What is the Best Extraction Method?

[TheDynamiteGuy]

What is the best method for extracting those precious little trichomes? Would that be "Dry Sieve" or "Bubble Bag"? Which one gives the highest yield and the highest quality? Then there is chemical extraction. I don't know if I like that idea, isn't residue a problem? Let's hear those opinions, I want the most medicine for my buck. :cool:


The Dynamite Guy
Fly Fishing the Rockies + Rocky Mountain High Priceless!

[Green Supreme]

Well both dry and water extract have their merits. I like both and will always make both. As to solvent extraction, I think I'd rather not ingest solvent if I don't have to and because of water and dry extraction I don't have to. Good luck. Peace GS

[c-ray]

what about coconut butter?

[Alchemist]

supercritical carbon dioxide.......



by a long shot

[c-ray]

what about low pressure CO2?
for the sake of quality

from http://edenlabs.org/supercritical_extraction.html
There are two basic types of CO2 extraction. Low pressure cold extraction involves chilling CO2 to between 35-55 degrees F and pumping it through the plant material at between 800-1,500 psi. Supercritical Fluid extraction involves heating the CO2 to above 87F and pumping it above 1,100 psi. Usually this work is done between 6,000-10,000 psi. Supercritical Fluid CO2 can best be described as a dense fog whereas the first method described uses the CO2 in a dense liquid state.

Low pressure CO2 is often the best method for producing high quality botanical extracts. CO2 has a high loading rate in this state meaning that you will have to pump many volumes of CO2 through a given volume of botanical. The loading rate is typically 10-40 volumes. For this reason, it is important to have a high flow pump and a CO2 recycle system unless wasting high volumes of CO2 is not a concern.

Supercritical CO2 has a much faster loading rate 2-10 volumes and a wide range of uses. The downside is that some extracts can be damaged by either the high pressure breaking molecular ring structures or the fact that moisture in the botanicals can react with the CO2 and form carbonic acid which can turn some oils rancid. Following proper procedures can avoid these problems.

[Green Supreme]

Low sounds good to me. Seems to me the issue with both is the machine required to do so. The best method means little if the finished product cannot be accessed. Peace GS

[Alchemist]

Hi Guys, I see the problem with co2 in the capital costs of the equipment.

I think high pressure is more efficient in terms of how much co2 is used, anything large scale and the co2 is recycled.

I think that high pressure would be great combined with a series of vessels for fractionation. Theoretically you could put your cannabinoids in one vessel and your essential oil fraction in another.

I think a liquid co2 extract is more like the BHO process and less selective.

there needs to be a lot more work done here

PEACE

[c-ray]

the high pressure is no good for terpenes though, it is worth it to use extra CO2
I think I asked those guys how much a system would run at one time and it was around $15-20k

[Alchemist]

I wonder if the high pressure de- natures the terepenes? high pressure is almost always used in combination with high temps in co2 extraction, 650 bar , 100c or 120c

They definitly wont oxidize in a co2 extractor thats for sure.

I have seen extracts done at medium pressure ( 350 bar, 5000 psi) (40-60c) and the terepenes were intact and fierce!!
I think fresher material works better with about 10% moisture, we will see.

[Springs]

See, taste and feel :)

Interesting subject, cant wait!

[Green Supreme]

There's a thread on IC mag about using Oxygen. Peace GS

[Alchemist]

i checked icmag for that thread...i want 3 mins of my life back!!

just kidding, co2 is the shiznit alright

[guest]

#1. Supercritical co2 extraction = >95% THC (this is how sativex is made)

#2. Column chromatogaphy > fractional distillation under pressure > column chromatogrpahy = >98% THC

#3. Column chromatogaphy > fractional distillation under pressure = 95-96% THC

#4. N-butane extraction under low pressure (ie BHO - propane might be better) = ~80% THC

#5. Manual extraction of trichomes by your favorite method, eg. Bubblebags.

HTH

[guest]

Co2 extraction is not the best by much. Its more efficent, but still uses solvents besides liquidifed co2. For most people only wanting to spend a few thousand number 3 on my list is most possible. That's if one has a strong background in chemestry...

All in all, n-butane is the best 99.999...% of non-scientists can hope for. Tho propane has benefits in some areas over n-butane.

Budder is emulsified iso-extract, or BHO. Its not inherently stronger than the oil. The increase comes from the heat which converts THC-A to THC when blending the oil.

[guest]

Ps. Stay tuned for upcoming madess! Things which have not been done will be done...(at least 6 months)

[d'artanian]

If u want all the medicine out of your plants. i would suggest a socklet-exstraction.

[Green Supreme]

Hmm the BHO we encounter here is butane honey oil. It can be in budder form or as oil. I'm gonna stick with water extract till something cleaner is found. Peace GS

[Lundin]

If u want all the medicine out of your plants. i would suggest a socklet-exstraction.

hmm:call:

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

http://upload.wikimedia.org/wikipedia/commons/thumb/4/41/Soxhlet_Extractor.jpg/257px-Soxhlet_Extractor.jpg

[guest]

The s.extractor is for heating vapors, etc. Not for extracting cannabinoids. You will want to use #2 or #3 on my list.

GS, with water extract you are also extracting any contamination (microbial, toxic, etc) on the herb, along with terpines, CBN and other acids and neutal cannabinoid degrades. For medical purposes we must have pure extracts (for Gov. Approval). The founder of THC claims a 3:1 ratio of CBD:THC is ideal. The two different mixes of testing satavex was 50:50 CBD:THC and 95% THC. IMO the first 3 I listed are 'safer' than water extraction. Imagine, someking a crystalized piece of 99% pure THC? Drool...no messing with oils!

[guest]

But yea, BHO = unhealthy. Even low-pressure n-butane BHO is unhealthy. Water is way better in that regard, I fully agree :)

[Green Supreme]

You mention thc but no mention of terpene content, its my understanding they help regulate the way thc works and its effects. Although some terps are lost in water, I can still smell the hash so some must be present. Mr.Sam the Skunkman has been known to say that thc is no fun without terps, not that it should be all fun but some would make folks pains more tolerable. One thing I have noticed about cannabis and my bad back is that I am very lucky as indicas numb my pain and sativea make me forget it. Hmm terps huh. Peace GS

[d'artanian]

The s.extractor is for heating vapors, etc. Not for extracting cannabinoids

The vapor condenses in the cooler and flows down to the shoxlet, extract whatever mey be in it, so it will drain into the flask again. and repeat the process as long as desired

[guest]

You mention thc but no mention of terpene content, its my understanding they help regulate the way thc works and its effects. Although some terps are lost in water, I can still smell the hash so some must be present. Mr.Sam the Skunkman has been known to say that thc is no fun without terps, not that it should be all fun but some would make folks pains more tolerable. One thing I have noticed about cannabis and my bad back is that I am very lucky as indicas numb my pain and sativea make me forget it. Hmm terps huh. Peace GS


Hey bro,

Those extraction methods can extract any chemical to which there are known prodcedures. The terps would be in indiviual factional distillations, one just needs to identify them, and further extract them.

Terps have been found to potentiate some effects of THC, but also to antagonise other effects of THC. I have not seen studies showing medical benefit of terps or neutral cannbinoids degrades.

Here's my take ATM:

High (assuming no access to pure CBC and A-THC):
75% THC
10% THCV
5% CBD

Medicine:
75% CBD
10% THC
5% THCV

And
50% CBD
45% THC
5% THCV

Terps IMO are mostly flavor/aroma, not decernable difference in effects of THC. But, I have not studied this. I will tho once I have my lab setup if you'd like to help test... :)

I think as far as extracts go, excluding terps will lower the experience is some ways, but also increase it in other ways, especially medicinally.

[guest]

Hey Gerber,

That's the problem, heat and vapor first, then condensate...no buieno for cannabinoid extracts.

HTH

[guest]

The thing about CBD is it low, even in varieites with traditonally high CBD (eg. Hindu-kush region). Not over 2-3% generally. So most of us are smoking very little CBD as a cannabinoid profile % and total % by weight of herb.

I plan to work with THC, THCV, CBD, CBC and maybe if possible A-THC and CBG.

I tottally agree that a mix of wide leaflet indica (WLI) (ie. CBD?) and thin leaflet indica (TLI) (ie. sativa, THC) is a great relief for lower back pain. It seems the litrature backs up your personal findings :)

I have had breeding on my brain for a while now! I am developing a few chemotype spefiic varieites (re: ratio, and quantity by weight). Namley CBD, THC, THCV and CBC. Also, the elusive A-THC if I can find those cultivars...(I'm using an advanced double super seceret bredding methodology :wink: )

Within the next year(s) I hope to have something worth showing others...

[Green Supreme]

I think Sam and GW have done a lot of research on terps and their effects. This info is not being released to the public for some reason. Peace GS

[guest]

Oh yea GS, the n-butane (and BHO) extract are ~80% THC, while retaining the full terp profile. Butane extraction is a defacto method for many essential oil extracts, that's why its a good choice for retaining the 'flower' chemical profile.

[Green Supreme]

Have read somewhere in the past that terps don't survive the pressure of butane. Before we extol the med virtues of butane you might want to look into the ethyl mercapitan they put into butane. Not real medicinal stuff. Peace GS

[guest]

Hey,

I'm not extoling butane, I agree using bullbebags are better than BHO for saftey/health.

Regarding GW studying terps: I think so too. But AFAIK GW isn't looking at them for use as meds. GW has many patents where one can get lots of info they don't release. And their book is great:

"The medicinal uses of cannabis and cannabinoids"

They have done much chemotype breeding, well, HortaPharm really did the chemotype bredding for the last 20 years. The ratio of cannabinoids is genetic, fixed. So breeding, while useing some Mendel laws, to select for specific chemotypes is simply a matter of numbers, along with some inherent skill and correct cultivar and cultivar cross choices of course.

Though there are areas of breeding chromotypes they did not explore...

[Green Supreme]

Sorry its just you brought up the butane thing and the medicine thing so many times I thought it needed to be pointed out. Peace GS

[Alchemist]

Co2 extraction is not the best by much. Its more efficent, but still uses solvents besides liquidifed co2. For most people only wanting to spend a few thousand number 3 on my list is most possible. That's if one has a strong background in chemestry...

All in all, n-butane is the best 99.999...% of non-scientists can hope for. Tho propane has benefits in some areas over n-butane.

Budder is emulsified iso-extract, or BHO. Its not inherently stronger than the oil. The increase comes from the heat which converts THC-A to THC when blending the oil.


hi guys!!

what solvents does co2 extraction use other than co2?


The soxhlet is a great apparatus but is only as good as the solvent your using

peas

[guest]

Hey

AFAIK the solvent used depends upon the chemical one wishes to extract.

Your right about the solvents for the soxhlet extractor, but its still a far cry from 'column chromatography > fractional distillation under pressure' and co2 extraction. Its also much less efficient than the other options.

And I forgot to say, the cheapest method to get 92-93% THC is a double fractional distillation under pressure. So all one buys is one fractional distillation apparatus (good ones are $2-5k), plus solvents and silicas, etc. And lots of chemistry knowledge...

Alchemist seem to know about chemistry, yes?

HTH

[Alchemist]

im a bucket chemist with some know how and some good resources.

the use of co-solvents or modifiers is common in co2 extraction but usually to extract more polar components. The non - polars are all readily soluble in co2.

great discussion!

be sure to update on your progress gojo!!

[d'artanian]

Hey Gojo
Chromatography and distillation is process that separates substances from a mixture(liquid). I have worked with both methods many times, but I do not understand how to use these methods for extraction. can you elaborate on how this is done.

and why do you recommend fractionated destillatio under pressure? would it not be better to use vacuum, since you then get a lower bp.

[guest]

the use of co-solvents or modifiers is common in co2
extraction but usually to extract more polar components. The non - polars are all readily soluble in co2.

^ FTW

I agree, great discussion.

[guest]

Gerber,

Check out this URL:
www.freepatentsonline.com/6730519.html.
(Besides chelating THC-A, one can isomer the CBD fraction to THC to harvest more THC overall).

That's a typo, your correct. Thanks for pointing it out. I meant to write "under reduced pressure"; or as you pointed out, under vaccume (<1mm HG; ideally 0.1mm HG).

Alchemist is correct that co2 is the most ideal, and 'cleanest' method in regards to residue. This is my method of choice, hopefully soonish I can play with it...

HTH

[d'artanian]

www.freepatentsonline.com/6730519.html.
this is a refinement process, separating the compounds from the crude cannabis oil.

[d'artanian]

you still ned to do a extraction in prior:yeahthat:

[guest]

Well the extraction process wasn't your question. As extraction solvent I am most likley going to use is a blend, I have to check my notes as I can't recall exactly. The extraction process is not something I will share. I want to share info, but not to my possible financial detrement. You can develope your own extraction process. The info one really needs, which you originally asked about, is within that patent.

HTH

[c-ray]

that's interesting Geber but I don't think we want pure isolates, I am a firm believer that patients will benefit from a wide variety of terpenoids as helper substances, variation can be good but maybe not for crack peddling pharmaceutical companies who like to get into bed with politicians

I found another patent a while back that was similar, using alcohol for extraction and simple pH swings and decanting to separate the goodies from the chlorophyll and waxes...I'll see if I can find it again

this is a great thread thank you everyone

[guest]

Petrolum ether IIRC is what I plan to use as an extraction solvent. I will also say I plan to pre-treat the extract and use factional extraction, seperation and re-combination of raw extract.

[d'artanian]

thanks C-ray, I also share your opinion.

Gojo, I just wonder why you recommend
# 2 Column chromatogaphy> fractional distillation under pressure> column chromatogrpahy => 98% THC

# 3 Column chromatogaphy> fractional distillation under pressure = 95-96% THC
as an extraction method, rather than soxhlet extraction?
And I do not see what the problem is, with a soxhlet extraction
That's the problem, heat and vapor first, then condensate ... no buieno for cannabinoid extracts.
can you elaborate on that?

[c-ray]

Petrolum ether IIRC is what I plan to use as an extraction solvent. I will also say I plan to pre-treat the extract and use factional extraction, seperation and re-combination of raw extract.

it is nearly impossible to completely separate petroleum distillates from cannabinoids, there will always be some in the final product, not exactly what we want to give to patients...but let's see what pee wee has to say on the subject

uLZptx6UQLk

[guest]

Hey c

That is why its fractionally distilled under reduced pressure, that is how the p.ether is completly removed. P.ether is very commonly used in medical extracts. Can you provide references showing your point? I'm curious about what you wrote.
Like I wrote I may be using p.ether, or some other blend. I can't remember exactly and have checked my noted yet.


"The Volatile Oils Vol 1"
By E. Gildemeister

http://chestofbooks.com/health/aromatherapy/The-Volatile-Oils-Vol1/A-Extraction-With-Volatile-Solvents.html

Millon placed the flowers into a percolator (appareil a deplacement) covered them with ether and renewed the menstruum after 10 to 20 minutes. The extract, obtained after evaporation of the ether, he kept in open containers because he thought that the air acted favorably on the odoriferous principle. This, however, was a deception. Unless the solvent is carefully removed with the aid of a vacuum, mere traces of it can be detected if the extract is kept in closed containers. Millon was not ignorant of the fact that the greater part of the extract consists of vegetable wax which is well nigh insoluble in alcohol. Hence he determined the amount of odoriferous sub-stances by ascertaining the difference in weight of the extract before and after treatment with alcohol.

Also check out:

1. "Optimization of Solvent Extraction of Moringa (Moringa Oleifera) Seed Kernel Oil Using Response Surface Methodology"
By S. Mani, S. Jaya and R. Vadivambal


2. Erowid:
If someone is concerned that a loved one is using impure solvents, a simple test can determine how much residue is present in the solvent by taking a half-cup of the solvent and evaporating it in a glass jar or cup. Once the solvent is completely evaporated (this should be done outside, as most of these solvents produce nasty fumes and are flammable) the bottom of the jar can be checked for residue. If any residue is present, it is probably not acceptable for any ingestion related use



HTH

[guest]

Who is pee wee?

[guest]

Also, the cc continues the purification...

[guest]

Hey gerber,

AFAIK they are far more efficient than s.extrator, especially when processing moderate to high amounts of cannabis. They are much less expensive if process large amounts of cannabis. The % of chemical extracted is greater than of a s.extrator, if proper procedures are followed. The extract is more pure depending upon procedure, ie. 'cc > fd urp > cc' = >98% thc

[Alchemist]

thats the problem with alot of separations : you must first dissolve the compounds in a carrier solvent or mobile phase.

thats the beauty of co2, no petro chemical solvent residues (which will always be there with other methods IMO) and the ablility to fractionate components based on their solubility in co2 at diff pressure + temps which provides dramatically diff densities

[guest]

I totally agree. I plan to play with both. I plan to use co2 for medical extracts and #2 for work with cannabis quantitation...but until I can afford co2 ill prolly use #2 for personal testing :)

[c-ray]

talk to skunkman, he did the research
I only know what I can taste and smell, bleah

[guest]

Hey c

Who is this skunkman everyone refers to? I have read very little about him, and I don't think I have ever read anything by him, does he post somewhere? He seems very knowledgeable, but where does he present his knowledge? Where can I read his opinion on this topic?

I have considered contacting GW pharm once I have developed my chemotype specific varieties, and other medicinal products I am researching. I would be interested in working with them in some areas. I know GW is looking for scientists to work with...and they sure know what they are doing! Tho I am not anywhere near the level of GW scientists, yet. ;)

I am emailing Hortapharm soon with some questions and possible corrections.

[guest]

Hey c

Have you ever smoked extracts of the quality to which I am referring? I have not. But I very highly doubt we would taste or smell solvents and chemicals. As for basic stoner DIY BHO or alcohol extracts I totally agree.

[c-ray]

skunkman is the W is GW pharmaceuticals

[Green Supreme]

Sam The Skunkman is partner in GW and Hortapharm. He created the original Skunk and is responsible for many of the genetic about since the 70's. Very knowledgeable fellow. He posts from time to time on IC mag. I have puffed CO2 oil before and is was very clean. Was weird though as many of the purer oils I have puffed have not liquid qualities to them they are more like solids. The CO2 was more runny. Peace GS

[c-ray]

terpenes

[guest]

Thanks guys.

GS, that's great you have tried co2. I'm not down with oils, I plan to convert to crystals and smoke them, if the crystals turn out the way I think they will. I am also working on sublingual, suppository and transdermal delivery.

C, why do you feel so strongly about terpenes? I spent a little while today looking for journal articles regarding medicinal value of terpenes. I really don't see the link. Can you provide references which helped form your opinion? And not only that, but why the push for tepenes in extracts to get high with? IIRC, within the limited research I have read (a while ago) there is possibly nominal potentiation to the effects of THC and CBD, and possibly more than nominal antagonization. Is Mr. Skunkmans opinion about terpenes [sic] "making THC more fun" conjecture or scientifically based? I mean to ask, did he carry out proper experiments, or is it that he smoked each and formed an opinion? I really want to know if terpenes are worth the trouble or not, but I want to wait for data to form an opinion.

Regardless, IMO terpens are not going to be allowed in most medical extracts. A big reason for extracts as medicine is the ability to exactly control how much medicine is used. Experts I have read from seem write as much, specifically, the doctor whom discovered THC and so far GW pharm visa-vi Sativex and government regulations. Medical experts I have heard from seem to agree in the opinion pure extracts and blends are ideal. Remember that Western medicine tries to limit variables to ensure medicinal efficacy.

Thanks all

[guest]

Wow, lots of interesting info in this thread...

Can one of you more knowledgeable folks instruct me as to the downsides of my usual extraction method? i.e., water extracted trichomes passed through 94 % food grade alcohol?

Thx

[d'artanian]

it sounds like a good extract
The advantage is that you get little chlorophyll in the extract, without the use of reactants. but the drawback is that you lose much of the water-soluble terpenes during water extraction, and that a portion of the volatile oils disappear along with the alcohol during evaporation

[guest]

Seems I was wrong about terpenes. Mia copa mia copa mia maxima copa! ;)

However, I still forsee legalized meds as not along a full terpene profile...

"Cannabis and Cannabis extracts: Greater than the sum of their parts"
Author(s): John M. McPartland
Ethan B. Russo
http://www.omma1998.org/McPartland-Russo-JCANT%201%283-4%29-2001.pdf

And...

