/minimun clean-up...

If you are going the boiling MEK/Freeze precipitation recrystalization method to clean up than id go with ph 5.6 as you will get maximum yield/highest purity this way.

The purer the mesc alkaloids you start with the easier the clean up is...

Also if one is seeking all alkaloids by all means do ron69s suggestion of 5ml 10% hcl to 25 ml water...that seems to pull everything out including the kitchen sink...

Remember also its not the PH of the HCL water before mixing with the d-limo that im refering too...Its what PH the HCL water will become after mixing with the D-Limo...

The pH of the d-limo gets basic because it has some bases dissolved in it; the bases are the alkaloids. Alkaloids are basic molecules ("alkaloid" means alkaline-like or basic-like). So when you salt out with your acid it is normal for the pH to go up, since some of the acid is getting neutralized by the basic alkaloids. The result of this (partial) neutralization is a salt as it always happens when an acid reacts with a base. In our case the salt is the alkaloid salt! (be it mescaline hydrochloride or mescaline acetate or whatever)..



NOTE: All of the above numbers are approximations...
They are purely estimations based on my trials and those of others that were posted on here and many other places...I must have read like over 1000 posts so far this month alone!!!
 
dg
#7 Posted : 9/7/2010 4:21:19 AM
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pretty good grasp for the most part there F Smile
you make some assumptions i doubt you've tested though
 
futura
#8 Posted : 9/7/2010 7:04:55 AM

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dg wrote:
pretty good grasp for the most part there F Smile
you make some assumptions i doubt you've tested though


Thats why I used APPROX in some of my resonses as they are purely estimations based on my trials and those of others that were posted on here and many other places...I must have read like over 1000m posts so far this month alone!!!
 
Virola78
#9 Posted : 9/7/2010 4:31:31 PM

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Thx for reply.
Where did you get such wisdom about solubility mesc at different pH?

Anyways, next time i will do 2 different pH for comparison (pH 69ron tek vs pH 6.0)
Always like to see what happens if i ... : )


“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
dg
#10 Posted : 9/8/2010 1:44:16 AM
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futura wrote:
dg wrote:
pretty good grasp for the most part there F Smile
you make some assumptions i doubt you've tested though


Thats why I used APPROX in some of my resonses as they are purely estimations based on my trials and those of others that were posted on here and many other places...I must have read like over 1000m posts so far this month alone!!!


sorry if that sounded like a put down!
i was trying to compliment you, for info gathered by reading, you did a very nice job explaining it!!! KUDOS
thanks for the help spreading accurate info Smile
 
dg
#11 Posted : 9/8/2010 1:46:39 AM
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Remember also its not the PH of the HCL water before mixing with the d-limo that im refering too...Its what PH the HCL water will become after mixing with the very Basic(PH 12.85) Cactus/Lile/Water mixture

to be clear, its the ph of the water/np mix, not the cacti/lye mix
 
dg
#12 Posted : 9/8/2010 1:48:18 AM
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also, have you tried the mek or tone "crash" yet
results are AWESOMESmile
 
w0mbat
#13 Posted : 9/8/2010 3:16:32 AM

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Thx for posting futura - we need more people to test assumptions and post data. Well done Smile
benzyme wrote:

i'm tellin ya, one day i'll interface a mass spec and uv-vis spectrophotometer to a modular synthesizer

 
futura
#14 Posted : 9/8/2010 3:44:22 AM

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dg wrote:
also, have you tried the mek or tone "crash" yet
results are AWESOMESmile

Havent tried that yet...will do it next extraction and post results...I am going to do an mek wash on 1 gram of the acetone/ipa washed stuff just to see if it cleans up further...

Oh and also I didnt think you were criticizing me in your earlier post I just wanted to make sure everyone reading my posts understand these are approximations as I dont have access to chromatography equipment to be certain 100% about the numbers...

And yes I also wanted everyone to know that PH numbers of HCL water are AFTER adding to your limo,naptha or whatever pulling solvent you are using...

The pH of the d-limo gets basic because it has some bases dissolved in it; the bases are the alkaloids. Alkaloids are basic molecules ("alkaloid" means alkaline-like or basic-like). So when you salt out with your acid it is normal for the pH to go up, since some of the acid is getting neutralized by the basic alkaloids. The result of this (partial) neutralization is a salt as it always happens when an acid reacts with a base. In our case the salt is the alkaloid salt! (be it mescaline hydrochloride or mescaline acetate or whatever)..
 
dg
#15 Posted : 9/8/2010 3:53:47 AM
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futura wrote:


Oh and also I didnt think you were criticizing me in your earlier post I just wanted to make sure everyone reading my posts understand these are approximations as I dont have access to chromatography equipment to be certain 100% about the numbers...
...


thanks, i know i can be a bit harsh at times!
if you have trouble with dual solovent crash-out, let me know Smile
 
Virola78
#16 Posted : 9/12/2010 9:39:58 AM

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futura wrote:
...I am going to do an mek wash on 1 gram of the acetone/ipa washed stuff just to see if it cleans up further...


Did the mescaline-HCl dissolve in the MEK?
was it 99% mek? what temperature?

I have understood that if one is going to use MEK for purification of mesc-HCl,
then one should recrystalize (using warm MEK) not wash.

“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
 
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