Hexane extraction

[Sativa Dragon]

Hello all,

For some reason I thought a soxhlet extractor would be useful for a Hexane extraction.

After reading here in the extractions area I see there is not a lot of people recommending it.

What would be a good extraction method for Hexane which I already purchased a liter of?

Peace

 

[Gray Wolf]

It makes a good cold extraction and we use it for alchemy, such as cleaning up other extractions and making cannabis acetate.

 

[nakadashi]

Hello all,

For some reason I thought a soxhlet extractor would be useful for a Hexane extraction.

After reading here in the extractions area I see there is not a lot of people recommending it.

What would be a good extraction method for Hexane which I already purchased a liter of?

Peace

You can use in a similar manner to how you would perform QWISO extraction.

 

[Hashmasta-Kut]

i see you are into warnings, so dont forget, Warning! dont forget to wear your safety gear when extracting with hexane if you are going to be exposed to the fumes.

 

[RHH]

My experience has been that hexane was difficult to purge although i may have been using vacuum without heart at that time. It's hard to remember. Everyone complained about the taste. It was a fun experiment but I didn't explore it further.

 

[Gray Wolf]

Hexane is highly forgiving and makes a killer extraction, but is a six carbon chain, so is harder to purge than butane with only four carbons.

Without vacuum, I've gotten it below the 130 ppm sensory threshold by washing it around three times with ethanol, and as result, there were few monoterpenes remaining.

With vacuum I've gotten it below sensory threshold just vacuum purging at 115F and -29.5" Hg, but there are still few monoterpenes remaining once the Hexane is gone.

We mostly use it for alchemy, and do extractions with something easier to purge and retain the lighter terpenes.

 

[RitualDelFuego]

I have a close friend who may require HHO due to allergic reactions. This friend of mine also knows someone with a child patient who has a similar reaction to some extracts (FECO/RSO) and I have read elsewhere that hexane concentrates tend to pick up much less poop when properly run.

Hey WOlf-- dont you think the hexane will purge more fully if it's vacuumed into a cold trap through a condenser?

 

[Gray Wolf]

I have a close friend who may require HHO due to allergic reactions. This friend of mine also knows someone with a child patient who has a similar reaction to some extracts (FECO/RSO) and I have read elsewhere that hexane concentrates tend to pick up much less poop when properly run.

Hey WOlf-- dont you think the hexane will purge more fully if it's vacuumed into a cold trap through a condenser?

A cold trap on the pump system will make it harder to purge the oil, because you can't run the chamber itself at 29.5" Hg, and not have the cold trap at even lower vacuum.

We've had more than one patient come to SPR after having a bad reaction to RSO made with naphtha, or Isopropyl.

Hexane is more forgiving than naphtha, because it is primarily Hexane, with some Pentane and Heptane contaminants, while naphtha is any hydrocarbon chain that boils between 30C and 200C.

Even light naphtha is just a boiling point range and can contain Benzene, a know carcinogen.

The pharmaceutical grade of Varnish and Paint Makers (VP&M) naphtha that Rick recommends, simply shows a boiling point above 242F.

http://www.homedepot.com/catalog/pdfImages/bf/bfb9e5da-773d-4116-a279-b23cf9345aaf.pdf

You might also consider a BHO or QWET extraction, both easier to purge.

 

[SkyHighLer]

A cold trap on the pump system will make it harder to purge the oil, because you can't run the chamber itself at 29.5" Hg, and not have the cold trap at even lower vacuum.

We've had more than one patient come to SPR after having a bad reaction to RSO made with naphtha, or Isopropyl.

Hexane is more forgiving than naphtha, because it is primarily Hexane, with some Pentane and Heptane contaminants, while naphtha is any hydrocarbon chain that boils between 30C and 200C.

Even light naphtha is just a boiling point range and can contain Benzene, a know carcinogen.

The pharmaceutical grade of Varnish and Paint Makers (VP&M) naphtha that Rick recommends, simply shows a boiling point above 242F.

http://www.homedepot.com/catalog/pdfImages/bf/bfb9e5da-773d-4116-a279-b23cf9345aaf.pdf

You might also consider a BHO or QWET extraction, both easier to purge.

^ "Even light naphtha is just a boiling point range and can contain Benzene, a know carcinogen."