"Cannabis is more than simply ?9-tetrahydrocannabinol"
Author(s): Ethan B. Russo and John M. McPartland
www.springerlink.com/content/gefrp0xg76d72926/

[Quote]Terpenoid cannabis components probably also contribute significantly to clinical effects of cannabis and boil at comparable temperatures to THC (McPartland and Russo 2001). Cannabis essential oil demonstrates serotonin receptor binding (Russo et al. 2000). Its terpenoids include myrcene, a potent analgesic (Rao et al. 1990) and anti-inflammatory (Lorenzetti et al. 1991), betacaryophyllene, another anti-inflammatory (Basile et al.1988) and gastric cytoprotective (Tambe et al. 1996), limonene, a potent inhalation antidepressant and immune stimulator (Komori et al. 1995) and anti-carcinogenic (Crowell 1999), and alpha-pinene, an anti-inflammatory (Gil et al. 1989) and bronchodilator (Falk et al. 1990).

Are these terpenoid effects significant? A dried sample of drug-strain cannabis buds was measured as displaying an essential oil yield of 0.8% (Ross and ElSohly 1996), or a putative 8 mg per 1000 mg cigarette. Buchbauer et al. (1993) demonstrated that 20

[Green Supreme]

Amen. Peace GS

[guest]

Preach!

[c-ray]

However, I still forsee legalized meds as not along a full terpene profile...

well that's what the pharmaceutical companies want as they are all about standardization, but it's not really what's best for the patients

[guest]

Hey guys,

Glad you like the papers. I am looking for more, I want to catagorize medicinal terpenoids and recreational terpenoids, and useless terpenoids. IMO there is still way to much assumption stated as fact.

Hey c,

I disagree. Its not big pharma per say, its Western medicine. It always wants proof before it allows something as medicine. What's wrong with that? I too want proof before I believe something in most casses.

I still stand by my statmenet that pure extract blends are ideal, not a full terpenoid profile. Not all terpenoids are helpful...I'm sure some terpenoids are not synergisitc at all and are complelty antagonisitc.

I am going to research terpenoids and flavenoids. For example, flavenoids were stated as good for sublingual.

If we ever want to have legit meds for those who really need them extracts are needed. See my previous info about health concerns from raw cannabis, a major issue for those who are already sick. Western medicine requires extracts, the medical efficacy must be proven before its accepted as medicine to the West...

I don't like big pharma either, but IMO they are innocent in this regard. Blame hundreds of years of Western medicine...

[Green Supreme]

Putting the med community and the word proof is at times laughable where cannabis is concerned. I mean if they cannot see the medicinal value after all these years they got their blinders on. If you are to create medicines from cannabis ,why not use all its healing power instead of just a small portion. I think as these companies do more research you will see more value to the terps as will the big pharmies. Oh well till then they can be our little secret, so we can chuckle at them teehee. Peace GS

[guest]

Hey

Its about preventing snake oil. And insuring medical efficacy. Proof is not laughable IMO, and its agreed cannabis is medicine, but, what part of cannabis has medical value, that's the question.

You can't just give a sick patient with low T count a bud and expect the same medical efficacy and benefits as a mix of proven extracts.

Why is it silly to ask for proof of cannabinoids and terpenoids? To me its silly to not ask for proof.

Raw cannabis and extracts like hash are less medicinally beneficial than a mix of pure extracts.

The reason I am always skeptical of miracle drugs of unproven value is because so many people are taken advantage of. Granted big pharma also takes advantage of people. The key IMO is there is proven medical value via phase I, II and III trials.

That's my take on it. Ill drop this point/discussion, we can all agree to disagree

Shalom

[guest]

Kwool. I've been doing more research on n-butane extraction, I still think n-butane is the best choice verses propane. There are a few n-butane extraction units are available for a under a thousand or two dollars :)

I found what seems to be a good brand a while ago: "Tamisium"[1]. I had planned to buy this first, then the columns and fractional distillation unit for #2 and #3. The Tamisium butane extractor uses no heat except room temperature and low vacuum. Thus the extracts from the Tamisium will be very clean and should have no residue, especially considering how easily n-butane is removed under even low vacuum. Considering that info it seems the n-butane extract should be as clean, as #2 or #3 on my list.

Pure n-butane is odorless. Sulfur containing compounds like mythyl mercaptan are generally not present. They are used for heating gases in homes to identify leaks, etc.

The good part about n-butane extraction, besides no leftover residue, is a large amount of terpeniods and flavoinoids are retained.


A few good links:

1. "Low-pressure solubility of propane and n-butane in refined soybean oil"
Author(s): M.V. Tresa, S. Mohra, M. Di Luccioa and J. Vladimir Oliveira


2. "Hemp Husbandry: Chapter 6: Cannabinoid Chemistry"
Author(s): Robert A. NELSON
http://www.rexresearch.com/hhusb/hh6thc.htm


3. "Sciencemadness Discussion Boards:
possibility for THC extraction"
http://sciencemadness.org/talk/viewthread.php?fid=10&tid=3240&action=printable


[1] Tamisium Butane Extractors
http://tamisiumextractors.com/

[guest]

I have not contacted the comapny who makes the butane extrator, I will soon. My assumptions about its functioning could be wrong.

[guest]

Ok, so here is my quick and dirty laymen pre-treatment method for raw cannabis to be used for cooking, hash or extracts. This method will greatly increase the total % THC, by a little or a lot. Definitely worth considering. This is good for use with dry or wet sive, cooking, or extraction:


1. Reduce raw cannabis to ~10% moisture content with a food dehydrate set to 95F max. Or better yet, use a "vacuum desicator" at room temp, or within a refrigerator to dry the cannabis; ideally using Co2 or No2 to prevent THC breakdown into CBN via O2. (I am testing this setup soon ;) )


2. Grind or use scissors to break up raw cannabis.


3. Add baking soda to an amount of water twice the volume of the raw cannabis (some suggest NaOH; "caustic soda" but I think baking soda will work). Bring the pH to at least 10.


4. Pour raw cannabis into alkaline water. This will allows for the decarboxalation of THC-COOH into THC, thus increasing % THC.[1]


5. Decant and filter cannabis.


6. 'Wash' cannabis in a volume of fresh, clean water. Decant and filter cannabis. Repeat washing.


7. Decant and filter cannabis.


8. Add cannabis to twice the volume of water in a pot on the stove. Heat the water to simmer and hold at simmer for two hours adding water as necessary. This heating isomerizes the inactive CBD into THC, and decarboxylates THC-A to THC. Thus increasing the % THC by up to 50%.[2]


9. Decant and filter cannabis.


--> At this point one can freeze the cannabis for use in bubblebags.


10. Dry cannabis with food dehydrator or vacuum desicator to <5% moisture content.


11. Grind cannabis with grinder and/or mortor and pestal.


12. At this point one can dry sive for kif, or use various extraction processes.



[1] Sciencemadness Discussion Boards: "possibility for THC extraction"
http://sciencemadness.org/talk/viewthread.php?fid=10&tid=3240&action=printable


[2] "Hemp Husbandry: Chapter 6: Cannabinoid Chemistry"
Author(s): Robert A. NELSON
http://www.rexresearch.com/hhusb/hh6thc.htm


GL!

[Green Supreme]

Just saying the AMA has only just now accepted cannabis as a medicine. Do you honestly believe that came about because research just showed medicinal values. Now if this is how it goes for cannabis, imagine for terps. Part of the problem here is GW not releasing their findings . I cannot really blame them. Why would they want to help folks that have opposed them every step of the way. So research is out there, it just takes an exceptional researcher to get at it. I am not that, but can see that the terps affect the the effects I get from cannabis. Just my 1 cent. I am not certified enough for 2 cents. Peace GS

[guest]

Oh yea,

When drying and processing cannabis, hash and extracts doing so under yellow light reduces conversion of THC to CBN. See "The medicinal uses of cannabis and cannabinoids" (Guy, Whittley and Robson circa 2005)

[guest]

GS,

Good point. And dude, your opinion ain't worth copper, IMO its worth paper!

[guest]

Gerber,

Check this out :)

Extraction of psychoactive material from cannabis

CycloKnight - 7-2-2005 at 05:08

I've carried out the soxhlet extraction of the psychoactive ingredients of cannabis at least a dozen times in the past.
I deleted most of my original photos, but just by chance I found this one still on my camera.

http://www.sciencemadness.org/scipics/soxhlet.jpg

I found that a simplified procedure for the extraction of pure cannabis oil (not pure THC, but still extremely potent) could be used that was quite effective, and produced a thick, translucent yellow oil, essentially the same as "honey oil".

This is how I did it:

1) Soxhlet extract cannabis for several hours using "dry" ethanol as solvent. That's right, ordinary ethanol (as dry as possible, 95% should be okay).

2) Filter it really good. I used vacuum filtration. Colour will be medium to dark green.

3) Now the magic part and this is why you can use ethanol do the extraction: Combine with activated carbon, mix it good and filter. Repeat this again. You will now be left with a very light yellow tincture! All chlorophyll has now been removed.

4) Distill off the solvent entirely under vacuum using a vigreux column to minimise product carry-over. This also removes the water which will be present from the extraction. If you do not have a vigreux column or equivalent, just distill very slowly - it will help to contain you product in the boiling flask. You will now be left with a rich, deep golden coloured slightly viscious liquid.

This next step is optional. If you feel it necessary, you may combine this liquid with a suitable organic solvent (ether, toluene, ect) and wash with dH2O, then back-extract that dH2O to minimise your losses. This will remove salts that have be extracted from the plant material. The organic solvent is then removed by vac. distillation and then continue with step 5.
The necessity of this extra step depends on 3 factors:

a) Quality of plant material, was it well cured, was it full of fertilizer before extraction? If so, do the wash. If a relatively large volume of plant material was extracted (i.e. leaves, trimmings, swag, etc), then do the wash.

b) Was ethanol dry? The drier the less salts that will have been pulled out.

c) Are salts going to be an issue? In practice I've found that the nitrate that gets pulled into the oil actually makes the final oil burn alot better. Organic material (whatever) that has been impregnated with ToC will burn much better than oil which has had all the salts removed.

5) Dilute with pure ethanol (non-denatured, use non toxic type!) to make up "Tincture of Cannabis". Inject it into ordinary "sticks" of organic (can I say "herbal"?) material to make what are known as "Reefers" (preferably the kind without filters), not that I know anything about that sort of thing. A dropper works very well for this, and the tincture dries in seconds. Its easy to dry layer upon layer to build up the potency to "unreal" levels, so I've read. I also read (or dreamt, I don't recall) that a dropper and a 15ml bottle of concentrated ToC is an instant "joint-o-matic" that will keep a party going all night (assuming it's that kind of party, and a supply of cigarrettes - hand rolled are best). 1 ounce of high quality bud will produce about 90 ml of tincture, and it will lasts longer than you would think (high potency, and high efficiency smoking in a pipe or vapourizer = lasts long time!)

I should also say, that I first started using n-hexane for the soxhlet extractions, then diethyl ether. Then I started the extractions with alcohol, removed the alcohol, then extracted with ether. A fair amount of time, work, and odours! I found it to be unnecessary.

I have never used chloroform, so I can't comment about that. (I mean for the soxhlet extractions...)

My experience based on the solvents I've used indicates that THERE IS NO SUBSTITUTE FOR ACTIVATED CARBON. No lab should be without activated carbon, it really cleans up the tincture good. IT REMOVES ALL OF THE CHLOROPHYLL. Solvent juggling to get the active ingredients without extracting any chlorophyll is very difficult. Butane is dangerous. I have done the butane extraction, but it can be difficult to get a good extraction. Could you imagine extracting with butane for several hours? Activated carbon is cheap and widely available. If you are interested in producing cannabis tincture - get the carbon. I still have some of the cannabis oil left, I could post a picture if anyone wants to see.

The final light yellow oil could then be worked to isolate the THC, but I have never carried that out.

PainKilla, those pictures about THC acetate are text from the book entitled "Marijuana Alchemy", by D.Gold.
It's an interesting little book.


[Edited on 9-2-2005 by CycloKnight]

[guest]

@ TD,

Some info I hope you will find helpful:
JohnWW - 9-2-2005 at 23:29

Cycloknight talks of using 95% ethanol as the solvent for cannabis oil. Because 95% ethanol carries a very high excise tax/duty in most countries, it is quite expensive, unless you can distil your own from materials like sugar, whey, sugary fruits, or starch. It is likely to be cheaper in many places to buy substitutes like methanol, propanol, isopropanol (the 68% azeotrope sold as "rubbing alcohol" is probably not good enough, though), tert-butanol (forms a 65% azeotrope); or else acetone. Most other otherwise suitable solvents are not completely miscible with water, or they form an azeotrope which is over half water. Whatever is used could, in theory, be distilled off afterwards, although contaminated by water in the case of those that form azeotropes. Of course, "denatured alcohol" or "methylated spirits", sold in supermarkets as a cleaning agent or fuel, being ethanol adulterated with methanol, a blue dye, and other substances such as pyridine or sucrose acetate to make it unpalatable, is much cheaper, but the contaminants may be undesirable for solvent extraction.

[Edited on 10-2-2005 by JohnWW]

[Edited on 10-2-2005 by JohnWW]
N

[guest]

FWIW,

An interesting breeding project I am soon starting is to try and breed so-called cannabinoid "knockout" chemotype/genotype (IIRC). Thus CBN, THCV, THC, acids, etc, will have no effect. This variety serves as a placebo control in medical studies on medical values of cannabis substances.

[TheForSaken]

"I have never used chloroform, so I can't comment about that. (I mean for the soxhlet extractions...)"

Can the chloroform be subtituted with DCM?

[Green Supreme]

That second last one, was that not a method you suggested inappropriate? Peace GS

[guest]

Hey GS

It only inappropriate in regards to efficiency, easy of use, total yield, non-separation of THC (for example), cleanleness (residue), etc.

For a DIY person a soxhlet extractor is a fair option. My biggest concern is that the extract is a mishmash, not a pure extract. More like hash oil, than THC extract. But the same can be said for n-butane extraction. Like some of you guys pointed out, terpenes can be very useful indeed! Using an soxhlet extractor is not for novices who are not willing to experience more error than success at first. However, ATM I still suggest n-butane extraction like that of the Tamisium.

The small, medium and medium/large Tamisium extractors are 'set it and forget it'. Easy for most novices and very efficient. I foresee much better and less unhealthy oil from the Tamisium extractors verses a soxhlet extractor for the novice.

Considering a decent soxhlet extractor can cost around $800 I would instead buy the medium sized Tamisium extractors which are also around $800.

The extracts should be cleaner from the Tamisium than the soxhlet extractor for novices.

I think one would be much, much happier with a Tamisium butane extractor than a soxhlet extractor...

I am ordering a Tamisium someday to try it out.

Warning:
The author suggests toluene but not a fume hood! Toluene is hazarduz and should be handled under s fume hood.

HTH

[guest]

Thanks for the reply Gojo.

But i still do not get what type of contaminant would remain in my hash oil when using top quality 94% alcool. From what i understand, the biggest downside is the price it costs...
cheers

[Green Supreme]

If its 94% I imagine that leaves 6 percent for contaminant. Peace GS

[TheForSaken]

You can't distill the alcohol even with a tall fractional, it will form azeotropes with the water, so why don't you simply use andydrous magnesium be generous-stir-let sit 10 minutes-stir again-then use gravity/vacuum filtration.
Always keep some Mg in the bottle of alcohol with a tightly sealed lid, otherwise she'll re-absorb moisture real quick.
Regards
TFS

[blat]

I'm wondering if anyone has ever extracted the essential oils with steam-distillation. I've always wanted to try but am weary as it is a potentially expensive experiment if it requires a lot of starting material.

[Alchemist]

"I have never used chloroform, so I can't comment about that. (I mean for the soxhlet extractions...)"

Can the chloroform be subtituted with DCM?

any chlorinated solvent will degrade THC from what ive read

[Alchemist]

I'm wondering if anyone has ever extracted the essential oils with steam-distillation. I've always wanted to try but am weary as it is a potentially expensive experiment if it requires a lot of starting material.

I think Shantibaba from mr nice seeds had an operation doing just this in switzerland before the crackdown there

[guest]

If its 94% I imagine that leaves 6 percent for contaminant. Peace GS

But in the case of food grade alcool, isn't that 6 % comprised of water? what type of contaminant can they put in a product designed for human consumption?
cheers

[Green Supreme]

Agreed, I would like to know what that 6% is too. Peace GS

ps. I like the idea of alcohol better in many ways than iso and butes

[guest]

Here is great resource:

"Introduction to secondary metabolism in cannabis"
Author(s): Isvett J. Flores Sanchez and Robert Verpoorte
Pharmacognosy Department, Institute of Biology, Gorlaeus Laboratories, Leiden University
Leiden, The Netherlands; 2008
https://openaccess.leidenuniv.nl/bitstream/1887/13206/6/01.pdf

Abstract**
Cannabis sativa L. is an annual dioecious plant from Central Asia. Cannabinoids, flavonoids, stilbenoids, terpenoids, alkaloids and lignans are some of the secondary metabolites present in C. sativa. Earlier reviews were focused on isolation and identification of more than 480 chemical compounds; this review deals with the biosynthesis of the secondary metabolites present in this plant. Cannabinoid biosynthesis and some closely related pathways that involve the same precursors are disscused.

[guest]

Hey,

Ill look into the alcohol now, but AFAIK the terpenoid and flavonoid profile of n-butane should be higher than alcohol...

[Green Supreme]

Ya but the 6% in alcohol may be less harm that the ethyl mercapitans used in butane. Be nice if you could get the butes without mercs but that does not seem an easy task. Peace GS

[guest]

Hey GS

In the US its not a problem to get pure n-butane (iso-butane is not good); I believe AirGas sells it. In Canada its not available? Have you checked welding supply shops?

Hey TD,

From what I understand 190 proof ethyl alcohol (~94%) is fine, though drying the extract under a high velocity fume hood or a vacuum desicator, or specific vacuum drying apparatus would make me feel better.

This should provide all info needed for food grade ethyl alcohol (190 proof, eg. 94%); tho I have not read it, I hope its not all about fuel grade. From what I understand grape alcohol is more ideal than corn for extracts; and organic is available:

"Ethyl Alcohol Manufacturing: 2002"
www.census.gov/prod/ec02/ec0231i325193t.pdf



Some relevant info on iso-oil, though I would not smoke it:

"On the safety in use of isopropyl alcohol and isobutyl acetate for the extraction of beta-carotene from Blakeslea trispora"

EUROPEAN COMMISSION
HEALTH & CONSUMER PROTECTION DIRECTORATE-GENERAL
Directorate C - Scientific Opinions
C2 - Management of scientific committees II; scientific co-operation and networks
Scientific Committee on Food Opinion of the Scientific Committee on Food
(expressed on 5 March 2003)

http://ec.europa.eu/food/fs/sc/scf/out165_en.pdf

[Green Supreme]

I thought that if it was for sale to the public that ethyl mercapitan had to be added. It is put in because butane is odorless making leaks hard to detect. Peace GS

[c-ray]

I'm wondering if anyone has ever extracted the essential oils with steam-distillation. I've always wanted to try but am weary as it is a potentially expensive experiment if it requires a lot of starting material.

it'll only grab the water soluble essential oils (terpenes) and not the cannabinoids

[c-ray]

If its 94% I imagine that leaves 6 percent for contaminant. Peace GS

the 6% would be mostly water and perhaps a bit of pesticides, herbicides, etc from the grain it was made with

it's possible to temporarily remove most of that water with a molecular sieve that has zeolite 3A beads

[c-ray]

n-butane like all petroleum distillates are nearly impossible to separate completely from cannabinoids, not exactly something we want to be feeding to sick people
like I said previously skunkman already did the work on this, no need to follow a dead end path

[guest]

Hey,

Ill look into the alcohol now, but AFAIK the terpenoid and flavonoid profile of n-butane should be higher than alcohol...

probably so...
But at he rate of the use i make of it, i doubt it will effect the final product that much.i.e.:

I take about 10 to 15 % of the extracted dried trichomes and submit them to the alcool, evaporate, combine the 90 to 85 % of trichomes to the oil. I find this gives a nice

[Green Supreme]

Hallelujahh C-ray. Sure love to see that info though. Peace GS

[guest]

@ GS

Nah, that's only when its used to het. Home, for example. Pure n-butane is common in the US, not sure bout Canada.


n-butane like all petroleum distillates are nearly impossible to separate completely from cannabinoids, not exactly something we want to be feeding to sick people
like I said previously skunkman already did the work on this, no need to follow a dead end path

Right now I don't agree. All evidence and data I have seen seems to claim the opposite, as long as a vaccume is used, as it is in the Tamisimu extrator AFAIK. N-butane is supposed to be rahter easily removed.

