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Tetrachloroethylene and Heptane. Options
 
Heulas
#1 Posted : 5/12/2017 1:30:10 AM

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I found a solvent containing 25-45% tetrachloroethylene and 75-100% heptane.

I've heard that heptane work wonderfully for DMT extraction, and so does TCE, but i'm worried about one little detail:

Isn't going to be sitting on the bottom of my solution as it is more dense than whater?
How much is this a problem?
 

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AcaciaConfusedYah
#2 Posted : 5/12/2017 1:57:23 AM

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DO you already have the solvent? Since the percentage of product seems to be varied in the ratio of heptane to TCE, it would be nice to test a small amount in some water and see what happens. It is most likely to be that there are only two layers due to the miscibility of heptane and TCE. If that is the case, then it could be that you form one layer of organic solvent either above or below the aqueous layer depending on the amount of TCE.

If there are three layers of separation, then the heptane will be on top, aqueous in middle, and TCE below.

the best thing to do, if you are determined to use this solvent, is to test it on some basified water and see how it separates.

Sometimes it's good for a change. Other times it isn't.
 
Sore
#3 Posted : 5/12/2017 3:57:59 AM

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Not really sure what is meant by the post but if it helps I saw you can use epsome salt (once processed) to absorb water in Acetone to make anhydrous acetone I know they're completely different but maybe you can apply the same principle if you need something pulled to the bottom of the solution?

Sorry if I've wasted your time
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Mindlusion
#4 Posted : 5/12/2017 1:44:47 PM

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its misicible. you wont get 3 layers. where you find the layer will depend on the density of the mixture

if its only 25% TCE then its probably still less dense than water. But its pretty dense so maybe not.

if not, just add more heptane or naptha or toluene or any NP to bring it up to the top.

i experimented with mixtures of xylene and CH2Cl2, at the right ratio you can get the density of exactly the same as water so it forms spherical globs in the middle of the solution, pretty cool. Then keep adding xylene it forms a top layer. This mixture was also seemed to be more efficient at extracting DMT than xylene alone, but not really remarkable.

if you do an A/B extraction, its actually preferred to have the solvent sink to the bottom, its easier to separate with a separatory funnel, as well as a turkey baster pipette. Only in STB extractions you can't do this because the bark material and sediments will get into it
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Ulim
#5 Posted : 5/12/2017 9:46:56 PM

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Sore wrote:
Not really sure what is meant by the post but if it helps I saw you can use epsome salt (once processed) to absorb water in Acetone to make anhydrous acetone I know they're completely different but maybe you can apply the same principle if you need something pulled to the bottom of the solution?

Sorry if I've wasted your time
Embarrased


In this case the post just asks where the solvent will be.
Normally naptha floats on top because its less dense than water. But in this case its not naptha.
Its heptane (Part of naptha) and TCE (Chlorinated ethylene) Chlorine is mightly fat so its roughly ~1.6 the density of water.

The question asked here what will happen if you try to use it for pulling.
Will it be on the bottom, top or will the heptane seperate from the TCE forming a bottom and top layer?

What you said doesnt apply here. What your thing is is drying solvents. In this case its not importan tho because heptane and TCE dont mix with water.

If you add epsom salt here it will just dissolve in the water and not do anything but increase the water density.
 
Heulas
#6 Posted : 5/13/2017 12:01:08 AM

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Thank you all, guys.

Mindlusion wrote:
if its only 25% TCE then its probably still less dense than water. But its pretty dense so maybe not.

if not, just add more heptane or naptha or toluene or any NP to bring it up to the top.



Well, this is a pretty nice and effortless idea, but i have some doubts:

Let's say, for example, i would like to pull with 50 ml of TCE+Hep, and the solvent on the bottom problem shows up:

- Add more solvent (not TCE), mix, and see if it solves the problem.
- If not, add more solvent.
- If solvent exceed a ml threshold (e.g: 30 ml) you can go two ways, as using 70 ml of solvent could get pricey and wasteful:

1) Get a separatory funnel.
2) Stick to a solvent who does not contain TCE.

Guess i have to experiment.



Anyway, really can't get why the % of the compunds could vary so much:

How come it's said to be 25-45% / 75-100%?

I guess it's because of the manufacturing:

More precise percentages probably mean more effort in the making, more effort mean more costs, and a more pricey final product to sell to just common people.
 