Like GW said, not all 'light naphthas' are the same, petroleum ethers are classified by boiling point,

"Petroleum ether is obtained from petroleum refineries as the portion of the distillate which is intermediate between the lighter naphtha and the heavier kerosene. It has a specific gravity of between 0.6 and 0.8 depending on its composition. The following distillation fractions of petroleum ether are commonly available: 30 to 40 °C, 40 to 60 °C, 60 to 80 °C, 80 to 100 °C, 80 to 120 °C and sometimes 100 to 120 °C. The 60 to 80 °C fraction is often used as a replacement for hexane. Petroleum ether is mostly used by pharmaceutical companies and in the manufacturing process. Petroleum ether consists mainly of pentane, and is sometimes used instead of pentane due to its lower cost.[1]"
http://en.wikipedia.org/wiki/Petroleum_ether

Benzene has a boiling point of 80C, so you want a fraction that has been specifically distilled and filtered to avoid benzene contamination. Petroleum either labeled with a boiling point of 30-60C is safe to extract with, it's almost entirely pentane, but is slightly cheaper and easier to obtain than pure pentane. Here's an example,

"Petroleum Ether, A.C.S. Reagent, 500ml (16oz)
For Research & Development
Not for drug, clinical use in humans, for food or food additive use

Specifications:
Meets ACS Specifications
Boiling range 35 degrees - 60 degrees C Pass
Maximum limits of impurities
Color (A.P.H.A.) 10
Acidity Pass
Copper corrosion Pass
Doctor test Pass
Residue after evaporation 10ppm
Sulfur 5ppm
Benzene (GC) 2ppm

CAS: 8032-32-4

FORMULA: N/A"

http://www.ebay.com/itm/Petroleum-E...905?pt=LH_DefaultDomain_0&hash=item3a826f1bf9

 

[RitualDelFuego]

the label on the can states the distillation range of the batch was 66-67.2

i'm willing to try and run a batch just to test.

maybe set up a test and run one batch then purge three samples of the same batch three different ways and test all three for resiuals??

 

[RitualDelFuego]

and on the subject of using other solvents, plenty of people talk smack all day about the evils of petrochems and yet i've noticed nobody using actual ethyl-ether (RSO is made with naptha or petrol-ether) or at least anyone who is using it is not talking about it much. Makes some good sense to me as a solvent for oil extractions unfortunately it's scheduled as a precursor.

the ethyl-ether is derived from ethanol and should be investigated further imo------

 

[queequeg152]

and on the subject of using other solvents, plenty of people talk smack all day about the evils of petrochems and yet i've noticed nobody using actual ethyl-ether (RSO is made with naptha or petrol-ether) or at least anyone who is using it is not talking about it much. Makes some good sense to me as a solvent for oil extractions unfortunately it's scheduled as a precursor.

the ethyl-ether is derived from ethanol and should be investigated further imo------

wow haha.
diethyl ether? thats what you mean riight? ethers in general are horrible to work with, and IMO are entirely unsuitable for use in even semi large sized extractions.

its also polar, you know that right? its going to pull in plenty of aqueous stuff.

you can use ether all day long in these tiny syringe L|L extractions, but its not worth it for very large scale stuff. its sketchy to store... and not to be taken lightly.

read any lab manual from the last 2 decades... its pretty much gosple, that one does not use ethyl ether unless no other suitable solvents are available.

and yea diethyl ether is trivial to make, very trivial, it was discovered in like... the 19th century after all. but it will not be cheap. you need concentrated sulfuric acid, which is not cheap.

i believe its technically cheaper to make chlorinated solvents(also trivial) with concentrated sodium hypo, and or some cheap methanol and HCL.

 

[queequeg152]

classic demonstration. lol, id bet a ham sandwich this has not been done in a highschool in the last 30 years.... we've become such pussies.

https://www.youtube.com/watch?v=vmedtpK0Pgk

ether is like chloroform... its incredibly dense vapors flow and fall anywhere they can. its incredibly volatile as well...
in the case of chloroform... you can actually see the vapors of chloroform spilling out of a hot flask and flowing all over a lab bench. perks of not working in a fume hood.

ethers auto ignition temperatures are very low. you can theoretically ignite it with a not so hot soldering iron.

you cannot see ether vapors what so ever... in my experience

 

[Gray Wolf]

and on the subject of using other solvents, plenty of people talk smack all day about the evils of petrochems and yet i've noticed nobody using actual ethyl-ether (RSO is made with naptha or petrol-ether) or at least anyone who is using it is not talking about it much. Makes some good sense to me as a solvent for oil extractions unfortunately it's scheduled as a precursor.

the ethyl-ether is derived from ethanol and should be investigated further imo------

Diethyl ether and dimethyl ether both work. Eiethyl is on the watch list, but dimethyl is not and is currently sold by Dr Z for extractions.

Petroleum ether would be a better choice than naphtha.

 

[RitualDelFuego]

Word to the wolves and thanks...

ethers auto ignition temperatures are very low.