I would love to be proven incorrect as I don't want to mess with unhealthy substances. But until I am shown otherwise I don't agree. You seem to know Mr. Skunkman? Could you ask him for data or other infos?

I don't see this as a dead end, but I would be hppy to be proven wrong.

Thanks

[guest]

the 6% would be mostly water and perhaps a bit of pesticides, herbicides, etc from the grain it was made with

it's possible to temporarily remove most of that water with a molecular sieve that has zeolite 3A beads

That's interesting C, I hadn't thought of that. I have glass microfilters from Whatman (GF) filter 0.7 micron. Will be used to filter mushroom particulate when testing psilocybin with TLC, which otherwise can mess up micropipett spotting and solid phase runs.

I can get larger microfilters for greater throughput but I may test filtering Everclear through the microfilter I already have.

Thanks

[Green Supreme]

Just a note. He doesn't have to know the man to be aware of his research. It and he{Sam the Skunkman} are quite legendary in our field. Kinda surprised you have not yet encountered any of his work in your research{Not dissin your researching. I am grateful for your contributions}. Might wanna look further into said fellow and his work. Peace GS

ps. I have heard from several people in the US using 4x refined butane bought in stores that say it has smell

[guest]

Hey bro,

I only assumed C might know him because C has broguht him up a few times. I assumed that meant C had read info by Mr. Skunkman, but no one has links to offer, or info. So that made me assume it was from personal communication like email.

I might have read info from Skunkman without knowing it, re: the GW book. I don't read icmag in general. I read the GW website after you guys mentioned it, but it has little info, tho all of it top notch. I searched for "sam skunkman" on google and got few results. I do most of my research in journals and big University libraries for original hard cover studies not on-line. If you have links I would be happy to read and catch up.

The limited info I found on icmag from Skunkman was of no value as the topics were not advanced.

I have no doubt he's a very smart guy, and that we all owe A LOT to him. I am not saying C-ray and skunkman certainly are wrong; just from what I know they are. I simply have not read info to the opposite. I would very much like to read the 'why's', I believe I could be wrong but I want to see why first. No offense intended to anyone, I'm a skeptic by nature most of the time, I like to 'why's and how's'.

No worries GS, I didn't take offense.

Many butane sources from a store is not pure, can be iso-butane too. A welding supply shop or service should have pure n-butane. AirGas in US sells it. I assume the butane from stores which smells is for a hibache grill or similar? Then the smell is required for safety. On the old OG there was a long list of sources for pure n-butane. Ill try to find it.

Shalom

[Alchemist]

I would think that butane would leave behind trace amounts in the extract as hexane is known for that as well. Could be the whole reason co2 was developed as a solvent.

I heard a story that goes like this

bavarian law of purity from 1516 governs that beer may only be made with 4 ingredients. hops, barley, malt and water.

~1900's , beer makers discover that a extract of hops can be used to make beer rather than pure hops, the concentrated form provides an easy form of hops for flavoring beer. they use hexane to make the extract and then remove the hexane. prolly a soxhlet as franz vons apparatus was widely used.

1960's with the advent of GLC for analysis of trace compounds reveals that certain beers contain trace amounts of hexane which is in violation of the bavarian law of purity.

around the same time co2 was being explored for its solvent properties in german labs, someone began using it to extract hop oil, which doesnt have any trace hexane remaining.


so, beer is resposible for co2 extraction technology....


* this may be true or maybe parts of it are true, we may never know *


peace

[guest]

Hey A,

That's an interesting story, thanks. I'm spending all day today on this topic. But I do agree that co2 is the way to go. Hummm, too bad we don't hangout together; we could do a group purchase of a single unit. I plan to buy a unit in the next year or two, max.

[guest]

While one the topic of oils...

Where do you guys get your oil pipes from? I am in the market for a nice glass vaporizer for oil and kif. A guy on icmag makes dank ones, I PMed him to see if he's still making them. Then there is www.okif.com they are supposed to sell the jam oil vaporizer as a glass bong. I go to the site and see no products.

So, how do you partake? And where do you get your piece(s) from?

I will post the link to the icmag thread in a minute

Thanks!

[guest]

Here the link for the vaps:

https://www.icmag.com/ic/showthread.php?t=27329



Here what the guy wrote re: making me a vap:

i designed an oil vaporizer that uses a titanium metal pad that is held on a hinge to swing under a down pointing tube that goes into a small water bubbler pipe. you heat the pad red hot and then drop a small dab of oil on it with a poker of some sort. the water chamber makes the oil vapor much much smoother. its very much like a one plate hot knife attached to a small waterpipe. i have a long waiting list for people who want them. if you look in my pictures ,you will see pictures of them.

peace.



It seems like one could use a standard bong and just buy the upside down bell bowl along with a titanium plate to place under the bowl. So one heat the titanium to THC/THCV temps with a vap gun with temp control. Then drop some oil or kif on the titanium plate. There are even titanium spoons one could use very well. In that thread at icmag there are sources for the upside down bell bowl, and then all one needs is titanium plate/spoon and a vaporizer heat gun.


http://i47.tinypic.com/2dgq9g9.jpg

http://i49.tinypic.com/rrme8g.jpg

[spaceman]

hashmasterkut

[guest]

Hey v

Yea he's the guy, but he's on a huge waiting list :( how about okif? Has anyone bought or used one? Where the hell is the product page on www.okif.com ?

I think I will need to build mine piece by piece, no one seems to be selling them
Thanks

[Green Supreme]

He's no secret here. Peace GS

[guest]

Who is no secret?

I didn't think I had secrets, that's why I asked where I can buy one. But I guess no one uses a setup like that? Otherwise I guess she/he would have told me where I can buy one.

Still hoping to find a unit I can buy...

[Zaxby]

This company has a new item: http://www.aqualabtechnologies.com/concentrate-utensils/skillet-vapor-curve.html

If I made iso-oil more I'd get one.

[guest]

Thanks! I hope they get in stock soon. I want the 45 degree one, and that's great the Ti plate is ready to go with the bowls wire. Schweet.

[Lungus]

The item in the pictures your inquiring about Gojo is called the Unobtanium Budder Bong and there are only a few around and they are custom made. I have one of them that I bought from someone else. By far the best way I've ever smoked oil. If you could show the picture to a glass blower and get them to make something similar, you could take a bicycle spoke and a small titanium plate and make the swingarm part yourself.

[c-ray]

you can use those with bho too
looks like a knockoff of the unobtanium vape developed by hashmasta kut

[Alchemist]

what kinds of yields are folks getting with their butane extractions? from buds? from bud trim? etc..

thanks in advance guys

[c-ray]

usually it's like 1-3g per oz

[outdoordreams]

I get 0 grams using butane................cause I refuse to use it!

[c-ray]

what you don't like poisoning yourself?

[Green Supreme]

Sorry my mistake. Oh Gojo I meant hmk is no secret here,. He used to be a member and if you do a search you will find we have an old unobtainium thread here. Peace GS

[guest]

Hola,

Can't you guys prove your opinion? I mean you are really positive yet no one has any info to show, how then did you guys form your opinions? (ODD, I'm not referring to you)

No offense intended, but I don't understand how you all formed your absolutist stance without a shred of data (at least that's what I've been shown/found so far).

I recently found some more info backing up my point; though its authority is questionable. I want to ask at a chemistry forum (non-cannabis) before I make up my mind.

Even if there was trace levels of butane how do you know its a harmful level? (See the study on health of iso-oil). Now one can say any residue is too much, and I would agree. However, I would also say that bubble hash or kif, etc, can be more unhealthy then high quality n-butane extracts that may have a very tiny bit of left over butane. Please see my previous posts. Raw cannabis can have harmful microbes, minerals, pesticides, etc.

FWIW, I sure hope you guys don't smoke herb grown with chemical salts, of which one macro is often radioactive (IIRC-see Lucas info), because it seems reasonable to assume it is less healthy then organic cannabis...no?

From my recent readings it seems a nanofilter might be able to separate n-butane from soybean oil (extract); I need more time for research as I am still unsure and don't fully understand yet.

Thanks for any info anyone can offer.
Shalom

[guest]

GS,

Ah, gotcha, thanks :)

[guest]

Hey all,

This big quote is from Erowd, ill post the link aand author in a few. Very good reading so I thought its worth posting the whole thing. Some butane info from below:


BUTANE (C4H10, n-butane, methylethyl methane, butyl hydride)
prop: bp -0.5 C
dis: oils
pol: non-polar
sol: ether, alcohol, water
otc: anywhere (butane cigarette lighters)
uses: lighter fuel, butane torches, curling irons (yes, really)
caution: extremely flamable
note: if you use this, you will have to work with sub-freezing temperatures or at least higher pressures like a small jar with a tight lid (higher pressures tend to raise boiling points thus improving solvent capabilities). the advantage is that you could boil it off at room temperature!





OTC Solvents FAQ

v1.0

This is version 1.00 of the OTC Solvents FAQ. It was preceded by two
draft versions, one of which has been widely distributed. This
version has been significantly updated, expanded, and corrected
Please destroy any earlier drafts of this document, as the
corrections and clarifications in this version may help avert
potential disasters which could result if the older information is
relied upon.

Significant effort has gone into the preparation of this FAQ, but it
is still lacking in a few areas. I need help with improving the
"solvents" section, especially what these solvents will and will not
dissolve. Some of the solvents listed are missing information on how
polar they are. It would also be nice to know which are the best
solvents for various substances.

Also, I would like to expand the "other substances" section,
specifically adding information on what will and will not dissolve
various interesting substances (or substances contained in) including
but not limited to: cinnamon, cannabinoids, citrus oils, DMT and
relatives, hot peppers, psilocybin/psilocin, aromatic oriental
mushrooms, LAA, garlic, opiates, ginkgo biloba, coca/cocaine, ephedra,
pseudoephedrine, ginsen, kava, and anything else you have information
on. (Information on any controlled substances would be just for the
purpose of satisfying curiosity; not to do anything illegal, of
course.)

I only took about 1 year of general chemistry in college, so I am not
exactly an expert on organic chemistry. It would be wonderful if
someone who is more knowledgable would suggest massive improvements
to the FAQ, or, better yet, if they would take over maintenance of
this FAQ altogether. Just keep in mind that the intended audience is
the not-too-much-above-average kitchen chemist. (Sometimes, it seems
that the more knowledgable people get a little too impatient with the
less knowledgable ones. Please don't be arrogant.) It wouldn't
hurt, however, to add extra information that would be useful to more
experienced chemists.

Please post any comments/additions/corrections to alt.drugs.chemistry
(or e-mail them to me by replying to the anonymous remailer if you
can figure out how to do it). Unfortunately, my news feed sucks, so
I may not see the comments posted to the alt.drugs.chemistry. If you
feel your comments have not been addressed within a week or two,
please post again so I will have a greater chance of seeing it. All
additions to this FAQ derived from comments, etc. will remain
anonymous unless otherwise requested.

Many thanks to those who have already contributed to this work.

========================= OTC* Solvents FAQ =========================

* OTC = over-the-counter

First draft: by "The Goose" on September 29, 1994
Draft version 0.1: by "The Goose" on October 25, 1994
Version 1.00: by "The Goose", last updated on May 19, 1995

PURPOSE: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

This document is intended to provide information on solvents and
other substances to people who have less than an expert knowledge of
chemistry. This information can be used as an aid and a reference by
kitchen chemists, etc. who desire to do relatively simple organic
extractions (e.g. THC from pot, DMT from whatever, LAA from morning
glory, psilocybin/psilocin from shrooms, etc. for those who don't
mind breaking the law. Mint oil, citrus oils, and essences from
various herbs, for those like myself who would rather stay legal.)
Recipes for organic extractions are not provided here. There is an
extensive file on organic extractions at hyperreal.com (in
/drugs/misc/chemistry-extracting).


DISCLAIMER/WARNING: . . . . . . . . . . . . . . . . . . . . . . . . .

I do not advocate breaking the law. References to illegal substances
are included, however, for informational purposes only (just to
satisfy everyone's curiosity). The authors of this document assume
no responsibility for the actions or consequences of what anyone may
do with this information. Even though efforts have been made to
assure accuracy, the information presented here is not guaranteed to
be accurate or complete. The use of any information contained in this
document constitutes an agreement to release the authors from any and
all liability for the said use of this information no matter what the
outcome of that use may be.

Most of the substances discussed in this FAQ are toxic to one degree
or another. Usually, after sufficient evaporation/separation/etc.,
such small quantities remain, that there is not a great risk of
poisoning, but you still need to watch out for contaminants. Many of
these substances contain contaminants of unknown toxicity. DO NOT
ingest unless you know what you are doing! You have been warned!
Also, it is not a good idea to breath the fumes from most of these
substances. You could get poisoned that way too. When evaporating
or boiling off solvents, make sure there is adequate ventilation.
Most of these solvents are flammable (or explosive). When working
with flamable solvents, avoid sparks (e.g. from electrical switches)
and open flames (e.g. from gas stoves). Using a hot plate with an
extension cord to get it away from the house is a good idea. Good
ventilation is the key to preventing both poisoning by inhalation,
and explosions resulting from the build-up of flamable fumes.

ALWAYS read the label of the products before you purchase them to
make sure they contain what you are looking for, and are not mixed
with a lot of other unwanted things. (See section on PURITY)

P.S. This information is incomplete, Never assume that something is
safe just because the information is not there!

P.P.S. Only you are responsible for your own actions!!

P.P.P.S. Use your head, damn it!!!


---------------- Answers to Frequently Asked Questions ----------------

1) What is petroleum ether?

A: Petroleum ether refers generically to the lower boiling fractions
of petroleum. Analytical grades may be quite pure, containing
only hexane and/or pentane, and having a boiling point no higher
than 69 degrees centigrade. The lower boiling fractions are most
useful when the solvent is to be evaporated or boiled off. The
petroleum ethers most often mentioned on the 'net usually consist
of somewhat higher boiling fractions of petroleum (e.g. 100 to
175 degrees centigrade). These are more useful when the solvent
is to be separated and discarded (e.g. when removing oil soluble
contaminants from water soluble extracts).


2) Are ether and petroleum ether the same?

A: No! Petroleum ether is a petroleum product. "Real" ether is
more commonly known as diethyl ether or ethyl ether. Its chemical
formula is C2H5-O-C2H5, and it is not a petroleum product.
Diethy ether is the "ether" that was traditionally used as an
anesthetic the early 1900's. Petroleum ether is sometimes
referred to as "ether" because its solvent properties are similar
to that of diethyl ether (i.e. it dissolves similar types of
substances and has a low boiling point). Often (but not always),
petroleum ether and diethyl ether can be used interchangeably.
It is usually easier for the layman to obtain petroleum ether.


3) Where can I get petroleum ether?

A: Chemical supply houses usually can provide petroleum ether. Ask
for it by boiling fraction or specific component (e.g. hexane,
pentane, etc.). It is best to have a reasonable knowledge of
chemistry when purchasing chemicals or solvents from professional
establishments. Many substances are controlled to some extent.
Often they will ask you to show identification, and sign a
statement explaining what your intended use is. This information
can be provided to government agencies such as the DEA. Since
most laymen would have a difficult time bluffing their way in a
chem supply shop, they probably would be tempted to use an
industrial grade which may be more easily obtained from local
retailers. These may take the forms of mineral spirits,
petroleum spirits, naptha, automobile starter fluid, etc. See
the SOLVENTS section below for more information on these products
and where to obtain them.


4) Where can I get solvent ?

A: Most solvents can be obtained from chemical supply houses. Just
keep in mind the precautions mentioned in #3 above. Many solvents
may be obtained from local retail establishments in industrial
grades either semi-pure or mixed with other (possibly useful)
solvents. For over-the-counter sources, see the SOLVENTS section
below.


5) What are polar and non-polar solvents?

A: The easy answer: Polar solvents dissolve substances that are
water soluble, but do not dissolve oily substances. Non-Polar
solvents dissolve oily substances, but do not dissolve water
soluble substances. Moderately polar solvents have a tendency to
dissolve both types of substances. Petroleum distillates are
non-polar, alcohols are moderately polar, and water is polar.

The better (but not necessarily more helpful) answer: Polarity
is a somewhat vague notion which gives a general idea of what
will dissolve what. The chemistry-extracting file at hyperreal
states the following:

Polarity and solubility is a nebulous concept. If you actually
look at what is dissolved by what, you can only find vague
general principles, and plenty of exceptions. Some authors
have tried to make 3 and 4 dimensional polarity or solubility
graphs, and put various solvents in various points as having
a combination of different types of solvent power.

See the SOLVENTS section below for more information on the polarity
of specific solvents.


6) What is the advantage of using a polar (or non-polar) solvent?

A: The advantage is that you are able to dissolve what you are
after, leaving behind the things you don't want. (e.g. petroleum
ether will dissolve cannabinoids but leave behind chlorophyll and
sugars. Alcohols and acetone will dissolve cannabinoids,
chlorophyll and sugars.)


7) What type of solvent should I use for extracting substance ?

A: Don't ask me. This FAQ was never intended to be a compilation of
recipes. Look at the various extraction techniques which have
been posted on the 'net or look in the chemistry-extracting file
at hyperreal.com. (hint: oily substances dissolve in non-polar
solvents, most other useful substances will dissolve in water.)


8) What is an acid-base extraction?

A: This is a technique in which alkaloids are extracted by taking
advantage of common solubility properties of most alkaloids. In
general, alkaloids are soluble in an acidic water solution, and
become insoluble when the solution is made basic. The solubility
rules for alkaloids are reversed for non-polar organic solvents.
The basic form (precipitate) is soluble in non-polar solvents,
and the acidic form is insoluble in non-polar solvents. Most
other materials in plants do not have these same solubility
properties. This allows for the isolation of alkaloids from most
of the other unwanted junk. For more information on specific
extractions, see the various extraction techniques on the 'net or
look at the chemistry-extracting file at hyperreal.com.


9) Why does my extracted material still smell like solvent?

A: Your extract may still smell like solvent because it still has
some solvent left in it or because some of the aromatic
components of the solvent are overstaying their welcome. Some
solvents have a high boiling point which makes it difficult to
separate it from your extract by boiling it off. Even if most of
the solvent solution boils off at a lower temperature, there may
have been a portion of it that has a higher boiling point. One
way to reduce the amount of excess solvent is to heat up the
extract even more. Be careful because higher heat may destroy
some extracts. Another way to lessen the smell is to to let the
excess solvent evaporate on its own by leaving your extract
exposed to the air for an extended period of time (anywhere from
overnight to several days). The down side of this is that the
longer your extract is exposed to air, the more it can be
destroyed by oxidation. Warmer temperatures encourage both
evaporation and oxidation while cooler temperatures do the
opposite. Room temperature is probably ok for most purposes. It
may well be next to impossible to get all of the residue out,
however. Picking a good solvent from the start can help you
avoid these problems to a large extent.


10) How dangerous are over-the-counter solvents?

A: It is always best to acquire reagent grade solvents, but since
this IS an over-the-counter solvents FAQ . . .
Some solvents are very dangerous by themselves while others are
almost harmless. Some contaminants in industrial grade solvents
could be quite dangerous (poisonous, carcinogenic, flammable,
etc.), while others are not. Most contaminants are not highly
toxic, and the government imposes some regulations on
manufacturers to prevent highly hazardous contaminants from being
distributed, so one could assume that the risks posed by
contaminants is fairly low. However, if you choose to use an
industrial grade, you always run some risk. Research and common
sense can help reduce this risk. See the section on PURITY below
for a more lengthy discussion on this topic. See the SOLVENTS
section below for information on the hazards of specific
solvents. See the OTHER SUBSTANCES section below for information
on the hazards of other miscellaneous substances.