Ulim
#7 Posted : 5/13/2017 12:13:12 AM

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Heulas wrote:


1) Get a separatory funnel.
2) Stick to a solvent who does not contain TCE.



Just use naptha man. Freeze makes for great recyclability.
 
Mindlusion
#8 Posted : 5/13/2017 5:02:51 AM

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Ulim wrote:
Heulas wrote:


1) Get a separatory funnel.
2) Stick to a solvent who does not contain TCE.



Just use naptha man. Freeze makes for great recyclability.


naphtha has the same problem of needing high volumes, 50mL quickly turns into 400ml after so many pulls, and its necessary to extract many times because naphtha is a poor solvent for dmt. And no one wants to freeze precipitate a single extraction 5 times, an incredible excessive amount of work , even just a few times.

this is just my experience as someone who does extractions everyday from reactions or from otherwise plants. It is a painfully slow and inefficient method. I prefer to use CH2Cl2 or xylene, besides the separatory benefits, to extract DMT because >90% is extracted in the first pull and virtually all of it in the second pull. All of the dmt is easily recovered within hours by salting out as the fumarate salt, and then the NP can be reused. Multiple grams are obtained with just 50mL solvent. in this hours upon days of time is saved, as well as solvent use is minimized.

In this way it is actually greener, even though tetrachloroethylene, while an excellent solvent, is a persistent pollutant. Definitely do an evap test and definitely salt out the alkaloids if you are going to use this solvent, don't evaporate it into the environment.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Heulas
#9 Posted : 5/13/2017 11:24:31 AM

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Not sure about what you said:

You suggest that for a matter of saving and pollution, to salt out the freebase from the solvent, and then just store the solvent until reusing for another extraction.

Then, if wanted, transform back fumarate to freebase, is this correct?
 
Heulas
#10 Posted : 5/14/2017 2:45:55 PM

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Ok guys, here we are:

- The solvent evaporates perfectly clean, without any visible trace or smell.
- In a NaOH solution, it floats perfectly on the top, without any noticeable layer on the bottom.

For anybody interested, reading on the container it says:

Hydrocarbons, C7, N-Alkanes, Isoalkanes, Cyclics, Tetrachloroethylene.

 
Mindlusion
#11 Posted : 5/14/2017 5:11:46 PM

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Heulas wrote:
Ok guys, here we are:

- The solvent evaporates perfectly clean, without any visible trace or smell.
- In a NaOH solution, it floats perfectly on the top, without any noticeable layer on the bottom.

For anybody interested, reading on the container it says:

Hydrocarbons, C7, N-Alkanes, Isoalkanes, Cyclics, Tetrachloroethylene.



success

read up on FASA/FASI to salt the fumarates out, they can be converted back to freebase easily by precipitating out of sodium carbonate water
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Heulas
#12 Posted : 5/14/2017 5:16:30 PM

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Thank you.

By the way, what's the point in converting to fumarate if i'm going to convert back to freebase.

Can't i just freeze precip the DMT from the solution, store the NPS and then let the spice dry?
 
Mindlusion
#13 Posted : 5/14/2017 5:25:31 PM

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Heulas wrote:
Thank you.

By the way, what's the point in converting to fumarate if i'm going to convert back to freebase.

Can't i just freeze precip the DMT from the solution, store the NPS and then let the spice dry?


I described this already in my above post, its easier, faster, more efficient, cost effective, and less wasteful.

And if your solvent contains 25% TCE, freeze precip likely won't work anyway
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Heulas
#14 Posted : 5/14/2017 5:32:10 PM

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Mindlusion wrote:
I described this already in my above post, its easier, faster, more efficient, cost effective, and less wasteful.


Totally going to study more.

Mindlusion wrote:
And if your solvent contains 25% TCE, freeze precip likely won't work anyway


That was the thing i was suspecting.

Thanks again.
 
downwardsfromzero
#15 Posted : 5/16/2017 10:05:38 PM

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heptane (pure): d20 = 0.6795 g/cm3
TCE: d20 = 1.622 g/cm3

A quick calculation: ((3*(0.6795))+1.622)/4 = 0.915125. So it'll float, definitely on NaOH soln. As has been found.

A fair guess could have been made beforehand.

Also: Health and Safety.




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