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simple titration, and dual solvent crystalization Options
 
dg
#1 Posted : 7/16/2010 5:14:28 AM
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DUAL SOLOVENT CRYSTALIZATION AND SIMPLE TITRATION
BY DG

begin extraction ala Foaf
(i will add some thoughts here: more base is better! also, recommend extreme blending with water and base (paint mixer on high ) about 24hrs before any np is added. this frees up the goodies, but minimizes emulsions.

image one:
this is for the average guy, no special equipment needed, see pic
besides any appropriate safety gear, gloves goggles etc

jars w' lids
coffee filters
cotton balls
acetone
water
pipette or baster or tubing
ph down sulfuric acid- pet store
crock-pot or pan and spark less hotplate combo is nice here
basic wide range ph papers
funnel
a freezer helps

lots of possible work arounds, or other improvements to gear, suction and better filtration, pipettes, lab glass etc, etc

image two:
1.pull CLEAN np from vessel, if cloudy or milky, add it back to the vessel with the polar, and wait until it clears up! or let set in jar over night and decant clear np before proceeding
2. add 1/2 cup water and
3. 20-40 drops of acid to the np.
shake well

image three:
it will look like this

image four:
3. with baster, suck up some of the water/emulsion layer, and let water pour over ph papers as it goes back into the salting vessel
4. continues adding drops of acid, shaking, and ph testing until ph 6-7 is reached

image five:
now its time to rid ourselves of the emulsion, i find heat to be the most effective fool proof method to do this. BE SAFE, SPARK-LESS, VENTILATION ETC!!!!

heat until the solution is clear, both the np, and salted layer
see image six

image six:
decant clear layer, a baster is fine.

image seven:
stuff a cotton ball tightly into the funnel, pre wet/ test the cotton ball, it shouls slowly filter thru, too fast is bad..
if its tight enough, the traces of np that might come along will float and the water only will come thru

image eight:
combine all saltings before proceeding,

add water to glass or stainless steel pan, fast boil it down.
notes: you want to remove as much water as possible w/o scorching product, i like medium heat on an average gas range.
as the concentration of the solution increases the sound the boiling makes changes, and it sounds syrupy. you may also notice the solution get cloudy(a sure sign you have gone far enough.
if you dont boil off enough, thats ok! but you will need to add more acetone see image nine to get it looking like image ten...

image nine:
let the solution cool a bit, and add acetone20-50% of solution, depending on concentrations.... it may boil rapidly, use caution

image ten:
when enough acetone has been added, the solution will get cloudy-the start of xtal formation

toss it in the freezer, crystals form overnight

image eleven:
in the morning it looks like this

image twelve:
while still freezing cold, filter thru funnel and coffee filter

image thirteen:
let filter dry for a day or so

image fourteen:
enjoy
additional notes,
re-use all solvents!!

dg attached the following image(s):
one.jpg (8kb) downloaded 3,000 time(s).
two.jpg (8kb) downloaded 2,959 time(s).
three.jpg (6kb) downloaded 2,874 time(s).
four.jpg (8kb) downloaded 2,856 time(s).
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six.jpg (6kb) downloaded 2,854 time(s).
seven.jpg (6kb) downloaded 2,843 time(s).
eight.jpg (7kb) downloaded 2,861 time(s).
nine.jpg (6kb) downloaded 2,851 time(s).
ten.jpg (6kb) downloaded 2,849 time(s).
eleven.jpg (4kb) downloaded 2,875 time(s).
twelve.jpg (8kb) downloaded 2,851 time(s).
thirteen.jpg (6kb) downloaded 2,866 time(s).
fourteen.jpg (7kb) downloaded 2,924 time(s).
 

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dg
#2 Posted : 7/16/2010 5:19:22 AM
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not sure why the pics came out that way...

questions?
fire away Smile
 
damiana
#3 Posted : 7/16/2010 7:12:49 AM

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Wow, that is crazy. So sulfuric acid in drops added to water to get the goodies from the NP solvent and then acetone added to water for freeze precipitation. Hmm. Is that pure mescaline then?
And the water freezes but the acetone doesn't right? Assuming all the mesc. went to the acetone from the heating step, you get crystal precipitation.