------------------- REFERENCE & GENERAL INFORMATION -------------------

TERMS: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

"bp" = boiling point (or boiling fraction in some cases)
note: boiling points are slightly lower at high altitudes
"C" = degrees centigrade
"dens" = density (in grams per ml unless otherwise specified)
"dis:" = what it dissolves
"F" = degrees Fahrenheit
"LD50" = (lethal dose 50%) dosage at which 50% of test subjects
(rats, dogs, etc.) died.
"mis" = miscible with
"mp" = melting point
"otc:" = (over-the-counter) where to find it, etc.
"pol:" = polarity ( > = more polar than, < = less polar than )
"prop:" = physical properties
"sol:" = what it is soluble in
"tox:" = data on toxicity. if not listed, DON'T assume it is safe!
"uses:" = common uses. this is nice to know when you are asking a
store clerk to help you find it.


SOLVENTS: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

ACETONE (dimethyl ketone, ketone propanone, propanone)
prop: mp -94.6 C, bp 56.48 C, dens 0.80
dis: water solubles, oils; mis: water, alcohols, chloroform, oils
pol: polar?/moderately polar?
tox: oral LD50 (rat) 9750 mg/kg
otc: hardware stores (acetone)
uses: thinning fiberglass resins, dissolving 2 part epoxies,
cleaning brushes and tools used with resins or epoxies,
cleaning greasy stuff
otc: some drug stores (pure, small quantities, expensive)
uses: dissolving fats, waxes, etc.
caution: flamable, reacts with some solvents
note: acetone is also used in fingernail polish remover, but
it is mixed with water, fragrance, etc.
note: may react with some alkaloids, may extract more organic
compounds than is desirable

ALCOHOL see ethyl alcohol, methyl alcohol, isopropyl alcohol

BENZENE (C6H6, benzol, phenyl hydride, coal naptha)
(included for comparison and cautions)
prop: mp 5.51 C, bp 80.1 C, dens 0.8794
dis: oils; mis: alcohols, chloroform, ether, acetone
sol: slightly soluble in water (1 part per 1403 parts H2O)
pol: non-polar
tox: 3000 ppm vapor considered high concentration, toxic via
inhalation or skin absorption as well as oral ingestion,
prolonged inhalation of low concentrations also toxic
otc: none known (you wouldn't want it anyway)
note: do not confuse with benzine which is a petroleum distillate
caution: a recognized leukemogen (causes leukemia)!
caution: highly flamable
caution: can react vigorously with oxidizing materials

BUTANE (C4H10, n-butane, methylethyl methane, butyl hydride)
prop: bp -0.5 C
dis: oils
pol: non-polar
sol: ether, alcohol, water
otc: anywhere (butane cigarette lighters)
uses: lighter fuel, butane torches, curling irons (yes, really)
caution: extremely flamable
note: if you use this, you will have to work with sub-freezing
temperatures or at least higher pressures like a small jar
with a tight lid (higher pressures tend to raise boiling
points thus improving solvent capabilities). the advantage
is that you could boil it off at room temperature!

CHLOROFORM (CHCL3, trichloromethane)
(included for comparison and cautions)
prop: mp -63.5 C, bp 62.26 C, dens 1.498
dis: oils, fats, rubber, alkaloids, waxes, resins
sol: 1mL in 200mL water; mis: alcohols, ether, petroleum ether
pol: non-polar
tox: oral LD50 (rat) 800 mg/kg, prolonged inhalation can cause
unconsciousness and poisoning (or even death)
otc: none known
note: non-flamable
caution: reacts violently with acetone + base, methyl alcohol +
sodium hydroxide or potassium hydroxide

DICHLOROMETHANE see methylene chloride

DIESEL FUEL (fuel oil #2)
composed of heavier hydrocarbons than gasoline
prop: bp higher than gasoline
dis: oils
pol: non-polar
tox: recognized carcinogen, see also petroleum distillates

DECANE (CH3(CH2)8CH3)
a minor component of kerosene, may be a minor component of gasoline
prop: mp aprox -29 C, bp aprox 174 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: see kerosene, gasoline
caution: flamable

DIETHYL ETHER (C2H5-O-C2H5, ether, ethyl ether, anesthesia ether,
ethyl oxide)
prop: bp 35 C
dis: oils, etc.
pol: moderately polar ( < water, alcohols; > petroleum
distillates and toluene )
tox: moderate oral toxicity, low inhalation toxicity, oral LD50
(rat) 1700 mg/kg, oral LD50 (human) 420 mg/kg
otc: found in automobile starter fluid
caution: very flamable, can form explosive peroxides with
prolonged exposure to air
note: this is the ether that was used extensively as an
anesthetic a few years back

ETHANOL see ethyl alcohol

ETHYL ALCOHOL (ethanol, methyl corbinol, spirit of wine, grain
alcohol)
prop: bp 78.32 C, dens 0.79
dis: water solubles, oils; mis water
pol: polar? / moderately polar? ( < water; > isopropanol )
tox: oral LD50 (rat) 21,000 mg/kg
otc: liquor store (Everclear, 95%)
uses: party, party, party!
caution: flamable, could get you drunk :-)
note: there have been reports of people using denatured alcohol as
a solvent. this may be ok if it is denatured only with
something that will be eliminated when the solvent is boiled
off (e.g. with methyl alcohol). if you don't think you can
eliminate the denaturant, then don't use denatured alcohol!

FUEL OIL (fuel oil #1 through fuel oil #6)
increasingly viscous petroleum distillates, generally with increasing
boiling fractions.
dis: oils
pol: non-polar
tox: see petroleum distillates
caution: flamable
note: fuel oil #1 is kerosene, fuel oil #2 is diesel oil
note: there are not many applications that could benefit from
using fuel oils as solvents

GASOLINE (petrol, gas, white gas)
composed of octanes, some heavier hydrocarbons (nonanes, etc.),
and some lighter hydrocarbons (heptanes, etc.)
prop: bp aprox 35-180 C (depending on what it contains)
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: gas stations
uses: automobile, etc. fuel
caution: very flamable
note: gasoline for automobiles contains additives, better to use
white gas.

KEROSENE (fuel oil #1, ultrasene)
composed mostly of heavier hydrocarbons than gasoline (10 to 16 carbon
atoms per chain)
prop: bp 175-325
dis: oils
pol: non-polar
tox: oral LD50 (rat, rabbit) 28,000 mg/kg, oral toxicity is low,
see also petroleum distillates
otc: fuel distributors, hardware stores
caution: flamable
uses: stoves, heaters, lamps
note: ultrasene is deodorized kerosene

HEPTANE (C7H16)
a component of starter fluid, gasoline, and some petroleum ethers
prop: bp aprox 98 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: found in starting fluid and some napthas
caution: highly flamable

HEXANE (C6H14)
a component of starter fluid, and some petroleum ethers
prop: bp aprox 69 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: found in automobile starting fluid and some napthas
caution: highly flamable

ISOPROPANOL se isopropyl alcohol

ISOPROPYL ALCOHOL (dimethyl alcohol, sec-propyl alcohol, isopropanol)
prop: mp -89 C, bp 80.3 C, dens 0.79
dis: water solubles, oils; mis water
pol: polar? (hydrogen bonded?), ( < ethanol; >> diethyl ether )
tox: oral LD50 (rat) 5,840 mg/kg
otc: automotive stores (fuel dryer, 99.9%)
caution: flamable
note: rubbing alcohol is usually only 70% alcohol, and 30% water

METHANOL see methyl alcohol

METHYL ALCOHOL (methanol, wood alcohol)
prop: bp 64.8 C, dens 0.79
dis: water solubles, oils; mis water
pol: moderately polar? (hydrogen bonded), ( < water, > diethyl
ether )
tox: oral LD50 (rat) 13,000 mg/kg, eliminates slowly and can
build up with repeated exposure/ingestion. toxic metabolites
include formaldehyde and formic acid. damages optic nerve.
otc: automotive stores
uses: fuel dryer
otc: hardware and paint stores
uses: shellac thinner, alcohol stove fuel
caution: flamable
note: often mixed with paint removers or varnish removers
note: good at penetrating cell walls and membranes

METHYLENE CHLORIDE (CH2Cl2, dichloromethane)
prop: bp 39.8
dis: oils
pol: non-polar
tox: oral LD50 (rat) 2136 mg/kg, VERY dangerous to eyes,
produces highly toxic fumes when heated to decomposition
(e.g. by open flames, etc.), may be carcinogenic in rats
otc: paint and hardware stores (mixed with methyl alcohol, etc.)
uses: paint and varnish remover
note: fire hazard is low (by itself)

MINERAL SPIRITS see petroleum spirits

NAPTHA (see below for types)
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: hardware and paint stores
uses: paint thinner, some lighter fluids, some spot removers
note: boiling fractions are similar to gasoline

NAPTHA (coal tar, naptha solvent)
prop: bp 149-216 C, dens 0.86-0.89
tox: see petroleum distillates
caution: flamable

NAPTHA, V.M. & P. (benzine, 76 degree naptha)
prop: bp 100-140 C, dens 0.67-0.80, flash point 20 F.
tox: see petroleum distillates
note: do not confuse with benzene
caution: flamable, autoignite 450 F

NAPTHA, V.M. & P., 50 degree flash
prop: bp 115-143 C, flash point 50 F
tox: see petroleum distillates
caution: flamable

NAPTHA, V.M. & P., high flash
prop: bp 138-165 C, flash point 50 F
tox: see petroleum distillates
caution: flamable

NONANE (C9H20, n-nonane)
a component of gasoline, a component of some napthas
prop: mp aprox -54 C, bp aprox 151 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: see naptha, white gas, gasoline
caution: flamable

OCTANE (C8H18)
a major component of gasoline
prop: bp aprox 126 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: hardware and paint stores (some napthas)
otc: sporting goods stores (white gas)
caution: highly flamable

PAINT THINNER see petroleum spirits, turpentine

PAINT and VARNISH REMOVER
usually composed of methylene chloride and methyl alcohol. may also
contain toluene and other solvents. see individual components for
more information

PENTANE (C5H12, n-pentane)
a component of some light petroleum ethers
prop: bp aprox 36 C
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: see petroleum spirits
caution: highly flamable

PETROLEUM DISTILLATES (gasoline, naptha, petroleum ether, mineral
spirits, petroleum spirits, fuel oils, xylene, etc.)
dis: oils
pol: non-polar
tox: generally low to moderate toxicity, laboratory experiments
show a slight carcinogenic potential for most petroleum
distillates. higher boiling fractions may be more
carcinogenic.
caution: flamable to highly flamable
note: petroleum distillates do not dissolve most water-solubles
note: petroleum distillates include everything from pentane to
heavy tars

PETROLEUM ETHER see petroleum spirits, naptha, starter fluid
note: generally (but not always) refers to the lower boiling
fractions of petroleum distillates

PETROLEUM SPIRITS (petroleum benzine, petroleum naptha, light
ligroin, petroleum ether, mineral spirits)
prop: bp 35-180 C, dens .64-.66
dis: oils
pol: non-polar
tox: see petroleum distillates
otc: hardware and paint stores
uses: paint thinner
caution: flamable
note: "petroleum spirits" often refers to the lower boiling
fractions of petroleum distillates. However, one "odorless
paint thinner" claiming 100% mineral spirits had a boiling
point of 175 C.
note: do not confuse with benzene

STARTER FLUID
composed of hexane, diethyl ether, and heptane. see individual
components for more information.
otc: automotive stores
uses: starting stubborn automobiles on cold days
caution: very flamable
note: some starter fluids may contain heavier lubricants

alpha-TRICHLOROETHANE (CH3CCl3, 1,1,1-trichloroethane, methyl
chloroform)
prop: bp 74.1 C, dens 1.3492
dis: oils, etc.?
pol: non-polar?/moderately polar? (insoluble in water)
tox: oral LD50 (dog) 750 mg/kg, avoid fumes
otc: super markets, hardware stores, etc.
uses: spot remover (brand name: "Energine"), industrial uses
include cleaning of metal parts and metal molds
caution: can react violently with acetone
note: non-flamable!

TETRAHYDROFURAN (OCH2CH2CH2CH2, diethylene oxide, cyclotetramethylene
oxide-1,4-epoxy butane)
(included for comparison and cautions)
dis: oils, etc.; mis: water, alcohols, ethers, hydrocarbons
pol: moderately polar
otc: none known
note: peroxides may be removed by treating with strong ferrous
sulfate solution made slightly acidic with sodium bisulfate
caution: same as diethyl ether (slightly more dangerous)

TOLUENE (C6H5CH3, methylbenzene, phenylmethane, toluol)
prop: mp -95 C to -94.5 C, bp 110.4 C
dis: oils
pol: non-polar
tox: oral LD50 (rat) 5000 mg/kg, oral toxicity is moderate,
inhalation of 100 ppm can cause psychotropic effects, 200 ppm
can produce CNS effects
otc: paint and hardware stores (mixed with methyl alcohol, etc.)
uses: furniture refinisher, liquid sandpaper, paint remover
note: low fire hazard (by itself)

TURPENTINE (spirit of turpentine, turpentine gum, turpentine oil)
prop: bp 154-170 C
dis: oils ?, etc.?
pol: non-polar? (insoluble in water)
sol: alcohols, chloroform, ether, glacial acetic acid
tox: aspiration causes pheumonitis, oral ingestion causes damage
to GI tract and kidneys, inhalation toxicity is high
otc: paint and hardware stores
uses: thinning varnish, paint, & enamel; cleaning brushes
caution: moderately flamable

WATER (H2O)
prop: mp 0 C (32 F), bp 100 C (212 F), dens .99999 @ 4 C
dis: anything that is water soluble
pol: polar
tox: non-toxic unless contaminated with a toxic substance
otc: your kitchen sink (contains chlorine, etc.)
otc: grocery store (distilled water or purified water)
uses: drinking, washing, etc.
note: distilled water is better for most things (and it's cheap).
water is ofter used with petroleum ether to separate water-
solubles from non-water-solubles. i.e. combine and shake
vigorously until your arm falls off, then separate.

WHITE GAS (petrol, gasoline)
prop: see gasoline
dis:, pol:, and tox: see petroleum distillates
otc: sporting goods stores
uses: fuel for camp stoves and camp heaters
caution: flamable

XYLENE (C6H4(CH3)2)
prop: (m-xylene) mp -47.9 C, bp 139 C
(o-xylene) bp 144.4 C
(p-xylene) bp 138.3 C
dis: oils
pol: non-polar
tox: oral LD50 (rat) 5000 mg/kg, see also petroleum distillates
otc: super markets, hardware stores
uses: some cleaners (e.g. for dissolving chewing gum,
brand name: "Goof-off"), some lighter fluids
caution: flamable


OTHER SUBSTANCES: . . . . . . . . . . . . . . . . . . . . . . . . . .

ACETIC ACID (CH3COOH, vinegar acid, methane carboxylic acid, ethanoic
acid)
prop: mp 16.7 C, bp 118.1 C
sol: water
tox: oral LD50 (rat) 3310 mg/kg
otc: grocery stores (vinegar)
uses: cooking, cleaning
caution: dangerous in contact with: chromic acid, sodium peroxide,
nitric acid, potassium hydroxide, sodium hydroxide, xylene,
oleum. decomposition (at high temp.) evolves toxic fumes
note: normal vinegar is 5% acetic acid, vinegar concentrate is 18%
acetic acid
note: can be used for extracting some alkaloids from plant material

AMMONIA see AMMONIUM HYDROXIDE

AMMONIUM HYDROXIDE (NH4OH, ammonia, aqua ammonium, water of ammonia,
ammonium hydrate)
prop: mp -77 C
sol: water
tox: oral LD50 (rat) 350 mg/kg, oral LDlo (human) 43 mg/kg,
inhale LClo (human) 5000 ppm
otc: grocery & hardware stores
uses: household cleaning ammonia
note: ammonia is a gas at room temperature. it is sold otc
dissolved in water (much as is done with hydrochloric acid).
note: a weak base. can be used to precipitate some alkaloids
from slightly acidic solutions.

CANNABIDIOL (CBD)
found in marijuana, organicly converted to THC, can be isomerized
into THC by refluxing with dilute acid
prop: mp 66-67 C, bp 187-190 C @ 2mm Hg
sol: acetone, petroleum distillates, alcohols, etc.
note: this is an oily substance, not water soluble

CANNABINOL (CBN)
found in marijuana, a degradation product of THC
prop: mp 76-77 C, bp 185 C @ .05mm Hg
sol: acetone, petroleum distillates, alcohols, aqueous alkaline
note: this is an oily substance, not water soluble

EPHEDRINE HYDROCHLORIDE (C6H5CHOHCH(CH3)NHCH3 HCL, a[1-(methylamino)
ethyl]benzyl alcohol hydrochloride)
prop: mp 187-188 C
sol: water (1gm/4ml), (insoluble in diethyl ether)
tox: oral LD50 (mouse) 400 mg/kg
otc: truck stops (Mini Thins, MaxAlert, etc.)
uses: bronchiodialator (for asthma)
caution: decomposes into toxic fumes at higher temperatures
note: pure ephedrine is no longer available otc in the U.S. current
otc varieties usually have guiafenesin
note: slightly stronger that ephedrine sulfate
note: pure ephedrine can be converted into methcathinone
note: now a controlled substance in the US

EPHEDRINE SULFATE ((C6H5CHOHCH(CH3)NHCH3)2 H2SO4, 1-phenyl-2-
(methylamino)propanol sulfite)
prop: mp 247 C
sol: water (1gm/20ml), alcohol (1gm/0.2ml)
tox: oral LD50 (rat) 600 mg/kg
otc: same as for ephedrine hydrochloride?
caution: decomposes into toxic fumes at higher temperatures
note: slightly weaker than ephedrine HCl
note: pure ephedrine can be converted into methcathinone
note: now a controlled substance in the US

HYDROCHLORIC ACID (HCl, muriatic acid, chlorohydric acid, hydrogen
chloride)
prop: mp -114.3 C, bp -84.8 C, dens 1.639 g/liter gas @ 0 C
tox: oral LD50 (rabbit) 900 mg/kg
otc: hardware stores (muriatic acid)
uses: cleaning calcium or lime deposits from cement, brick,
swimming pools, and ceramic tile.
caution: caustic
note: useful in isomerizing CBD to THC. useful in extracting
some alkaloids from plant material. HCl is found naturally in
low concentrations in the digestive juices of your stomach.

LYE see SODIUM HYDROXIDE

PARAQUAT
an herbicide used by Latin-American drug enforcers to kill marijuana
crops in bulk
tox: oral LD50 (rat) 57 mg/kg, dermal LD50 (rat) 80 mg/kg, can
cause severe damage to lungs (nasty stuff!)
note: avoid all marijuana that looks like it has any dye on it.
unfortunately, not all paraquat is used with dye.

TETRAHYDROCANNABINOL (THC)
found in marijuana, the psychoactive stuff
prop: bp 200 C @ 0.02mm Hg (other cannabinoids may have bp's
lower than 185 C)
sol: polar solvents, acetone, alcohols, etc.
note: this is an oily substance, not water soluble

SODIUM HYDROXIDE (NaOH, caustic soda, sodium hydrate, lye, white caustic)
prop: mp 318.4 C, bp 1390 C, dens 2.120
tox: oral LDlo (rabbit) 500 mg/kg
otc: hardware stores, etc. (Red Devil Lye, etc.)
uses: unclogging drains
caution: highly corrosive to body tissue
caution: can react violently with acetic acid or tetrahydrofuran
note: useful in precipitating some alkaloids from acid solutions

SODIUM SULFATE (Na2SO4)
by product of isomerization of CBD to THC when sulfuric acid is
neutralized with baking soda
sol: water
note: insoluble in alcohol
note: can be removed by dissolving resin in petroleum ether
and shaking with water

SULFURIC ACID (H2SO4, oil of vitriol, dipping acid)
prop: mp 10.49 C, bp 330 C, dens 1.83
tox: oral LD50 (rat) 2,140 mg/kg
otc: plumming supply stores (plummers' sulfuric acid)
uses: unclogging drains
otc: automotive supply stores (battery acid)
caution: battery acid may have lead in it
caution: caustic, use care when mixing with water as it heats
rapidly when dissolved and causes spattering (add slowly to
water drop by drop)
note: useful in isomerizing CBD to THC

VINEGAR see acetic acid

[guest]

Part 2:


Substitution. . . . . . . . . . . . . . . . .

