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Evaping white spirit? Options
 
SHroomtroll
#1 Posted : 11/3/2010 4:15:25 PM

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Before i found heptane in my groccery store Laughing i bought a gallon of white spirit not knowing how freaking heavy it is to evap...

So i did a few pulls with it before starting using heptane and barely pulled anything out of the solvent.

Problem is that it´s probably still way to much solution so i need to get the volume down.


Ive tried putting in front of a warm fan for a few hours but the stinkiness is to much, it smells in the entire appartment and even outside my window.


Any suggestions since i don´t wan´t to throw away this most likely dmt containing solvent.
 

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Trickster
#2 Posted : 11/3/2010 5:31:52 PM

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SHroomtroll wrote:
Before i found heptane in my groccery store Laughing i bought a gallon of white spirit not knowing how freaking heavy it is to evap...

So i did a few pulls with it before starting using heptane and barely pulled anything out of the solvent.

Problem is that it´s probably still way to much solution so i need to get the volume down.


Ive tried putting in front of a warm fan for a few hours but the stinkiness is to much, it smells in the entire appartment and even outside my window.


Any suggestions since i don´t wan´t to throw away this most likely dmt containing solvent.


As I wrote in a different thread:

Evaporation rate depends on the following:

1. The liquid temp.
2. Ambient air pressure.
3. Airflow over the liquid surface.
4. Surface area of the liquid.

Increasing any of the above will increase your evaporation rate.

If you evap it into the atmosphere, you cannot avoid the stink. The faster you evaporate it the stinkier it is.

A more professional solution to the problem would be to use a distillation setup, especially vacuum distillation setup. It is good for many reasons:
1. You will get most of your solvent back.
2. There will be no smell (almost).
3. It will be faster.

It is not that expensive. I've assembled mine for less than $30.
Do not seek the truth, just drop your opinions.
 
Methtical
#3 Posted : 11/4/2010 12:22:48 PM

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What kind of volume of white spirit are we talking here? In my experience it takes a long long time to evaporate, anything over 100mls is going to take an age - I trust you have tried freeze precipitation already?

Methtical
 
SHroomtroll
#4 Posted : 11/4/2010 1:11:34 PM

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it´s well over 300ml, and yes i already got some goddies out my freezing it, but i know there is alot left.

I´m thinking about putting it in front of a heat fan 1-2 hours per day very close to a open window, i have all the time in the world i just don´t to poison myself with the fumes...
 
Trickster
#5 Posted : 11/4/2010 1:59:30 PM

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SHroomtroll wrote:
... i have all the time in the world i just don´t to poison myself with the fumes...


So you decided not to poison yourself quickly, but over a long timeWink ?

Here is an idea to avoid evaping whitespirit completely:

1. Extract your spice from whitespirit with diluted acid (vinegar).
2. Basify the acidic solution.
3. Pull with Heptane.
4. Reduce combined pulls.
4. Freeze-precip.
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SHroomtroll
#6 Posted : 11/4/2010 2:30:31 PM

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Thanks you that sounds like an awesome idea, you really made my day with all your help...


It´s cool that the ansverto both my problems is A+B extraction Very happy
 
Trickster
#7 Posted : 11/4/2010 3:45:47 PM

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SHroomtroll wrote:
Thanks you that sounds like an awesome idea, you really made my day with all your help...


Glad to be of help. Just make sure that pH of your basic solution is around 11.5 - 12.5. Too low and your yield will suffer. Too high is a waste of lye. On the other hand, high pH helps to avoid emulsion. Do more smaller pulls rather than fewer big pulls. To be on the safe side I do 5 pulls. 3 is the minimum number.

If you have time, let your acidic solution settle. Decant and discard any solids that may crash out.
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SHroomtroll
#8 Posted : 11/4/2010 4:03:17 PM

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Will the acidic sollution mix with White spirit? or will i get two layers and discard one?
 
Trickster
#9 Posted : 11/4/2010 4:34:17 PM

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SHroomtroll wrote:
Will the acidic sollution mix with White spirit?


No. White spirit is practically inmiscible in water (<0.1%)
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SHroomtroll
#10 Posted : 11/4/2010 5:00:22 PM

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Ok cool so i will get one layer of white spirit that i should discard and one layer of acidic water that should contain the spice?
 
soulfood
#11 Posted : 11/4/2010 5:04:45 PM

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I had similar issues with white spirit. I actually kept the leftover solvent in a jar with the lid off almost a year ago and it's still in there.

Anyways, I did what trickster has outlined, only I used fumaric acid. I'd also recommend evaporating the acidic phase completely, then make the sodium carbonate paste which is then dried and then pull with the solvent. With the excess water you'll end up having to do more pulls than is necassary. Though if your only base to hand is lye it's probably better keeping that phase in solution.
 
Trickster
#12 Posted : 11/4/2010 10:21:34 PM

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soulfood wrote:
I had similar issues with white spirit. I actually kept the leftover solvent in a jar with the lid off almost a year ago and it's still in there.