Wow!
PEACE
 
Mill
#4 Posted : 7/16/2010 7:41:23 AM

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Since acetone and water are miscible the water shouldn't freeze...I believe the idea is that adding acetone will lower the solubility of the alkaloid salts in water and cause them to precipitate.

dg- nice work! could this tek be applied to salts other than sulfate? Also the product looked quite clean...does this tek somewhat select for the meskal, while leaving most the impurities/other alkaloids in solution?
 
w0mbat
#5 Posted : 7/16/2010 11:18:59 PM

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1) Why was it necessary to add the acetone? I thought mescaline sulfate was insoluble in cold water & would have precipitated out on its own if left in the freezer

2) What was the starting material (Pedro/Torch/?)? How much? What was the weight of the final product?

3) Are you confident that the way in which you added sulfuric acid dropwise was enough to salt out all the freebase mescaline in the NP?
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i'm tellin ya, one day i'll interface a mass spec and uv-vis spectrophotometer to a modular synthesizer

 
narmz
#6 Posted : 7/18/2010 1:38:13 AM

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How are the effects of the sulfate salt? I've been curious about whether or not there would be noticeable side-effects from using sulfuric acid, and whether folks who are sensitive to sulfur would be unable to ingest it without irritation.
Everything I post is made up fiction. SWIM represents a character who is not based in or on reality.
 
dg
#7 Posted : 7/29/2010 4:43:29 AM
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damiana wrote:
Wow, that is crazy. So sulfuric acid in drops added to water to get the goodies from the NP solvent and then acetone added to water for freeze precipitation. Hmm. Is that pure mescaline then?
And the water freezes but the acetone doesn't right? Assuming all the mesc. went to the acetone from the heating step, you get crystal precipitation.

Wow!


1.yes, uniform crystal growth, consistant result, foafs lab test shows no other alkaloids or impurities present
2.no, the water/tone are miscible, and will not freeze if enough acetone is added to force precip
 
dg
#8 Posted : 7/29/2010 4:48:27 AM
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Mill wrote:
Since acetone and water are miscible the water shouldn't freeze...I believe the idea is that adding acetone will lower the solubility of the alkaloid salts in water and cause them to precipitate.

dg- nice work! could this tek be applied to salts other than sulfate? Also the product looked quite clean...does this tek somewhat select for the meskal, while leaving most the impurities/other alkaloids in solution?


see my last reply... basically, yes, leaving behind crud-yeilding pure needles of m.sulphate

the titration portion should be used with any salting, to prevent the gross over titration most teks cause, sorry over acidifying the np pulls crap, and makes for a pita of clan-up, or just plain crude extract.....

as for forced precip with other salts, play around with solubilities and solovents, many possible routes to precip exist
this one just works really well, and has easily repeatable consistant results Smile
 
dg
#9 Posted : 7/29/2010 4:55:02 AM
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w0mbat wrote:
1) Why was it necessary to add the acetone? I thought mescaline sulfate was insoluble in cold water & would have precipitated out on its own if left in the freezer

2) What was the starting material (Pedro/Torch/?)? How much? What was the weight of the final product?

3) Are you confident that the way in which you added sulfuric acid dropwise was enough to salt out all the freebase mescaline in the NP?



very astute questions the w0m...

1.m.sulphate never crashed out of cold water for me...if it did, it'd be hard to filter in a frozen lump!
2. material was mix from the garden, i have 50-100 different clones- not sure what to call pedro or torch though, lol. mostly pachs, bridges, and peruvians. yeild approx 10g. from "abit"of cacti........
3. yes, but always re-use the np, so if it did, it'd come out next run anyways
3.a. evapping np left crude brown powder with zero activity when bioassayed :wink
 
dg
#10 Posted : 7/29/2010 5:01:19 AM
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narmz wrote:
How are the effects of the sulfate salt? I've been curious about whether or not there would be noticeable side-effects from using sulfuric acid, and whether folks who are sensitive to sulfur would be unable to ingest it without irritation.


about the same as hcl, and citric ime, but takes a bit more than the hcl. i ate 250mg at the river this weekend, had a nice mild trip, 12hrs of swimming and rock-hopping joy

if the proper amount of acid is used its pretty well bound up(no free sulf ions floating around), seriously doubt it'd bother sulphur sensitive folks either way though.
good question i will ask my pharm friend when next we meet

everyone who has tried it found much much less stomach irritation than with other "dirty" salts for example
 
w0mbat
#11 Posted : 7/31/2010 5:09:07 AM

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dg wrote:


mage nine:
let the solution cool a bit, and add acetone20-50% of solution, depending on concentrations.... it may boil rapidly, use caution

image ten:
when enough acetone has been added, the solution will get cloudy-the start of xtal formation

toss it in the freezer, crystals form overnight


I have a few questions about dual solvent recrystallization:

1) All you do is make a concentrated solution of crude mesclaine hcl dissolved in water, and then add 20-50% of the water volume in acetone (i.e., if you have 1000 mL water, then add 200-500 ml acetone)?