It is not always easy to come up with the exact solvent discussed in
any particular recipe. Consequently, it may be advantageous to
consider substituting an over-the-counter solvent for a hard-to-get
one. This can often be done successfully if you keep a few things in
mind. The main thing to look for is what the solvent dissolves.
If you are trying to dissolve an oily substance (such as cannabinoids
from pot or oil from lemon peels), look for solvents that will
dissolve oils (e.g. polar solvents, etc.). Be aware that some
solvents may dissolve more than you bargained for. Alcohols and
acetone will dissolve things that petroleum distillates won't, like
sugars and chlorophyll. Another thing to look for is boiling point.
Naptha solvent (coal tar naptha) has a boiling point so high that you
wouldn't be able to boil it off to separate it from THC (the THC
would boil off with it). Solvents with lower boiling points are
much easier to boil off, and usually leave less residual solvent.
Petroleum distillates are usually a mixture of various hydrocarbons
with a variety of boiling points. The boiling fraction of any
particular petroleum distillate refers to the range of boiling points
of its components.


PURITY: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

There are basically two ways that impurities can get into solvents,
etc. The first way is inherent in the manufacturing process. Very
few products are pure at the time of manufacture. The general idea
is to produce a product that meets certain minimum purity
requirements. The product is refined to remove contaminants until
the minimum purity level is reached. Most manufacturing methods
favor low cost production over purity of product. Industrial grade
products are used in applications that require only marginal purity.
With reagent grade chemicals, however, a high degree of purity is
required. Reagent grades are refined until they are ridiculously
pure (e.g. something like 99.999% pure). This additional refining is
costly, and as a result, reagent grades are usually many times the
price of industrial grades. Industrial grades are used in a lot of
commercial products, and are often available at hardware stores, etc.
Reagent grades are generally only available at chemical supply
stores. Unfortunately, most kitchen chemists would have a difficult
time bluffing their way in a chem shop without arousing suspicion.
Additionally, many reagent grade products are watched closely by
certain government agencies, where the industrial grades are not.
(e.g. acetone)

The other way impurities can be introduced is when the manufacturer
intentionally places additives into a product to enhance its
performance (or appearance) or to dilute an expensive component.
Since the performance enhancing additives usually cost more, the
expensive, big brand names are the ones most likely to use them.
When performance enhancing additives are present, the product labels
often boast a lot of features. The less expensive, more generic
looking products are less likely to add performance enhancers but are
more likely to dilute their product. Some additives may actually be
useful, however. e.g. Paint and varnish removers often combine
methylene chloride with methyl alcohol, and furniture refinishers
often have toluene combined with methyl alcohol.

When dealing with industrial grades, always read the label carefully
to determine if it contains things you don't want. Unfortunately,
not all products list every component on their labels. Try calling
the emergency accidental poisoning numbers listed on the labels.
Tell them your dog ingested some of their product, and that the vet
asked you to call the number. Try to get as much information from
them as you can about what the product contains. Work up a likely
story (including symptoms) before you place the call. One crude
method of testing for contaminants in solvents would be to place a
few drops on some clean glass, and let it evaporate. The amount of
residue remaining gives a very rough idea of how much other crud is
in the solvent. Feed a generous amount of this residue to the
neighbor's cat, and if it dies, the product may be too toxic. :-)

Actually, the likelyhood that contaminants in an industrial grade
product are highly toxic or carcinogenic is probably much lower than
most people think. Relatively few substances are highly toxic and/or
significantly carcinogenic. Many things in our everyday environment
are carcinogenic if you are exposed to massive quantities, but potent
carcinogens are not all that common. Due to government regulations,
many (if not most) industrial grade products are not allowed to
contain significant amounts of dangerous substances, anyway. (Who
wants a cleaner or solvent that will leave a highly hazardous
residue?) Even with all of these assurances, there is always a
certain amount of risk associated with the use of industrial grade
products.

In order to reduce the risks associated with contaminants, the
following precautions are in order:

1) use reagent grades when possible
2) if reagent grades cannot be obtained, then make every effort
to acquire the purest product available (read labels, study
manufacturing methods, etc.)
3) purify the product (if you can) before using it
4) use minimal amounts of these products (a liter of solvent
boiled down to a few cc's may still contain a liter's worth
of contaminants)


Some people recommend purifying petroleum distillates by adding
water, shaking vigorously for a long time, and then discarding the
water. This will only help remove water soluble contaminants. A
better way to purify most liquids is to distill them. Unfortunately,
this is not always easy to do if you don't have the right equipment.

One thing I have been intending to try is to shake paint stripper
(containing methyl alcohol and methylene chloride) with a generous
quantity of water to see if I can separate the methylene chloride.
If anyone has comments on whether this will work, please let me know.


USEFUL HINTS: . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Boiling off solvents with low boiling points (less than 100 C):

Place the solvent into a small pan or shallow, wide mouth jar.
Shallow containers with wide openings aid in allowing the vapors to
escape quickly. Place the container with the solvent into a larger
pan of simmering water. Don't allow the water to come to a full
boil. Boiling water is really no hotter than simmering water.
Rapidly boiling water can splash into your solvent, or cause the
solvent container to tip over. Watch the level of the solvent as it
boils away so that the container won't get too light, and tip over.
If the level of the solvent is too low (i.e. 1 cm below the level of
the water), then remove some of the water. Anchoring the solvent
container in place may help. Use hot pads to avoid burning yourself.
Remember to use good ventilation to avoid the build-up of toxic or
flamable fumes. If the boiling point of your solvent is too close to
100 C, you can add sugar or automobile antifreeze to the simmering
water to raise it's boiling point a little, or use the method below
for higher boiling point solvents.

Boiling off solvents with higher boiling points (greater than 100 C):

Follow the method and precautions for lower boiling point solvents
with the following differences: Use melted shortening (or vegetable
oil if you don't have shortening) instead of simmering water. If
your solvent container is glass, place it in the shortening as soon
as it is melted, and then heat it up from there. This will help keep
the jar from cracking. Elevate the solvent container slightly from
the bottom of the larger pan to aid in even heating. A few nails in
the bottom of the shortening works for me. Place a candy thermometer
in the shortening to measure it's temperature. Heat the shortening
until it is 20 or 30 degrees centigrade hotter than the highest
boiling point of your solvent or until the solvent begins to boil at
a comfortable rate. Always keep the temperature of the shortening
well below the boiling point of the dissolved product you are trying
to recover, or you may loose significant amounts of it to
evaporation. Be careful to not let solvent or water splash into the
hot shortening or you may get some spattering of hot grease. If your
solvent container is glass, allow it to cool slowly when you are done
to keep it from cracking. If you are extracting cannabinoids or
other oils of similar or higher boiling points, you may want to raise
the temperature of the shortening to about 160 C for a minute or two
to help eliminate solvent residue. (It can be tough to get rid of
all of it, though.)

Preventing boil-overs:

Some solvents may have a tendency to boil over quite easily. This
can waste valuable product as well as pose fire hazards, etc. By
making sure that the solvent level is well below the top of its
container, many boil-overs may be avoided. It is common practice in
chemistry to use boiling chips to control excessive boiling. Glass
marbles can serve the same purpose, and they are easy to get. Put as
many marbles into your solvent as needed to control the boiling.
Marbles may be removed a few at a time as the solvent level drops.
Remember that valuable extract may coat the surface of the marbles.
Wash them with a very small quantity of solvent and add this to the
rest of the solvent when it is mostly boiled off.

Refluxing in the kitchen:

Find a pan with a lid that can be put on upside down, and still
remain stable with a reasonable fit. Place your solvent, etc. into
the pan, and put the lid on upside down. Place ice in the lid. Heat
the solvent until it begins to boil gently. The heat may be applied
directly, or for better temperature control, you may use a method
similar to the ones listed above for boiling off solvents. If you
use hot shortening to apply heat, be careful to not let water from
melting ice or solvent condensing on the sides drip into the hot
grease. Tying a rag around the top of the solvent pan can help. As
the ice melts, scoop out the water and add more ice.

Getting rid of water in oil extracts:

Sometimes water can get into an oil extract when it is purified by
dissolving in petroleum ether, and shaking with water. As the last
of the solvent boils off, the water forms beads in the bottom of the
extract. These beads of water begin to spatter when the extract gets
too hot. By adding a small amount of acetone or alcohol, the water
will tend to evaporate off as the alcohol or acetone is boiled off.
Make sure that the alcohol or acetone is not contaminated with large
amounts of water or this may be counterproductive. This process may
be repeated until all of the water is gone.


REFERENCES: . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

- Dangerous Properties of Industrial Materials, Litton Educational
Publishing, Inc. (got a lot of good information here)

- CRC Handbook of Chemistry and Physics

- The Merck Index

- Some dictionary of technical and scientific terms

- Labels from numerous OTC products

- Comments from people on the 'net (many thanks to contributors)

- The chemistry-extracting file at hyperreal.com

- Things I remembered, but don't know where I read them

- My own ingenuity and experience (nothing illegal, of course!)

[Green Supreme]

We all been through this before about the time hmk was still here, so we are pretty bored with it. Maybe try the link to a thread at IC mag. Peace GS

http://www.icmag.com/ic/showthread.php?t=143983&highlight=butane+extract

[guest]

Ill look it up. But if its been investigated why no evidence put forth? I still agree n-butane is not ideal; but now I want to know if there is leftovers or not...

[c-ray]

have you tried talking to these folks:
http://www.internationalhempassociation.org/

[Alchemist]

I believe there will be trace amounts of butane remaining no matter what the separation method

Im not really sure if a bit of butane (esp pure n-butane) is bad for you...

if it is bad for you, should we all abandon our bic lighters in favor of magnifying glass' ?

[Green Supreme]

We use beeline. It is hemp twine that is coated in bees wax. Light it from a candle and avoid the butane altogether. Peace GS

[guest]

Hey all,

Well I joined a well known chemistry forum and asked the following question in the Organic Chemistry child-forum. The response(s) so far backs up what I have been writing, however, I still want to wait for more responses from other chemists at the organic chem forum...I'm still on the fence

It seems that according to the person who responded, as long as one makes high quality n-butane extract AND then makes it into budder. all n-butane will be gone :) I am still not convinced, but I'm close...

Note:
"Budder." = lightly heated and whipped; eg. emulsify. Heat just past the Bp (boiling point) of n-butane which is -0.5C, thus 'boiling' off n-butane.



"Fully remove all n-butane from extraction?"

Me:


Hi forum members,

I have been trying my damnedest to find the answer. I am interested in botanical extraction using pure n-butane as the extraction solvent. Am I correct in my understanding the under low vacuum all n-butane will be removed from the extracted 'oil'? If not is boiling the n-butane off at room temperature a viable option?

If not please point me in the right direction.

Thank you for your consideration, and I apologize for my rather simplistic question, Lukia



Chemist:

Hi there. I have performed extractions using this method before and although I do not have access to equipment which would allow me to analyse the extract to see how much residual butane there is, in theory the butane should evaporate off under normal conditions.

Butane boils at -0.5 degrees C, so at room temperature it should evaporate off your product. If you are worried about some butane getting 'stuck' in your extract then you could try heating the extract gently or dissolving the extract in a suitable solvent and then evaporating off the solvent. Don't think it should really be much of a problem though, I would be more worried about impurities left behind by the butane (unless you know it is pure).




Me:

Hi,

Thank you very much. I thought as much in terms of general ease in removing n-butane. I may have access to a MS but not for a while. Could you possibly suggest a solvent one could use to remove remaining butane if one believes there is indeed n-butane remaining? (And am I wrong in thinking that using a solvent to remove a solvent is less than ideal?)

I have access to pure n-butane and the extraction apparatus I am interested in operates under low pressure (IIRC 300psi) with working temperature at ambient room temperature and light vacuum to remove the butane.

Again, thank you for your time, Lukia

[guest]

I'm sure you guys have seen this:
(I have no idea if it's accurate/correct or not; pure is what is needed)

http://www.icmag.com/ic/showthread.php?t=31950

No source of pure N-Butane has been found available in stores, only through Gas Supply Companies. The best brand of butane I have used is Colibri Butane. I highly recommend Colibri, and you should be able to find it at most Fine Cigar and Tobacco Shoppe’s. Below is a list of other brands that are good for making Honey oil with. If you cannot find Colibri try to find one of the butane brands listed. And by all means avoid Ronson, Bernz-o-matic or other butane not listed below, they add smell to their butane and this smell is left behind making the oil taste very bad.

Other Brands that are good to use: COLIBRI, NEWPORT, CORA, CTC, COLTON, DUNHILL, DAVIDOFF, FACKELMAN, WIN, NIBO, SAROME, CALOR GAS MATCH, UNILIGHT, K2, SUPERGAS, VENTTI, VECTOR, King butane, Lucienne and Blaster. However this in no way is a complete list.

[guest]

@ C,

Not for info on butane, I have browsed it before tho. I will look at it, thank you for the suggestion.

Shalom

@ GS,

Is the wick stiff? That's pretty cool. But it sounds hard to use? I like not using lighters but the red stuff on a match worries me. Never thought about your method tho, I do like how it sounds.

[Green Supreme]

Here is a spoil and a pack. Peace GS

[guest]

Ah, thanks for that. So you dip it in beeswax? Or it is pre-dipped? Does it affect flavor/aroma of herb?

Thanks

[Green Supreme]

Predipped, it basically adds less taste than lighters or matches. Peace GS

[guest]

Cool. I'm totally going to try and source it, thanks man.

[Green Supreme]

Try here. Peace GS

http://www.freshheadies.com/catalog/beeline-29/

[guest]

(Thanks for the link)

Wow GS,

That guy HMK is a real douche bag! WTF is his deal? I don't get why he was sniping at you. And what's all this crap about [sic] "the bubbles are terpenes" and [sic] "I have proof but I keep my method and results secret". WTF, lol. You a troll? Gimme a break!

On a good note, that guy "NotaProfessor" is a good read, a smart guy. And if one reads through the mercaptan discussion (crap?) he seems to say as long as one boils off butane any present methyl mercaptan or mercaptan is boiled off; but I have some doubts about that.


Hummm:

NotaProfessor:
when a substance has a vapor pressure equal to the atmospheric pressure (=~760mm), it boils.

[#2 also adds to the H2S and mercaptan discussion as methyl mercaptan has a vapor pressure of 1520mm@26C. H2S is 15,600mm@25C. Butane is about 10,000mm@25C. All that shit's long gone as soon as it gets warm....

So basically above (^^^) NotaProfessor is claiming because all three substances have a vapor pressure above that of the atmosphere (~760mm) at 25-26C they will all 'boil' off (vaporize) from the oil. That is, once the oil temperature is greater than 26C the butane and mercs will vaporize, especially if one is whipping the oil.

A point worth mentioning is the bp of butane is -0.5C, which as the chemist I contacted wrote, would mean if the oil reaches -0.5C the butane will boil off. At first there seems to be a contradiction between NotaProfessor and the chemist I contacted, however, at -0.5C the vapor pressure of butane will be much lower than 10,000mm, while still being above atmosphere level of ~760mm, thus n-butane will boil off at -0.5C and 25C.

All in all, if one is not sure the butane is pure, making budder. with oil temp at 27C while quickly whipping oil should (according to NotaProfessor) boil off methyl mercaptan, mercaptan and n-butane. But I don't make any claims there; only about pure n-butane.

Why I will never use iso-oil:
[sic] "isopropanol is 44mm@25C" wow!
---

I for one would only use pure n-butane as I am now fairly certain it can be removed from the oil as I have described. I am definitely buying on of those Tamisium extractors; tho I want to know how they work first; ie. vacuum, etc.

To me much of that Icmag thread is garbage and a good example why I love C-W and hate Icmag. We act like adults here, even when we disagree. If anyone reads that thread start at page 3. I really like that science is welcome at C-W without a bunch of d.bags posting nonsense. This single thread at C-W probably has more, and better info on this topic then any other I have read (granted I have not read a lot of them). Keeping to science is the way IMO.

NotaProfessors info on farts was pretty comical and surprisingly relevant!

Interestingly here is a DIY vacuum/heat butane vaporizer setup:

Note:
The vacuum is not needed if one simply exceeds ambient vapor pressure (~760mm) and the bp of n-butane. Also note the oil doesn't need to boil, this author is using boiling water, far exceeding the bp of butane and probably lowering the quality of the oil...

Making budder. with oil will remove all residual butane; the heat and whipping are the key.

Hi.
Materials needed;
Bho
mason jar
foodsaver brand vacuum lid for mason jars
vacuum pump or foodsaver machine.
boiling water

To further remove residual B from BHO oil, I use a vacuum pump.
1-put oil in mason jar.
2-attach vacu lid and run pump.
3-put jar in hot/ boiling water
4-keep water hot and pump running till it stops bubbling.

The vacuum will lower the boiling point of the B and help remove it.
This will remove just about all residual butane.

[d'artanian]

On a good note, that guy "NotaProfessor" is a good read, a smart guy. And if one reads through the mercaptan discussion (crap?) he seems to say as long as one boils off butane any present methyl mercaptan or mercaptan is boiled off; but I have some doubts about that.

that shit is the one of the smellyest compunds known to man. thats why they use it as a contaminant. I belive that if it is present in any significant amount, you will smell it.

[guest]

Hey gerber,

Yea I agree. Did you read that thread GS linked to? The info NotaProfessor posted about smelling farts is very relevant. He posts a study showing the lower limit which we can smell farts, pretty interesting. I agree that if one leaves the extract in a small enclosed container overnight one will smell if even miniscule amounts are present.

I am pretty confident that using n-butane as extract solvent is totally safe (residue wise) as long as one fully boils off the n-butane. But like I mentioned, I'm not so sure about the mercs; even tho we should be able to smell nearly any level of its presence. To be sure I am still going to source pure n-butane.

Oh yea, did you see the s.extractor info I posted? That guy seems to like using n s.extractor.

I am for sure going to order a Tamiusim n-butane extractor if its legit, along with #1 and #2. Though #1 will take a while.

Peace out

[guest]

Cool, the chemist responded to my last question.

The chemist seems to agree using a Tamisuim n-butane extractor will remove all n-butane, re: vaccume; even tho a vaccum should not be necessary if making budder..

Where he muses about using a second solvent to [sic] "bring the 'trapped' butane to the surface so it can boil off" one can instead just make budder.; the whipping will also bring the 'trapped' n-butane to the surface...


Me:


Hi,

Thank you very much. I thought as much in terms of general ease in removing n-butane. I may have access to a MS but not for a while. Could you possibly suggest a solvent one could use to remove remaining butane if one believes there is indeed n-butane remaining? (And am I wrong in thinking that using a solvent to remove a solvent is less than ideal?).

I have access to pure n-butane and the extraction apparatus I am interested in operates under low pressure (IIRC 300psi) with working temperature at ambient room temperature and light vacuum to
remove the butane.

Again, thank you for your time, Lukia



Chemist:


I'm just playing around with ideas here really.

I think if you were going to give the solvent idea a try, you would use one which will dissolve all of your extracted chemicals so solvent choice depends on the extract. Butane is non polar, often produces a very oily, sticky 'tar' like extract from plant material. Because of the nature of the extract residual butane becomes a worry. I think that it extracts polar compounds too. You could try using a solvent with a higher density than butane, so that when the extract has dissolved in the second solvent, the 'trapped' butane is released and rises to the surface. If it has a lower boiling point (which it will if your other solvent is liquid under standard conditions) then it should evaporate off first.

I suppose that using a solvent to remove another solvent might be a bad idea, the second solvent in the idea I stated would probably be even harder to remove than the butane because of it's higher boiling
point. Considering your using a partial vacuum to remove the butane anyway, I wouldn't even bother.

Like I said I'm just throwing some ideas about. I reckon that when you get access to the MS you will find that the amount of butane left in the sample is minimal if at all. It would be interesting to hear what
the results are though when you analyse it.

What are the properties of the extract? What botanicals are you extracting from?

[guest]

Hey all,

Well I spoke with David, the owner creator of the tamisiume butane extractor. A real nice guy.

He told me he has not tested an extract with an MS. But, he agreed to split the cost of MS testing if I get the testing done. Then he can host the results. to me that speaks highly of his character and belief in his product.

He did tell me he tested an extract with HPLC and the purity was ~90%. If accurate HPLC results that is very good. Most BHO and budder. clocks in about 80%. We didn't discuss what he tested for but I'm sure you all can figure it out. I asked for the results but he said they got burned down with his house! The HPLC results was on the older design. I will test the extract with TLC and GC/MS. I will report all results.