White spirit has been developed in 1924 as a non-volatile cleaning solvent.

soulfood wrote:
... I'd also recommend evaporating the acidic phase completely, then make the sodium carbonate paste which is then dried and then pull with the solvent.


Interesting. Never tried this route. Can you suggest any andvantages over the one I suggested?

soulfood wrote:
With the excess water you'll end up having to do more pulls than is necassary.


You can always reduce the excess water as much as you want.

Working with basic phase I prefer aqueous solution rather than a paste, because I can measure its pH and not overbasify it. This will reduce extraction of unwanted substances that have pKa well above that of DMT.

Is there a simple tek to separate an NPS from a paste.

With liquid basified solution I use a traditional sep funnel that works very well. I can do 5 pulls in less than an hour.
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soulfood
#13 Posted : 11/4/2010 11:23:41 PM

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Using sodium carbonate you won't overshoot the pH.

The deal with the paste is it needs to dry and then be powdered so the whole process is probably much longer, but as the alkaloids have nothing to migrate into, less solvent is used. I use dry acetone come to think about it so if using naphtha/heptane etc I suppose you can extract from a paste without drying.
 
SHroomtroll
#14 Posted : 11/5/2010 2:11:01 PM

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I have now mixed vinegar and water 50/50 and mixed it with the white spirit, So now i have the acidic sollution in the bottom with the solvent on top.

So am i correct when i understand that the dmt alkaloids will go from the solvent to the acidic mix? how much vinegar do i need to make sure it don´t stay in the solvent.

Should i stir it? and how long should i have it in the jar?

I stil don´t have any good lye source (see my kaustik soda thread) but i will take a trip tomorow to a few hardware and paint shops.
 
Trickster
#15 Posted : 11/5/2010 6:24:02 PM

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SHroomtroll wrote:
I have now mixed vinegar and water 50/50 and mixed it with the white spirit,


Having a pH meter, I would use less vinegar, but that's OK.

SHroomtroll wrote:
So am i correct when i understand that the dmt alkaloids will go from the solvent to the acidic mix?


Yes.

SHroomtroll wrote:
how much vinegar do i need to make sure it don´t stay in the solvent.


I used a dozen ml to drop pH of 200 ml of water from 7 to 4. This should be enough. I deliberately keep pH at 4 or above in order to avoid extracting unwanted stuff.

SHroomtroll wrote:
Should i stir it? and how long should i have it in the jar?


Yes. Stirring helps to reach an equilibrum of distribution of extracted substance between the 2 solvents. If you stir all the time, I do not think you should keep it longer than 10-15 min.

I would do 3 washes, not just one.

SHroomtroll wrote:
I stil don´t have any good lye source (see my kaustik soda thread) but i will take a trip tomorow to a few hardware and paint shops.


Instead of lye you can make Sodium carbonate (a pretty strong base) at home by baking Sodium bicarbonate (baking soda) in an oven for a couple of hours. I do not remember the temp. Serch the forum, it is somewhere here.
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SHroomtroll
#16 Posted : 11/5/2010 9:32:35 PM

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Ok will try that, what happens if i let the acidic/solvent mix be in the same jar to long?

Edit: i looked up the sodium carbonate thing and have put 100g of Sodium Bicarbonate in the oven...

But i can´t find how much i should use formy mix, it´s about 3dl of liquid, more vinegar than water.
 
Trickster
#17 Posted : 11/5/2010 11:33:36 PM

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SHroomtroll wrote:
Ok will try that, what happens if i let the acidic/solvent mix be in the same jar to long?


I do not think it matters. Maybe longer is even better, especially if you do not want to stir it too much.

SHroomtroll wrote:
Edit: i looked up the sodium carbonate thing and have put 100g of Sodium Bicarbonate in the oven...

But i can´t find how much i should use formy mix, it´s about 3dl of liquid, more vinegar than water.


I do not know. Do you have some pH paper? Go for pH ~12 - 12.5.

I am running an extraction now and I've monitored how aqueous solution changes its colour in the process of basification.

- pH ~4 - the solution is clear dark burgundy.
- pH ~6 - it becomes thick, opaque and gray.
- pH ~8 - it gets less viscous, but still dark gray.
- pH ~10 - very dark gray and more fluid.
- pH ~11.5 - almost black and as fluid as the original acidic solution.

So, watch your basified solution color. Black is an indication that your pH is about right.
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SHroomtroll
#18 Posted : 11/6/2010 11:31:35 AM

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I made a sample with about 50% of my vinegar solution, i put a few teaspoons of my sodoium carboante in it and after some stiring and foaming it turned preety dark, almost black.

So Now i guess all that´s left is to try to pull with some solvent and hope for

1. high dmt precence

2. no soap.


So how can i optimise my solvent pulling to achieve some kind of compromise between these goals....

I have heptane at home, but ive read alot of peoplepulling with acetone when they use sodoium carbonate, which is betterfor me?

Also if i use heptane should i heat it?


Edit: after 30mins there has formed a black layer in the bottom and the rest of the sollution is still dark yellow/brownish,

i will try to add some more sodoim carbonate and stir...
 
 
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