2) How does this work? As you add acetone, does the solvating ability of the solution go from being like that of water closer to that of acetone? If so, why not add even more acetone? (since mescaline HCl would presumably be even more insoluble in the solution as it's solvating ability becomes closer to that of pure acetone)

3) Will this produce results that are significantly better (in terms of purity as well as yield) than washing 1-2x with acetone, and then 1x with 99% isopropyl alcohol?

4) I noticed that can of acetone appears to be from a hardware store. What are your thoughts on using technical grade acetone, rather than ACS acetone?
benzyme wrote:

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

 
benzyme
#12 Posted : 8/1/2010 2:58:40 AM

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sorry for the poor res, was taken from a camera phone. ultrasound-assisted recrystallization of sp extract in 60% acetone/40% water, in salted ice bath. the grackle will filter later
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w0mbat
#13 Posted : 8/1/2010 4:25:42 AM

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benzyme wrote:
sorry for the poor res, was taken from a camera phone. ultrasound-assisted recrystallization of sp extract in 60% acetone/40% water, in salted ice bath. the grackle will filter later




What does the ultrasound accomplish? I assume it helps with crystal formation, but do you know how & what else it does?

Also, is 60% acetone / 40% water the best ratio to use for recrystallization? Does that just apply to mesc sulfate, or would it also work for mesc HCl? (the reason I ask is b/c dg mentioned using around 20-50% acetone)
benzyme wrote:

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

 
benzyme
#14 Posted : 8/1/2010 5:16:30 AM

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the cavitation bubbles are thought to act as nucleation sites; collapse of the bubbles literally fuses crystals together.
the power is cycled such that intermittent pauses allow for periods of cooling. the process also cleans the crystals.

60:40 was just an arbitrary binary solvent ratio chosen, the point was to make it more acetone than water so it wouldn't readily freeze and the crystals could easily crash out. it should also work well for HCl.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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benzyme
#15 Posted : 8/1/2010 11:23:37 PM

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(bottom sample is the bird's, mp. 183 - 187)

compare with

benzyme attached the following image(s):
0801001719.jpg (197kb) downloaded 2,629 time(s).
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
XMR 46JqfBqi7JNM1W5rXXZ1FF1CBKKLoGEVBRya9Cn3RJmPbQhT4GeZpVKWbwaVe4vUMveKAzAiA4j8xgUi29TpKXpm3whx5MW
BTC 3CNrz6Tj17U35GLkRB1zsNtVoedorw8oja
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dg
#16 Posted : 8/3/2010 2:22:02 AM
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work for hcl salts even though they are very soluable in cold water?

ps, erowid could use some new pics eh?
 
benzyme
#17 Posted : 8/3/2010 2:48:31 AM

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wih HCl, you'd want to use cold ethanol (or isopropanol)/acetone binary mixture.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
XMR 46JqfBqi7JNM1W5rXXZ1FF1CBKKLoGEVBRya9Cn3RJmPbQhT4GeZpVKWbwaVe4vUMveKAzAiA4j8xgUi29TpKXpm3whx5MW
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dg
#18 Posted : 8/3/2010 3:13:14 AM
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fyi, the hcl will crash out of water just fine, if mek is used Smile
a slightly different approach is needed though,


a write up for another day---- recrystalization of dirty mesc.hcl using MEK and water---
 
benzyme
#19 Posted : 8/3/2010 3:19:16 AM

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mek, dmk (acetone).. not much difference. the salts are insoluble in either.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
XMR 46JqfBqi7JNM1W5rXXZ1FF1CBKKLoGEVBRya9Cn3RJmPbQhT4GeZpVKWbwaVe4vUMveKAzAiA4j8xgUi29TpKXpm3whx5MW
BTC 3CNrz6Tj17U35GLkRB1zsNtVoedorw8oja
ETH 0xd433198cb786145767c67d874b36cd7d42baf57a
 
damiana
#20 Posted : 10/7/2010 11:56:14 PM

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Question for the OP.

Couldn't one just add the acid drops directly to the water till that was at ph 7 ish and then add that to the NP?

SWIM is going to do this, and she is excited to get some white crystals this time.
PEACE
 
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