So here the dealio:
(This is my understanding from speaking with the owner/designer of the butane extractor)

The separation tank runs at 100-110F using a custom hot plate, this will boil off butane; and supposedly mercs too (not sure on the mercs). N-butane bp is 32F (~-0.5C). One can purchase an accessory recovery tank to recondensate the n-butane.

The unit operates under pressure (IIRC 300 psi), and David said one can increase the pressure by 20 psi. The pressure in the unit, along with the heat, creates a vacuum in the separation tank, thus boiling off the butane under vacuum. The vacuum will 'pull' any 'trapped' n-butane (if present) to the surface to boil off.

One can actually add a real lab grade pump to the separation tank, increasing the vacuum. The problem is a non-sparking pump is expensive. The vacuum already present in the separation tank should be totally effective. (esp. considering n-butane in theory doesn't need a vacuum, boiling off is supposed to be sufficient)

David said a redesigned 1oz (raw matter weight) extractor will be available soon for $400-600. Those smaller units are great size, they fit on a dining room table and don't need to be broken down to reclaim the butane. Do not use the extractor inside unless under a fume hood!!!

After extract and separation is complete, I would still suggest one makes budder. as I described. Better safe, and paranoid, than sorry...

HTH. I will post lots of pics and info and assay results from the 1oz unit when I get it :)

[guest]

"OCCUPATIONAL SAFETY AND HEALTH GUIDELINE FOR n-BUTANE"
www.cdc.gov/niosh/docs/81-123/pdfs/0068.pdf

[guest]

I am very much liking NotaProfessor:
*
Vacuum [fractional] distillation would be a way to separate out terpenes from oil. Terpenes BPs are in the 50C range at 0.5mm pressure. Cannabinol and cannabidiol have BPs in the 150C range at 0.5mm pressure

[guest]

Finally!

Some info by SamSkunkman. According to what he wrote it is my belief the BHO he tested was not very good because he could smell the solvents. That, and maybe his GC wasn't calibrated correctly. I would like to see the results. Also, what's up with Sam using a GC to qunatitify the butane? Its possilbe but why not use a MassSpec?

Using n-butane extraction under pressure and then separation under heat/vacuum, and finally emuslified should in theory remove all n-butane. The problem is other gases they add to butane like propane, mercs, etc. If the butane is not pure n-butane then redissovling the extract to remove all impurities (hydrocarbons, etc) should make the extract completely pure.

I was also thinking one could put BHO in a inexpensive pump vacuum desicator in a DIY incubator at 100-110F. That would work well, especially if the BHO was not overly thick or too viscous. Set and forget for 24-48 hours.

Here is a great bit of info which is the actualized musings of the chemist I contacted; re: use a second solvent to remove the first (butane). However, this step should not be needed. However, I rather like the process and the end product should be as pure as conventional possible. I will test making BHO with and without this step using a GC/MS. In this step one would use pure ethanol ([sic] "spectroscopy grade absolute ethanol, which has virtually no impurities") to redissolve the BHO. Thus, 'un-trapping' any residue butane and most other impurities. One would then place the redissolved BHO into freezer at or below -20C for 24hours. The precipitate separates thus the butane and most other impurities (hydrocarbons not n-butane) separate from the extract; thaw and filter out the extract. Finally, place the extract into the vacuum desicator:

By "gunnaknow":
I've said this many times and repeat now - redissolve bho in ethanol and butan residue will be free to go out of solution.

To evaporate ethanol use vacuum if you have one and want to use it,
if you don't - double boiler will help to evaporate along with partial decarboxilation.



For pure extract this simple method may work

Even tho a vacuum desicator shouldn't be necessary. MS testing is needed


Dry and process raw cannabis under yellow light. Line dry or use a food dehydrator (low temp), or vacuum desicator to about <10% moisture content. Break up buds.

Pretreat raw dried cannabis with alakine water (pH >10 with caustic soda). Wash a few times with clean water.

Place filtered and washed cannabis in double the volume of water and bring to simmer for two hours.

Filter cannabis and dry as before.

Use Tamisumie extractor

Evaporate/boil off any residual n-butane with inexpensive pump vacuum desicator in a DIY incubator (100-110F; heat with yellow incandescent bulbs; heat-pad, hot water jugs, etc)

(not necassary and/or feasable?). Whip into budder. while still warm and semi-liquid state from the incubator

Enjoy!




For a VERY pure extraction I am trying this method:

This shouldn't be necessary; testing with MS is needed to see if this step is indeed necessary. I am trying this method for sure :) I DO like the idea of this extract process. This process would nullify any worries Sam has about the affinity of cannabinoids to butane. That is, all n-butane and most other possible impurities will be removed regardless of their affinity to cannabinoids.


Dry and process raw cannabis under yellow light. Line dry or use a food dehydrator (low temp), or vacuum desicator to about <10% moisture content. Break up buds.

Pretreat raw dried cannabis with alakine water (pH >10 with caustic soda). Wash a few times with clean water.

Place filtered and washed cannabis in double the volume of water and bring to simmer for two hours.

Filter cannabis and dry as before.

Use Tamisumie extractor

Dissolve BHO extract (and residual n-butane) with pure ethanol (only a little is needed)

Place solution in freezer (-20C) for 24 hours

Place redissolved extract at room temp to thaw and filter out extract with Whatman filter paper or better yet glass microfibre filter or the prefilter (model GF/B) or microcentrifuge, filter paper is the least expensive but also flimsy; both filters are easy to get at Ebay and Amazon. (rinse with distilled water?)

Evaporate ethanol and water azeotrope from extract using a glass or pyrex vaccum desicator in an oven set to 79C, or 174F for 12-24 hours until purged.

(not necassary and/or feasable?). Whip pure extract into budder. after extract has been warmed into semi-liquid state before re-solidifying.

Enjoy!


Here is a good thread from icamg, sam_skunkman posts one (odd?), but other posters have worthwhile info. HMK is still a d.bag in that thread too, crazy...
http://www.icmag.com/ic/showthread.php?t=120677



Sam_Skunkman:

(Please see the quote by gunnaknow after this quote by Sam Skunkman)

his is a simple home way to do what real labs use to get out all the solvents from extracts. If you analyze oil made with Butane with a GC you will find traces of Butane still in the oil no matter how carefully you try and remove all the solvent. A vacuum flask over boiling water is the best way to get all the solvent (or at least almost all removed). I think anyone who likes oil has tasted oil with solvent still in it, it is not nice, or good for you. I don't even like ethanol, which is pretty safe to consume small amounts of, but I just hate the taste and smell of any and all solvents besides my concerns for health reasons. Carbon dioxide can be used as a solvent, but until it is available I won't touch any oil.
Almost all of the BHO I have tasted in the past tasted to me of Butane, faintly at least.

The real problem is that because of the affinity of butane to THC, it works very easy to extract and is all that much more difficult to remove all the butane from the extract.

Every BHO I ever tested on my GC had small amounts of butane left in it.
Not surprising...

-SamS




Gunnaknow:

[Quote]Thankyou Hashmasta, I have read that page several times over the last few years. The oleaginous wax particles are hydrocarbons, like butane but they possess more carbon and hydrogen atoms, making them much less volatile. They are basically the hydrocarbons that you find in paraffin wax, with 20 or more carbon atoms. However, it's not just these solid at room temperature hydrocarbons that are the problem. As I said before, the Near Zero Impurities bench mark only sets limits on non volatile impurities.

There are volatile hydrocarbons that could also be present, that would also be hard to remove by purging. Hydrocarbons with more than 6 carbon atoms, that are liquid at room temperature, will be difficult to remove completely without the addition of vacuum purging. They are basically the order of hydrocarbons found in things like naptha and kerosene/paraffin. Alkanes like hexane, heptane, octane, nonane, decane etc and their related alkenes, alkynes, cycloalkanes and alkadienes. With the addition of low pressure, those hydrocarbons upto about c11 can be removed. Much past c11 and you start to get too close to the boiling points of cannabinoids.

However, there is another way to remove any residues of hydrocarbons above c11. The miscibility of ethanol with alkanes is limited to alkanes up to undecane (c11), mixtures with dodecane (c12) and higher alkanes show a miscibility gap below a certain temperature (approx. 13

[guest]

Ok me again!

@ TD, I think this should answer your original question?

More research and conclusions. Assuming I am going to use the extraction method using pure butane and then pure ethanol (95%) I wanted to know the bp of the azeotrope of pure ethanol (95.63%) and water (4.37%). It is lower than the bp of either ethanol or water. The bp of that positive azeotrope is 78.2C, which is also above atmospheric vapor pressure.

Thus, one filters the extract from the solution after 'thawing', eg. with a Whatman "glass microfibre" filter, or maybe just a Whatman "prefilter" for the glass filter above (model GF/B), or micro-centrifuge, etc. One could easily use a glass (or pyrex) vacuum desicator in an oven set to 79C, or 175F, to fully boil off the azeotrope of ethanol and water. Can't get more pure than that without specialized chemistry equipment.

And that's some pure extract! Even c-ray may agree? ;)

Easy peasy!

[guest]

Of course putting the ethanol extract in the oven may not be the smartest move safety wise...gotta come up with some more safe.

[guest]

A tip to dissolve the BHO with ethanol:

Use a ultrasonic bath, like the kind for jewelry, or the good lab ones, put the vial in the bath. Or test-tube shaker, or some other vibration apparatus.

Maybe affix the vial of BHO and ethanol solution to a paint can and using a paint can mixer (eg. Ace hardware) to shake the hell outa the solution. You don't have to say what it is, its an 'experiment'. Maybe buy the cheapest 1/2 or gallon of paint to use so they don't get annoyed.

GL!

[guest]

On the trail...

So I was reading about precipitating DNA with ethanol in the freezer. This is similar to what we want to do with ethanol after redissovling the BHO and placing in the freezer.

The freezer should reach or exceed -20C, residential stand up freezers will not come close. One could use a "reach in" horizontal 'meat' freezer, or a small lab grade freezer. After freezing it seems spinning in a microcentrifuge for 10-20 minutes will even further precipitate impurities into the very cold solution. Thus one has two stages of impurity precipitation: freezer and microcentrifuge.

It may be possible to only use a microcentrifuge.

I presented my current working method for extraction to the organic chemistry child-forum for review. I have a few open questions I hope they can answer such as use of freezer and/or microcentrifuge, washing cannabis with alkaline water (from caustic soda), aspiration or filtration or both, safety of using vacuum desiccator in an oven, etc.

MSDS of ethanol:
http://www.distill.com/materialsafety/msds-eu.html

[guest]

Some relevant info from a basement chemist calling herself/himself "Zero". Although IMO Zero's info is inferior to what I have presented so far (re: freezer, extraction, microcentrifuge, etc):

From an underground 'bible' by Zero[1]:

The best way to collect and store the oil is probably to let all of the butane evaporate off and then redissolve the oil in some anhydrous or high-% alcohol, and then pour this into a vial and let it sit out for a day or two to allow the alcohol to evaporate. Trying to transfer the oil into a small container while it is still solvated by the butane is too risky. I learned the hard way about this, thanks to the volatile temperament of butane. I had filled a vial almost all the way to the top and was preparing to drop those last couple
drops in, so that cleverly, I could let the last of the butane evaporate from the vial and the oil would all be neatly contained. But when the last drop hit the mother lode in the vial, it changed the temperature of the solution in the vial upward by a hair and it all "superboiled" out of the vial and onto my fingers, which of course startled me and caused me to drop the vial. I suggest dissolving it in alcohol as I mentioned above. If you can
get pure or 99% isopropanol (isopropyl), use it, because THC's photosensitivity reportedly does not occur in isopropanol.

The final product is a deep yellow-amber oil of the highest quality, incredibly pure and potent. I remember well some of the prime "honey oil" hash oils that hit the market in the late 1970s, and this stuff stands up to (if not exceeds) any of them. It's amazing how this method extracts only the good fraction and leaves the junk in the weed. But that's exactly what it does. Note also that this oil has a somewhat higher melt/vaporization point than traditional hash oils; the traditional dispensing method (dipping a needle or paper clip in,
getting some goop on the end, and warming it with a flame to get it to drip off into your bowl) still works with this stuff, but it seems you have to be more careful with it because it doesn't heat to liquid state as quickly or in the same manner, and it can more easily be
allowed to burn up on your needle. So be careful.

Those who prefer a tincture-like preparation can of course thin the product a little with a bit of warm high-percentage alcohol like Everclear or 90-whatever-% isopropyl, then drop it onto buds or let a joint absorb some, then let the alcohol evaporate. I also observed that unlike hash oil derived from traditional methods, this product is not immediately soluble in room-temp alcohol; it needed to be warmed before it dissolved fully.

So there it is. Spread the word far and wide: honey oil is BACK!





[1] "CLANDESTINE CHEMIST'S NOTEBOOK: (Manual for Drug Manufacture)"
By: Zero
OCT. 26, 2003
http://textfiles.group.lt/uploads/clandestine.txt

(The author Zero claims BHO extraction is supercritical, but I am unsure. AFAIK buitane is a critical gas.)

THE CLANDESTINE CHEMIST'S NOTEBOOK: Ver. 1

CONTENTS:


1: Methamphetamine ~"~"~"~"~"~ Crystal Meth, Speed
[List]
Birch Reduction Methamphetamine #1

Birch Reduction Methamphetamine #2

RXN Methamphetamine #3

RXN Methamphetamine #4

Getting Red Phosphorus from Matchbooks

2: Methcathinone ~"~"~"~"~"~ Cat, Jeff

Methcathinone Manufacture #1

Methcathinone Manufacture #2

3: GHB ~"~"~"~"~"~ Liquid E, Date Rape Drug

GHB Manufacture #1

GHB Manufacture #2

4: MDMA ~"~"~"~"~"~ Ecstasy, X

MDMA Manufacture #1

5: Phencyclidine ~"~"~"~"~"~ PCP, Angel Dust

Phencyclidine Manufacture #1

6: Cocaine ~"~"~"~"~"~ Coke, Blow

Cocaine Manufacture

7: Opiates ~"~"~"~"~"~ Heroin, Codeine

Extracting Codeine from Codeine Pills

Converting Codeine into Morphine, then into Heroin

Synthetic Heroin Synthesis (fentanyl)

Codeinone from Thebaine

Conversion of Thebaine to Codeine

Conversion of Oxycodone to Oxymorphone

8: Marijuana ~"~"~"~"~"~ Weed, Bud

Extracting Hash Oil using Butane

Extracting Hashish

9: Psilocybin ~"~"~"~"~"~ Shrooms, Caps

Growing Psilocybin Mushrooms

10: Salvia Divinorum ~"~"~"~"~"~ Dream Herb, Salvia

Producing Salvia Extract

11: DMT & 5-MeO-DMT ~"~"~"~"~"~ Toad Venom

Milking 5-MeO-DMT from Toads

Extracting DMT from Plants

DMT & DET Synthesis


12: Ketamine ~"~"~"~"~"~ Special K

Ketamine Manufacture from Scratch #1

Ketamine Synthesis #2

13: Dextromethorphan ~"~"~"~"~"~ DXM, Red Devil's

DXM Coricidin Extraction

Simplified Acid/Base Extraction of DXM

Converting DXM into DXO




Wheee!

[guest]

More info ;)

Well it seems that 0'F (-18'C, not -20'C), will suffice for the freezer stage. However, the author (below) doesn't mention precipitation of hydrocarbons like butane, etc. When in doubt go colder. Most domestic freezers are supposed to run from 0-5'F; thus one should be able to use the home freezer set to the coldest setting.

When I was reading about DNA I knew that -20'C may be colder than needed, however, with lack of info I figured better safe than sorry.


I want to read more about the proper temp for butane, etc, in ethanol solution in the freezer.

I have doubts one needs a microcentrifuge; placing solution in a freezer for 12 hours should be sufficient. But, I also assume a microcentrifuge has a better chance at a pure extract...

I think using aspiration and filtering, or at least filtering is better than adding water and bicarb as described below:

...
Rather than using filters, I always found adding lots of water (with a little bicarb to neutralize the acid) to precipitate it out, after both water & alcoholic solution had been chilled to 0'C caused the cannabinoids to precipitate out in a highly resinous form, so you could actually just decant off the liquid after leaving to settle (still at 0'C) for a while


And it looks like using an alkaline wash to pretreat cannabis to convert THC-COOH into THC is not wise. It seems the alkaline solution will itself convert THC to CBN. This is not good. So for now I think only simmering cannabis with water to "isomer" CBD > THC and "decarboxylate" THC-A > THC is wise.

Good info:
[Quote]The idea to increase potency of cannabis-derived oils by refluxing in presence of catalytic amounts of strong acids (normally toluene + H2SO4) is well known. The theory goes that cannabidiol is converted into delta8/9-THC. Well, all clear so far.

But I just found that delta9-THC itself decomposes upon longer contact with acids. As usual, elevated temperatures increase decomposition rate.

Ref: J Pharm Sci 1974, 63(10), p.1563

Let me just quote one sentence from the abstract:

[Quote]The half-life of delta9-tetrahydrocannabinol is about 15 min at 37

[guest]

A good point about increasing THC by converting THC-COOCH to THC vs the loss of THC during conversion of THC-COOCH to THC is most raw cannabis AFAIK has little (relative) amounts of THC-COOCH to start with

[guest]

Hmmm,

I'm trying to decide between molecular sieve anhydrous ethanol (spectroscopic grade ethanol) and ~94% food grade hydrous ethanol as the solvent for redissovling the BHO.

Spectroscopic grade ethanol is supposed to be a better solvent than ~94% food grade ethanol. However, storing pure ethanol can be difficult, tho adding a bit of Mg is supposed to help storage (thanks to someone one page 2 or 3 for that). Pure mthanol is expensive and most people don't have a molecular sieve, A3 zeolite, etc, sitting around to clean it up if incorrectly stored.

Food grade ~94% ethanol is a good and proven solvent. The azeotrope has a lower bp than either pure ethanol or water; thus one boils off ~94% ethanol at a good deal lower temperature. Storage and access to ~94% ethanol (Everclear) is easy. It seems a bit safer to use ~94% ethanol if boiling off ethanol from extract in a vacuum desiccator within an oven.

For now I am planing on using Everclear. Unless someone knows why I should use pure ethanol instead?

[guest]

I found a guy on icmag who seems to be contradicting the other person I quoted regarding freezer temperature. He says -21'C (-5.8'F) is good for ~94% hydrous ethanol (Everclear). The difference is only about 5 degrees and about 5 degrees lower than what a normal domestic freezer will reach. I'm going to try and pin down the correct freezer temp, but for now I am assuming 0'F (~-18'C) is sufficient.

Oh yea, to assist in redissolving the BHO into ethanol, besides assisted shaking, warming the ethanol is a great help.

This guy suggests the use of a NaOH (sodium hydroxide; caustic soda) bath with pH >10 to pretreat cannabis to remove chlorophyll. That's interesting, because as I mentioned an NaOH bath would convert THC-COOCH to THC. However, the NaOH bath will also convert the THC to CBN. A short bath under 5 minutes might be worth it, if using cool water the conversion of THC to CBN should be quite limited.


[Quote]
The best way to extract a good oil with alcool is to use it the cooldest possible (minus 21

[guest]

Info about using an alkaline wash (pH >10 with sodium hydroxide) as pretreatment:

(I am sure many of you have read all or most of this info already. I am posting here for reference and completeness of info.)

I made a few typos late last night, "THC-COOCH", should be "THC-COOH".

Using an alkaline wash is supposed to decarboxylate 2-carboxylic acids (2-COOH) to their respective cannabinoids (ex. THC-COOH > THC) and THC-A into THC. Not only that but alkaline bath is supposed to remove chlorophyll into the water as well. Using hot water may be wise (simmering); however, I am planing on simmer in plain water for 2 hours as the next step in the process (after wash in alkaline water).

I tried to find info showing alkaline bath will degrade THC to CBN, but I only found info showing acidic bath will do that.

1. Pate, D.W., 1994. Chemical ecology of Cannabis. Journal of the
International Hemp Association 2: 29, 32-37


Cannabinoids were originally thought to exist as the phenolic compounds, but later research (Fetterman et al. 1971a,
Masoud and Doorenbos 1973, Small and Beckstead 1973, Turner et al. 1973b) has indicated their existence predominantly in the form of carboxylic acids which decarboxylate readily with time (Masoud and Doorenbos 1973, Turner et al. 1973b), upon heating (De Zeeuw et al.
1972a, Kimura and Okamoto 1970) or in alkaline conditions (Grlic and Andrec 1961, Masoud and Doorenboos 1973). There are over 60 of these type compounds present in the plant (Turner et al. 1980).