TRUE. Thanks for reminding me to mention something about how dangerous ether is. Ether MUST BE STORED DRY on desiccant. (and it's way more flammable than it smells... worst joke of the week)
If stored improperly DiMethylEther can form dangerous peroxides.
http://en.wikipedia.org/wiki/Diethyl_ether_peroxide it states :

"It is a colorless oily liquid that is an extremely brisant and friction sensitive explosive material. Amounts of less than 5 milligrams can damage chemical apparatuses.[who?] The dangerous properties of ether peroxides are the reason that diethyl ether and other peroxide forming ethers like tetrahydrofuran (THF) or ethylene glycol dimethyl ether (1,2-dimethoxyethane) are avoided in industrial processes."

BLeh. It's not my intention to hijack the HEXANE EXTRACTION THREAD :-D

DME is just another liquid solvent... Hexane is awesome. non-polar, doesn't like water, absorbs plenty of oils but not so much wax (when cold) ....

 

[RitualDelFuego]

So on the subject of hydrocarbon solvents, hexane specifically, they are all different fractions of the same process if I understand. Hexane is a fraction of petroleum which occurs after butane propane and pentane more or less.

So I have "HexanesACS" with a lab cert specifying it is 99.9% hexanes being the fraction between 66-67.2 with like around 60% being n-Hexane and the rest being iso-Hexane and MethylPentane

So my question about all this is: Is this mixed Hexanes fraction plenty good for organic extractions that are just going to get winterized in ethanol anyway or what?

 

[SkyHighLer]

So on the subject of hydrocarbon solvents, hexane specifically, they are all different fractions of the same process if I understand. Hexane is a fraction of petroleum which occurs after butane propane and pentane more or less.

So I have "HexanesACS" with a lab cert specifying it is 99.9% hexanes being the fraction between 66-67.2 with like around 60% being n-Hexane and the rest being iso-Hexane and MethylPentane

So my question about all this is: Is this mixed Hexanes fraction plenty good for organic extractions that are just going to get winterized in ethanol anyway or what?

"The contaminant-free purity of ACS Reagent Grade Hexanes is mainly used in food production as a safe, easily evaporated non-polar solvent, particularly in extracting oils from seeds.

Hexanes Specifications Limits Typical Lot Analysis
Assay, min
(Hexane Isomers & Methylcyclopentane) (GC) 99.5% 99.9%
n-Hexane, vol% 45-65% 53.35%
Color (APHA) 10 <10
Residue After Evaporation 10 ppm <10
Water Soluble Titrable Acid 0.0003 meq/g <0 .0003
Analine Point C 57-68.9 65.7
Bromine Index 30 max <2
Distillation Range 65-70 66-67.2
Specific Gravity 15.6C 0.660-0.690 0.6767
Sulfur Compounds (as S) 50 ppm Pass
Thiophene To Pass Pass
Water 0. 1% 0.0036%"

http://www.ebay.com/itm/NC-12886-He...753?pt=LH_DefaultDomain_0&hash=item3f38a3d571

"Methylcyclopentane is an organic compound with the chemical formula CH3C5H9. It is a colourless, flammable liquid with a faint odor. It is a component of the naphthene fraction of petroleum. It usually is obtained as a mixture with cyclohexane. It is mainly converted in naphthene reformers to benzene..[2]"

http://en.wikipedia.org/wiki/Methylcyclopentane

G.O. Joe?

 

[Gray Wolf]

So on the subject of hydrocarbon solvents, hexane specifically, they are all different fractions of the same process if I understand. Hexane is a fraction of petroleum which occurs after butane propane and pentane more or less.

So I have "HexanesACS" with a lab cert specifying it is 99.9% hexanes being the fraction between 66-67.2 with like around 60% being n-Hexane and the rest being iso-Hexane and MethylPentane

So my question about all this is: Is this mixed Hexanes fraction plenty good for organic extractions that are just going to get winterized in ethanol anyway or what?

It will do the job. With hexane, it is important to adequately purge, because our liver can turn it into 2.5 Hexane dione.

 

[RitualDelFuego]

it still makes me nervous, being a petro chemical and all...


then i dug a jar of extract out of the back of the freezer and started working on it only to discover it was an abandoned acetone experiement. yuk...

I really like the way butane can be expunged from the resin with food grade ethanol. Hexane sort of puts up a bit more of a fight. that's the only reason I mentioned the ethers earlier, because they might purge faster/safer than alcohol as a dewaxing solvent.


i have blasted straight cold hexane through frozen dry herb with compressed argon... it made a good extract but when it came to winterizing there's a little finesse there that needs to happen.... So it's always in the back of my mind. But the Butane/ethanol regimen works so well

 

[Pastelero]

Short question,

I read Graywolf´s Tutorial on how to purge Hexane (mix with water & ethanol, wait until layers will stratisfy, pour the layers off).

Does this also apply 1:1 to pentane as well?