2. "Why should cannabis products be heated before eating?"

http://www.cannabis-med.org/english/faq/12-heating.htm

In the plant the cannabinoids exist mainly in their carboxylic forms as cannabinoid acids. However, the phenolic form of THC is responsible for the psychotropic and the most medicinal effects. Decarboxylation (separation of CO2) to the phenolic form occurs readily over time, upon heating or under alkaline conditions.

The ratio of THC acids (THCA) to phenolic THC has been reported to range between 2:1 (Africa) and >20:1 (Switzerland) in leaves and flowers of Cannabis sativa. In plants grown in Middle Europe (United Kingdom) from Moroccan, Sri Lankan and Zambian seed stocks the THCA/THC ratio was 17:1 compared with 2:1 in the plants from the original areas (Africa, Asia). In hashish (cannabis resin) the THCA/THC ratio was reported to range between 6.1:1 and 0.5:1, the latter in hashish from India. Thus, the percentage of phenolic THC of all THC in cannabis products varied between less than 5% in cannabis leaves grown in Switzerland up to 65% in hashish from India.

Cannabis products with a high content of phenolic THC (e.g. hashish) may be very potent without heating, but usually the potency of cannabis products is considerably increased with heating (smoking, cooking).

Modified according to: Grotenhermen F. Pharmacokinetics and pharmacodynamics of cannabinoids. Clinical Pharmacokinetics 2001, in press.




3. "Cannabinoids: Encyclopedia II"

http://www.experiencefestival.com/a/Cannabinoids_-_Herbal_Cannabinoids/id/622322

Cannabinoids - Herbal Cannabinoids

Herbal cannabinoids (sometimes called classical cannabinoids) are nearly insoluble in water but soluble in lipids, alcohols, and other non-polar organic solvents. However, as phenols they form more water-soluble phenolate salts under strongly alkaline conditions. All herbal cannabinoids are derived from their respective 2-carboxylic acids (2-COOH) by decarboxylation; that is, catalyzed by heat, light, or alkaline conditions. Herbal cannabinoids occur naturally only in the cannabis plant, and are concentrated in a viscous resin that is produced in glandular structures known as trichomes. In addition to cannabinoids, the resin is rich in terpenes, which are largely responsible for the odor of the cannabis plant.[1]


4. by "Machine Elf"
http://www.icmag.com/ic/showthread.php?t=95343&page=2


As previously stated most THC in the plant is actually THCA, I believe typically 80-90% THCA in fact pre-decarboxylation. THCA is not psychoactive. As also stated why thinking an acid would cause decarboxylation of another acid is beyond me. An alkaline substance (base) or non polar solvent would be the logical key, as with heat. An acid is looking to donate a proton to a base. THCA has an extra COOH group attached which makes it acidic. Adding an acid (which is looking to donate its proton) to THCA will cause no reaction. Adding a base to an acid, which can accept a proton, will cause a reaction. But I am unsure if adding a base to THCA will cause a "true" reaction as there is no proton to donate when the CO2 decarboxylates (it goes back to the carbon) Hmmmm. Perhaps the base will merely act as a carrier for the donation of the proton, the CO2 decarboxylates and the proton goes back to the THC and the base is returned to its donor state. I am unsure as to the exact mechanism light, O2 and heat cause decarboxylation as well the mechanism involved with solvents as to what attaches where. I have been trying to discern such but I have never been able to find primary literature that will truly elucidate the problem.

I have eaten raw cannabis it does nothing. Delicious and spicy though! Good as a chew like tobacco snuff only spicy and cancer free.

THCV is tetrahydrocannabivarin. THC's boiling point is 157 degrees Celius according to Mcpartland, Russo. 2001. Cannabis and Cannabis Extracts: Greater Than the Sum of Their Parts? Journal of Cannabis Therapeutics. 1(3/4):103-132

Another good link I found when checking out some THCA structures that shows the process of decarboxylation: http://cannabis-science.com/cannabis_chemistry.html




[1] "Cannabinoids: Encyclopedia II"
There are over sixty known herbal cannabinoids. Of these, tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) are the most prevalent and have received the most study. Other common ones are listed below:

CBG Cannabigerol
CBC Cannabichromene
CBL Cannabicyclol
CBV Cannabivarol
THCV Tetrahydrocannabivarin
CBDV Cannabidivarin
CBCV Cannabichromevarin
CBGV Cannabigerovarin
CBGM Cannabigerol Monoethyl Ether


THC is the primary psychoactive component of the plant. Medically, it appears to moderate pain and to be neuroprotective. THC has a greater affinity for the CB1 receptor than for the CB2 receptors. Its effects are perceived to be more cerebral.

CBD is not psychoactive, and appears to moderate the euphoric effects of THC. It may decrease the rate of THC clearance from the body, perhaps by interfering with the metabolism of THC in the liver. Medically, it appears to relieve convulsion, inflammation, anxiety, and nausea. CBD has a greater affinity for the CB2 receptor than for the CB1 receptor. It is perceived to have more effect on the body.

CBN is the primary product of THC degradation, and there is usually little of it in a fresh plant. CBN content increases as THC degrades in storage, and with exposure to light and air. It is only mildly psychoactive, and is perceived to be sedative or stupefying.

These compounds may be in different forms depending on the position of the double bond in the alicyclic carbon ring. There is potential for confusion because there are different numbering systems used to describe the position of this double bond. Under the dibenzopyran numbering system widely used today, the major form of THC is called delta-9-THC, while the minor form is called delta-8-THC. Under the alternate terpene numbering system, these same compounds are called delta-1-THC and delta-6-THC, respectively.

Most herbal cannabinoid compounds are 21 carbon compounds. However, some do not follow this rule, primarily because of variation in the length of the side chain attached to the aromatic ring. In THC, CBD, and CBN, this side chain is a pentyl (5 carbon) chain. In the most common homologue, the pentyl chain is replaced with a propyl (3 carbon) chain. Cannabinoids with the propyl side chain are named using the suffix "varin", and are designated, for example, THCV, CBDV, or CBNV. It appears that shorter chains increase the intensity and decrease the duration of the activity of the chemicals.

Cannabinoids were first discovered in the 1940s, when CBD and CBN were identified. The structure of THC was first determined in 1964. Due to molecular similarity and ease of synthetic conversion, it was originally believed that CBD was a natural precursor to THC. However, it is now known that CBD and THC are produced independently in the cannabis plant. Cannabinoid production starts when an enzyme causes geranyl pyrophosphate and olivetolic acid to combine and form CBG. Next, CBG is independently converted to either CBD or CBC by two separate synthase enzymes. CBC is then enzymatically cyclized to THC. For the propyl homologues (THCV, CBDV and CBNV), there is a similar pathway that is based on CBGV.

Cannabis plants can exhibit wide variation in the quantity and type of cannabinoids they produce. The mixture of cannabinoids produced by a plant is known as the plant's cannabinoid profile. Selective breeding has been used to control the genetics of plants and modify the cannabinoid profile. For example, strains which are used as fiber (commonly called hemp), are bred such that they are low in psychoactive chemicals like THC. Strains used in medicine are often bred for high CBD content, and strains used for recreational purposes are usually bred for high THC content, or for a specific chemical balance. Some strains of more than 20% THC have been created.

Quantitative analysis of a plant's cannabinoid profile is usually determined by gas chromatography (GC), or more reliably by gas chromatography combined with mass spectrometry (GC/MS). Liquid chromatography (LC) techniques are also possible, although these are often only semi-quantitative or qualitative. There have been systematic attempts to monitor the cannabinoid profile of cannabis over time, but their accuracy is impeded by the illegal status of the plant in many countries.

Cannabinoids can be administered by smoking, vaporizing, oral ingestion, transdermal patch, intravenous injection, sublingual absorption, or rectal suppository. Once in the body, most cannabinoids are metabolized in the liver, although some is stored in fat. Delta-9-THC is metabolized to 11-hydroxy-delta-9-THC, which is then metabolized to 9-carboxy-THC. Some cannabis metabolites can be detected in the body after several weeks.

Cannabinoids can be separated from the plant by extraction with organic solvents. Hydrocarbons and alcohols are often used as solvents. However, these solvents are flammable and many are toxic. Supercritical solvent extraction with carbon dioxide is an alternative technique. Although this process requires high pressures, there is minimal risk of fire or toxicity, solvent removal is simple and efficient, and extract quality can be well-controlled. Once extracted, cannabinoid blends can be separated into individual components using wiped film vacuum distillation or other distillation techniques. However, to produce high purity cannabinoids, chemical synthesis or semisynthesis is generally required.

[guest]

BTW:

Here is a good microcentrifuge for $250.00, it is inexpensive but should suffice. I am unsure of its RPM but it should be fast enough, I'll call and find out. All told one could spend less than $600-800 for everything needed to process 1oz at a time, including the Tamisiume extractor:
http://www.bestlabdeals.com/Revolutionary_Science_Microcentrifuge_p/rev004.htm


Also, I was thinking about a DIY centrifuge. This may work, tho not as well as a real centrifuge:

Lay a bikecycel (minimum 21 gears for torque) on its side so one and still spin the pedals. Affix the vial of cold solution to the spokes, right next to the rim. Then shift to the lowest gear and start peddling with you arm. Try to keep a constant speed, and as fast as you can go. Keep it up for 10-15 minutes.

[guest]

Filter pore size:

I am trying to find the ideal micron size for filtering the extract from the ethanol solution. I don't want to go too big, or too small. For DNA work 0.2-0.8

[guest]

Terpenoids

I was worried that when boiling off the ethanol I would also boil off useful terpeniods and flavonoids. Then I found the great list below! When boiling off ethanol we use 78'C, way below the bp of terpenoids and flavonoids.

For illustrations and explanations of many of the chemicals (terpenoids, etc) see the Google scans of the book by E.Russo, "Cannabis Therapeutics in HIV/AIDS", p.112-114.

Fig. 1.: http://books.google.com/books?id=qUMQqa1PT4QC&pg=PA112&lpg=PA114&ots=fi_IxPahdq&dq=cannabis+terpenoid+boil+point

Fig. 2.: http://books.google.com/books?id=qUMQqa1PT4QC&pg=PA114&lpg=PA114&ots=fi_IxPahdq&dq=cannabis+terpenoid+boil+point



http://weed-forums.com/questions-beginner-help/5811-vaporizing-temps-cannabinoids-others.html

For those who choose to vaporize, here's a helpful little list.
Enjoy!


Phytocannabinoids, their boiling points, and properties:

?-9-tetrahydrocannabinol (THC)
Boiling point: 157*C / 314.6 degree Fahrenheit
Properties: Euphoriant, Analgesic, Antiinflammatory, Antioxidant, Antiemetic

cannabidiol (CBD)
Boiling point: 160-180*C / 320-356 degree Fahrenheit
Properties: Anxiolytic, Analgesic, Antipsychotic, Antiinflammatory, Antioxidant, Antispasmodic

Cannabinol (CBN)
Boiling point: 185*C / 365 degree Fahrenheit
Properties: Oxidation, breakdown, product, Sedative, Antibiotic

cannabichromene (CBC)
Boiling point: 220*C / 428 degree Fahrenheit
Properties: Antiinflammatory, Antibiotic, Antifungal

?-8-tetrahydrocannabinol (?-8-THC)
Boiling point: 175-178*C / 347-352.4 degree Fahrenheit
Properties: Resembles ?-9-THC, Less psychoactive, More stable Antiemetic

tetrahydrocannabivarin (THCV)
Boiling point: < 220*C / <428 degree Fahrenheit
Properties: Analgesic, Euphoriant





Terpenoid essential oils, their boiling points, and properties:

?-myrcene
Boiling point: 166-168*C / 330.8-334.4 degree Fahrenheit
Properties: Analgesic. Antiinflammatory, Antibiotic, Antimutagenic

?-caryophyllene
Boiling point: 119*C / 246.2 degree Fahrenheit
Properties: Antiinflammatory, Cytoprotective (gastric mucosa), Antimalarial

d-limonene
Boiling point: 177*C / 350.6 degree Fahrenheit
Properties: Cannabinoid agonist?, Immune potentiator, Antidepressant, Antimutagenic

linalool
Boiling point: 198*C / 388.4 degree Fahrenheit
Properties: Sedative, Antidepressant, Anxiolytic, Immune potentiator

pulegone
Boiling point: 224*C / 435.2 degree Fahrenheit
Properties: Memory booster?, AChE inhibitor, Sedative, Antipyretic

1,8-cineole (eucalyptol)
Boiling point: 176*C / 348.8 degree Fahrenheit
Properties: AChE inhibitor, Increases cerebral, blood flow, Stimulant, Antibiotic, Antiviral, Antiinflammatory, Antinociceptive

?-pinene
Boiling point: 156*C / 312.8 degree Fahrenheit
Properties: Antiinflammatory, Bronchodilator, Stimulant, Antibiotic, Antineoplastic, AChE inhibitor

?-terpineol
Boiling point: 217-218*C / 422.6-424.4 degree Fahrenheit
Properties: Sedative, Antibiotic, AChE inhibitor, Antioxidant, Antimalarial

terpineol-4-ol
Boiling point: 209*C / 408.2 degree Fahrenheit
Properties: AChE inhibitor. Antibiotic

p-cymene
Boiling point: 177*C / 350.6 degree Fahrenheit
Properties: Antibiotic, Anticandidal, AChE inhibitor

borneol
Boiling point: 210*C / 410 degree Fahrenheit
Properties: Antibiotic, ?-3-carene 0.004% 168 Antiinflammatory

?-3-carene
Boiling point: 168*C / 334.4 degree Fahrenheit
Properties: Antiinflammatory





Flavonoid and phytosterol components, their boiling points, and properties:

apigenin
Boiling point: 178*C / 352.4 degree Fahrenheit
Properties: Anxiolytic, Antiinflammatory, Estrogenic

quercetin
Boiling point: 250*C / 482 degree Fahrenheit
Properties: Antioxidant, Antimutagenic, Antiviral, Antineoplastic

cannflavin A
Boiling point: 182*C / 359.6 degree Fahrenheit
Properties: COX inhibitor, LO inhibitor

?-sitosterol
Boiling point: 134*C / 273.2 degree Fahrenheit
Properties: Antiinflammatory, 5-?-reductase, inhibitor

[guest]

Hey GS,

Sorry about not providing a citation for that quote by "gordonlui"[1] regarding the matrix holding solution molecules and even a vaccum won't help. It is from the same thread I linked to where Sam had a lot to say. Here ya go:

Thread: "Making Honey Oil Like A Pro, by Master Thai"
By "gordonliu"
http://www.icmag.com/ic/showthread.php?t=39661&page=9
[1]

"making honey oil like a pro"

my question is, are you referring to isomerization, acetylation, or a simple extraction

there are ways to produce a high purity (>95%) extract on a large scale, but they go beyond simple extractions and generally require laboratory glass (more than a sep funnel).


also, i must maintain this:


it is extremely difficult to obtain the solvents necessary to do much of this chemistry in a purity high enough for consumption


lab grade is very far below hplc, and i hesitate to use hplc (depending on the solvent)

it is essentially impossible to obtain pharmaceutical grade solvents (even in a university research setting) outside of industry.


also, electric stoves or any conceivable CMEMORY incarnation of such a device is extremely dangerous when used with flammable solvents.

in a lab, all electronics utilized inside of a hood or on a benchtop are SPARK FREE!!

lastly, because it is impossible to remove 100% of the solvent used in these extractions under any circumstance, i just want you guys to know that even heating for days on end is not going to remove all of the solvent.

you need a small sample quantity (so that the solvent molecules are not too deeply embedded in a matrix) and a high vacuum pump.

even after a day at .02 mm hg, a sample will still contain traces of solvents boiling at 60 or above





I wanted to get a better idea of gordonliu's knowledge. Below are the only relevent google search which turned up. This person seems legit, and seems to agree that one can make a solvent and impurity free extract with ethanol. I am using ethanol as the second solvent...

Thread: "hexane oil"
By: gordonlui
Weedtracker: http://www.weedtracker.com/forums/concentrates-186/hexane-oil-1964.html

re: hexane oil

hexane, butane, iso, etc. all solvent extractions that use toxic chemicals are bad because there is absolutely no way to remove all the solvent from the extract. not even a rotoevap with an insane vacuum and moderate heat will remove the solvent molecules. only ethyl alcohol extractions or scf extractions will be totally safe and non-toxic. (that last extraction technique has yet to truely make its way into the cannabis community although some people will disagree and say their chemist friend made them some, although that is extremely unlikely)

no one should be afraid of mercaptins from butane extractions, especially from clinics, because proper butane oil is made with clean butane. you can even get the msds from the manufacturer. i use king butane and it contains something like 96% n butane and 3.5 percent iso butane and .5 percent hexane.




Thread: "how do you make your oil"
By: gordonlui
Forum: https://www.icmag.com/ic/showthread.php?t=85437


Here she/he states one can not isomerize cannabinoids into other cannabinoids. He is specifically referring to the myth/bad choice of using acid to isomerize THC into THC acetate. However, this could apply to isomerizing CBD to THC with heat, it could be out dated info, I'll look into it, unless anyone knows?

by some person:
Cannabis ALchemy bt D.gold is the best book on th esubject

you can convert cannabinoids into THC if you knwo the correct process

rotate the THC molecule its 10x more potent when eaten

learn to make THC acetate

By godonlui:

haha. every time i read that (book) I laugh. first of all, you cant isomerize any of these other cannabinoids to THC. sorry. doesnt work. you are 1 methyl group short. no matter what bonds rearrange, you will never get a new methyl group.

secondly, refluxing THC in alcohol with acid, even in catalytic acid, will completely change the molecule.

not only will you not change anything else into THC, but you will also change THC into another molecule that will have different affects.


THE ONLY ONE OF THESE HIPPY CHEMISTRY EXPERIMENTS THAT HAS ANY POSSIBLE UPSIDE IS ACETYLATION OF THC.

acetylation is the same process that is performed to convert morphine into heroine. acetylated natural products are more non-polar, and travel through blood-brain barrier more efficiently (IE: they go into the brain before most of the molecules are metabolized by the body)

[guest]

Hey c,

Yea we all agree about co2, now who will win the lottery and buy us each one? ;)

What I am trying to do is develope a simple and relativley inexpensive method any stoner can follow; all while providing a pure extract (no impurities) with lots of terpenoids and flavonoids. AFAIK, this method should provide the absolutly best extract one can produce (short of Co2 (which often lacks non-cannabinoids)).

I hope I have it nearly figured out already, but like GS said, gotta test. I'm sure I might change something(s), but I am pretty sure this method will work and leave zero impurities:


Ideally process all cannabis and extracts under yellow light.


Dry cannabis using a line or a food dehydrator (low temp), or probably most ideally would be a vacuum desiccator utilizing carbon dioxide or nitrogen, not oxygen, in a cooler or at room temperature. Reduce cannabis to about <5% moisture content. Lightly break up buds.


Pretreat raw dried cannabis with alkaline water bath (pH >10 with sodium hydroxide) for 30-60 minutes (I'm not sure if the time is correct). Wash a few times with clean water.

This will decarboxylate 2-carboxylic acids (2-COOH) to their respective cannabinoids (ex. THC-COOH > THC). It will also decarboxylate THC-A into THC and is supposed to extract chlorophyll from cannabis.


Place filtered and washed cannabis in double the volume of water and bring to simmer for two hours.

This will isomer CBD into THC and decarboxylate THC-A into THC. One can see a large increase of THC from THC-A; there is generally very little CBD in today's cannabis.


Filter cannabis and dry as before.


Use Tamisiume extractor, or other pressurized and high quality n-butane extraction apparatus. (Or other solvent(s))


Dissolve BHO extract with pure food grade ~94% ethanol (Everclear), only a little is needed. Warm ethanol to facilitate dissolving BHO. Using a shaking/vibration apparatus can be helpful, like a ultrasonic bath, tube vibrator, etc.


Place solution in freezer (-18'C; 0'F) for 12-24 hours. This precipitates impurities like hydrocarbons (butane, propane, hexane, etc).


Remove and place vials in microcentrifuge. Centrifuge for 5-15 minutes at ~11400 xg. This precipitates impurities like hydrocarbons (butane, propane, hexane, etc).


Filter out extract (was BHO) with Whatman filter paper "Grade 5V"; 2.5 micron pore size. Filters are easy to get at Ebay and Amazon. Aspirating the solution (and precipitates) may be a wise before filtering the extract from solution.


Evaporate ethanol and water azeotrope from extract using a non-sparking (no metal on metal) hot plate under a glass wide mouth vial affixed with a vacuum apparatus. Set the hot plate to 79'C, or ~175'F and vacuum as near to 0.01mm hg as possible; for 1-6 hours until purged (not sure about purging time). If doing this in an enclosed room a fume hood, or other ventilation should be used.


(Optional) Whip pure extract into budder. after extract has been warmed into semi-liquid state before re-solidifying.


Enjoy!

[guest]

Hmmm,

I made typo, I forgot THC-A is THC-COOH (or would that be THCA-A?; I have to check my notes), so my directions may seem a bit silly and redundant. I'll fix it now.

It seems the decarboxylation temperature of THC-A (aka THC-COOH) is 50'C (122'F)[1] OR 100'C (212'F)[2] OR 106'C (220'F)[2], thus to decarboxylate it into THC one might not need to simmer the water, less heat is preferable. The problem I have with the conflicting figures is they came from the same (suspect) source! (E.Rosenthall-WTF?)

Because I don't trust E.Rosenthall I will continue to look for authoritative info on the temperature conversion of THC-A into THC.

Because THC-A and other cannabinoid 2-COOH acids decarboxylate in the alkaline wash, the warm water bath could probably be shortened to an hour. Using two different methods should increase the % of decarboxylation.

According to the following study the method one uses to decarboxylate THC-A into THC is important. Proper methods can read a maximal of 70% THC-A into THC; verses only a 30% 9onversion of less ideal methods (ex. smoking!!-wow). I will get this paper today and try to copy their method, or McGuyver their method...

"Isolation of ?9-THCA-A from hemp and analytical aspects concerning the determination of ?9-THC in cannabis products"
author(s): Franz E. Dussy?, ?, Cornelia Hamberg, Marco Luginb

[outdoordreams]

Gojo empty your mail box dude!

I heard Ed Rosenthall is definitely not the guy to listen too. (no offense ED)

[guest]

Hey bro,

Will do! Gimme 5 minutes.

Yea its too bad that E.Rosenthal, G.Cervaties, etc, are "gurus".

[guest]

I'm way excited!

This little project of mine is turning out quite well and cheaply! All told, not including the fume hood and extraction apparatus (ie. Tamisiume Extractor http://www.tamisiumextractors.com ), the cost of tools needed for my working method is around ~$200-500, depending if new or used.



This post will detail how to set up a vacuum apparatus in the form of a $20.00 aspirator (using water as the "working liquid") and a heating apparatus (hot plate and crock pot) to effectively, quickly, safely and completely boil off all ethanol on the cheap!


The most expensive tools one would need to buy are a microcentrifuge (new $250+; used $100+), lab quality hot plate (new $100+; used $50+), aspirator with pump and parts ($100-150), lab stands with clamps, vacuum tubing, nipple lid, wide mouth glass vial, crock pot, etc ($50+) and [optionally] a fume hood (new $600+; DIY $100-200).

All told (not incl. fume hood):
new ~$500+ and used ~$300+

One could buy a $400-800 Tamisium Extractor, with another $300-600 (or $600-800 w/DIY fume hood) in used/new equipment, tools, solvents, glassware, stands, etc.

Thus, for about $800-1,500 one can create extracts as pure (theoretically) as that from a $20-30K Co2 super critical extraction apparatus! And anyone can do it, no chemist background required. Also, this extract should be loaded with many different terpenoids and flavonoids!


I was in error before when I wrote the partial vacuum should be as close to 0.01 mm hg as possible (see below). That is good news because to create that hard of a partial vacuum is very expensive. In fact, one can fully remove all ethanol with as low as 20 mm hg*. IIRC normal air pressure is ~760 mm hg.

A good point about boiling off ethanol is the bp is low enough to negate the need for a lesser partial vacuum (eg. rotovap) to lower the bp. That is, one can easily heat a water bath to the normal air pressure bp of ~94% ethanol which is 79'C (175'F).




Below I will describe how to setup an aspirator using water as the "working liquid", and how to setup a heat source to boil off ethanol.


In my next post I will describe how to build a fume hood for doing extractions in enclosed spaces.



...............



So, you ask, just what does a water aspirator do?



*"How Not To Do It: Water Aspirators"
By: Derek Lowe
http://pipeline.corante.com/archives/2008/08/25/how_not_to_do_it_water_aspirators.php

[snip]
The low-tech way to get the sort of pull-it-though vacuum you need for these things is a water aspirator. You don’t see these as much any more, and you don’t see them at all in industry, since they necessarily pull solvent vapors into the water stream. But they work. An aspirator is basically a narrowing tube that hooks up to a hard-spraying water tap and has a sidearm fitting. The accelerating blast of water pulls the air in the tube along with it as it goes, creating a useful vacuum. If you wanted to make one rather more environmentally friendly, you’d keep a well-stocked dry ice condenser in line with it to trap out the solvent vapors before they go down the drain (which is what your rota-vap should have on it, anyway), but even with that, you’re always going to be turning the water flow into a waste stream. As I say, you don’t see them as much these days.





How do I use an aspirator with water as the working liquid?


Using a 'water aspirator' with volatile solvents like ethanol without a water trap is a no-no. Mainly because most systems are run to waste, the one I am presenting is not run to waste. The amount of ethanol being removed is very minimal and thus proper disposal of waste water is easy.

There is no need for constant flow of fresh water as suggested by J.B.Nimble. My method only uses the aspirator for 2-4 hours max at any one time. Thus, one 5 gallon bucket of ice cold water should suffice for 2-4 hours. One can also add frozen ice packs to keep water temperature low. Water temperature of a mere <25'C (80'F) must be maintained, that temperature should not be hard to maintain for a few short hours.

Because my setup uses no run to waste, or overflow, all contaminated water (with ethanol) is still within the 5 gallon bucket. One simply disposes the water according to local environmental regulations.



This is my current thinking:


Setup a hot plate and put a crock pot full of water on the burner. Heat water to 79'C (175'F).


Place stand next to crock pot and set clamps so they hold the glass test tube and the aspirator. The water level outside the glass should be above the level of solution.


Attach aspirator to stand with clamps and setup the rest of the aspirator system.


Remove the glass test tube with solution from the microcentrifuge. Then filter the precipitates (hydrocarbon, etc) from the solution (ethanol and extract). Pour the solution into the filter and collect the filtered solution in a glass test tube which will fit into the stand clamps. Safely dispose of the filter (with precipitate) according to local environmental regulations.


Attach test tube to stand with clamps so the test tube is in the water. Make sure the water level is above the solution level.


Attach the vacuum tubing to nipple on test tube and turn on the water pump. Run aspirator system for 2-4 hours depending upon amount of solution.


Once extract is fully purged unplug water pump, allow pressure and water to drain. Then one could whip the extract into 'budder.' while it is pliable; or leave it be. Either way, set test tube aside and allow to cool and harden.


Once the extract has hardens cover the test tube with a piece of cloth and use a pair of pliers to crush the glass. Apply pressure at the location of the extract. Separate out the glass and collect the extract.


Enjoy!






OK, OK, you sold me, how do I setup a water aspirator?



Here is my suggestion, I got the idea from Jack B. Nimble's work (see below):

Read the picture for important context and information about what water pump and aspirator to buy. The full size picture is hosted at imageshak, all rights reserved)
http://img121.imageshack.us/img121/5059/aspiratorsetup.th.jpg (http://img121.imageshack.us/i/aspiratorsetup.jpg/)





"The Construction and Operation of Clandestine Drug Laboratories", 2nd Ed
by Jack B. Nimble
HTML by Rhodium

"Aspirator Vacuum Station"
http://www.erowid.org/archive/rhodium/chemistry/equipment/aspirator.html
I think an aspirator pump should be the main vacuum source in a clandestine laboratory. To save water, or if your water pressure is low, you can construct a recirculating pumping station. This station has been completely redesigned since the first edition, and this units performance is truly outstanding. Details of this pump are shown below.

You'll still need a source of running water to keep the unit cool and flush out condensed solvents as the unit runs. It works quite well, however, and the pump can provide a higher pressure than most any municipal water supply. Use a 5 gallon can, plastic pail, or something similar to house the system. The overflow should have a fitting allowing the attachment of a one-inch or larger drain hose or the unit can be placed in a sink or bathtub. The pump is of the jet pump-type variety, and should be in the range of 1/3 to 1/2 horsepower. Units made for hot tubs and small swimming pools are also satisfactory; just be sure to check the rated pressure. The pump should provide a pressure of at least 20 psi, but 30 to 40 is much better. Their pressure is usually rated in "feet of head". Multiply feet of head by 0.4335 to convert to psi. The use of submersible pumps is not recommended as they raise the temperature of the water, and quickly reduce the vacuum. One pump can usually power two aspirators. The intakes to these aspirators can be connected with a tee for increased pumping speed, or they can be used independently. Increased pumping speed is especially needed when evaporating large quantities of volatile material. As with all aspirator pumps, the colder the water, the higher the vacuum. Adding ice to the reservoir greatly increases the vacuum.

This unit will outperform most any municipal water supply. With 30 psi, it approaches the vacuum of many mechanical pumps. It can handle solvents and other corrosive vapors easily. It can also function out in the country where water pressure is low or otherwise unreliable. The pail should not seal up air-tight. Leave a small space around the aspirator outlet to allow air to enter. The unit will not drain properly without an air inlet.

The baffle is important. It keeps bubbly, aerated water from being sucked up by the pump, which otherwise seriously would affect performance. Use one half of a lid to the can as baffle, and secure it permanently with silicone.





Good Resources:

Chemistry link-o-rama, you WILL learn a lot for this great page, or you already a chemist:
http://www.erowid.org/archive/rhodium/chemistry/index.html


CU at Boulder, Organic Chem:
http://orgchem.colorado.edu/hndbksupport/vacsys/vacsys.html

[guest]

Use a fume hood or other ventilation for indoor work


It is important to use a fume hood or work in a well ventilated area when using n-butane or other volatile chemicals.

Uses:
A fume hood would be used for the extraction apparatus to remove gas.

A water aspirator would be used for boiling off the ethanol to remove gas (and lower pressure).

Its not hard to build a portable fume hood using plexiglass and a little math.

The fume hood will have to be large enough so the extraction apparatus can fit inside.

I will do a pictorial how to when I build one, but here's the dirty:

Build a three sided box, say 3'x2'x2' (LxWxH), although a truncated triangular footprint might provide better air velocity[1]. Attach a removable 'front' piece of plexiglass with an opening of around 2 feet (enough room to comfortably work). Build an upward sloping 'roof' (like a house's roof). At the center of the roof attach a squall cage fan or in-line fan which can provide a "face velocity" of 90-100 ft/min. If one can't reach a minimum of 80 ft/min than decrease or increase the size of the opening accordingly. Attach a 4" plastic drier hose to the fan and vent it outside.

That's it. Now when extracting with n-butane do so within the fume hood.

SEE:
"Design for a Miniature Portable Fume Hood"
By: R.A. Bailey & S.C. Wait, Jr.
J. Chem. Educ. 76(2), 228-229 (1999)
HTML by Rhodium
http://www.erowid.org/archive/rhodium/chemistry/equipment/portable.fume.hood.html

[guest]

Edit:


If one is boiling off more than a little ethanol solution one may have to setup a run to reservoir system. The problem is gas absorption (by water) will be reduced as the water becomes more infused with the ethanol as gas. Or instead of running to reservoir, one could scoop out water and then simply replace it with cold water.


To maximize vacuum try to limit the infusion of air into the water. Bubbles and air in the vacuum tubes will reduce ethanol gas absorption by the water. The colder the water the more oxygen it will hold and the greater the vaccum.


It might be wise to use filter paper with a pore size under 2.5 microns. There are filter papers with pore size of <2 micron. Or one could use a glass microfibre filter of under 1 micron (ex. 0.25 micron).

Last time I posted about filter pore size I implied one disposes of the filtrate (ethanol/extract solution). That was unintentional, lack of proof reading, sorry. The hydrocarbon precipitates will be filtered out of the solution and remain on the filter.

[TheForSaken]

...

[guest]

Hey,

Haha, that hood sounds way DIY, thanks.

Good idea about the used source, but to ensure a partial vacuum of under 20 mm hg the specific pump and aspirator I mentioned (in the picture) should be used (by newbs at least). The aspirator I suggest is inexpensive but good, it's the Nalgene aspirator.

In the limited studies I have found 20 mm hg was commonly used to evaporate EtOAc from a DNA solution. The specific tools I suggest will reach <15 mm hg, more likely <10-12 mm hg.

Using other pump sizes or aspirators would work but one would not have a good idea of the actual partial vacuum. Better safe than sorry IMO. And the Nalgene aspirator is cheap.


Water boils at room temp here


Did I make a typo? Or explain something poorly?



BTW,

What do you think about using the aspirator?

Would you change what I am suggesting in any way?

Do you have any thoughts or suggestions or correction?


Thanks bro


Check out this thread:

"Advice on Pond Pump for aspirator setup?"
http://www.sciencemadness.org/talk/viewthread.php?tid=4128

[Lungus]

Did I make a typo? Or explain something poorly?
I believe he was alluding to his rig being able to produce enough vacuum to boil water at room temp.

[guest]

Hey bro,

How ya been? Long time no see. If you are correct that's great. Do you have a chemistry background? Any suggestions or corrections for me?

Thanks

[guest]

Hmmm,

I am going to research the bp temperature EtOAc when under partial vacuum of 10-20 mm hg. It would be good to lower the hot water bath temperature to retain some terpenoids and favonoids that would otherwise be boiled off.




TheForSaken,

Do you know the partial vacuum of your aspirator setup?

[TheForSaken]

Hey gojo,
This link may be of interest to you, about converting a fridge compressor into a vacuum...
http://www.paragoncode.com/shop/vacuum_pump/

And this link, shows a nomograph.
Scroll down to "The pressure-Temperature Nomograph"
http://www.erowid.org/archive/rhodium/chemistry/equipment/distillation4dummies.html
You may already be educated in this not sure. If not, hope this helps.
Regards
TFS

[guest]

Hey TFS,

Great point about the in-line pressure gauge. I didn't even think about it. Thanks a lot. I still have a lot to learn.

That is a very slick vacuum setup. And so inexpensive. Great link for sure. I would prefer to use oxygen as working gas and not water as working liquid, better vacuum AFAIK.

That second erwod link is very good. I have read it before but I didn't remember the part you cited, thanks. That will indeed be very useful.


Thank you very much, I appreciate any info or thoughts you would like to share.

I am really looking forward to testing this setup. This setup should totally change peoples view on non-co2 SC extracts. It puts big pharma quality medical cannabis extracts in the hands of patients as DIY...well, IMO even better than big (boring) pharma of 50/50 (THC/CBD). I hope clubs will be willing to sell extracts such as this if proven via GC/MS to be solvent free.

I am going to work up a detailed parts list and location for purchase. But not for a few days or more.

Good times. All the best, gojo

[guest]

(OK, here is a big post, but full of good and new info (to this thread), please read it all)



Kwool!

I found a few on-line calculation tools which compute the bp of ethanol at any given mm Hg or mbar. This means with a partial vacuum of 20 mm hg (26.7 mbar) the bp of ethanol azeotrope is 2.2'C (35.6'F). However, that's not good news because it means the bp of flavonoids, terpenoids and cannabinoids has also decreased. And considering how far 2.2'C is from average indoor temperature (20-25'C) one can assume many terpenoids, flavonoids, etc will be boiled off with a vacuum of 20 mm Hg at room temperature. Thus, I looked into raising the partial vacuum to match room temperature. (See below)

"Boiling Point Calculator for Ethanol and Water"
www.partyman.se/boiling-point-calculator/


I found a great patent which essentially is doing what I am suggesting. In the patent one is dissolving a pharmaceutical chemical in DMSO and then dissolving the DMSO compound into ~95% ethanol. The ethanol solution is then purged (of the DMSO and ethanol) under vacuum. This is proven effective to remove all solvents and suitable for pharmaceutical grade drugs, even intravenous drugs. This is great news for my project considering the amount of butane is very minimal after filtering out the precipitates of hydrocarbon, plant waxes, etc. Thus, my method should definitely work considering the level of DMSO in the patent is much more than the amount of butane in high quality BHO.


In this project one would replace the DMSO (from patent) with BHO (which is not a high bp solvent), and the ethanol will still be the "co-solvent" (which has a higher bp than butane). In my method I am using ~95% ethanol azeotrope as the co-solvent because it has a greater density than butane, thus when ethanol vaporizes it carries any remaining (un-vaporized) butane with it. However, because the bp of butane is the lower of the two the butane will start to vaporize before the ethanol.

When redissovling BHO into ethanol a ratio (by weight) of 1:3 to 1:10 should suffice. The solution should not be viscous, it needs to be fluid so it can be filtered efficiently. The less ethanol one uses the better as it means there will be less ethanol to boil off.


..........................


After reading the posts by TFS (thanks bro) I revamped my design a little.

I was reading the specs on the Nalgene aspirator and it seems the ultimate vacuum is only 723.9 mm Hg, not enough partial vacuum for my purposes. However, I did find another great option.



Aspirator:
(Find on Ebay, etc)

"Water-jet" aspirator pump with pressure gauge. The ultimate vacuum is 25 mm Hg at 20'C water temperature.
www.sigmaaldrich.com/catalog/ProductDetail.do?N4=Z162124%7CALDRICH&N5=SEARCH_CONCAT_PNO%7CBRAND_KEY&F=SPEC


Nalgene vacuum plate:

This is used to seal the vacuum chamber and connects to the aspirator via. 1/4" I.D. Vacuum tubing.
Nalgene model #5306-0130
www.nalgenelabware.com/products/productDetail.asp?product_id=222&subcategory_id=168&category_id=168&brand_name=Labware&category_name=Vacuum+Equipment&subcategory_name=


Glass vacuum chamber:

Bell wide mouth jars are preferred, a mouth diameter of 12.5 inches might be wise to facilitate the scraping/removal of purged extract from bottom of jar. Get the model with plain top and plain bottom:
www.hyvac.com/Products/Systems/Bell_jar_specs.htm


Microcentrifuge:

These can get pricey, but the "Revolutionary Science Micro
Centrifuge RS-102" is only $250. However, it only accepts centrifuge tubes of 2ml, not large, but it does accept 4 tubes at time. Reaches 10,000 RPM.

Model #500327
www.balkowitsch.amazonwebstore.com/Revolutionary-Science-Micro-Centrifuge/M/B000X2FR5I.htm

Full detail:
www.revsci.com/pdescription/405/


Microcentrifuge filter tubes:
(Find on Ebay or Amazon)

Microcentrifuge filter tubes are great! The filter I am thinking about has a pore size of 0.2 microns, thus any precipitate should be filtered out. There are two compartments in the tube: a filtrate compartment where the filtered solution collects and the top filter compartment where the precipitates collect. This is good as filtration under centrifuge is far superior, and faster, than simply pour the solution into filter paper.

"VectaSpin Micro" Sigma model #6832-0401, holds 1.25 ml of solution:
www.sigmaaldrich.com/catalog/ProductDetail.do?N4=Z338591|SIGMA&N5=SEARCH_CONCAT_PNO|BRAND_KEY&F=SPEC&lang=en_US%3E


Water Pump:

Little Giant is good, get these specs: 1/3-1/2 HP, 35-40+ psi, 2+ GPM. Important, make sure the pump as a flow rate control so one can lower the GPM (for example), thus increasing pressure to achieve the proper partial vacuum. If the pump has no flow control add a valve in line on the inlet vacuum tube before it reaches the aspirator, then adjust the valve to adjust the partial vacuum.


.................


Temperature and Partial Vacuum:

As I mentioned, 20 mm Hg is probably to low for high quality extract at room temperature. However, the good thing about a partial vacuum is it can negate the need for a hot plate and crock pot.

My goal is to provide just enough of a partial vacuum so the bp of ethanol is within normal home temperatures. Thus, one won't need heat, and the boiling off of terpenoids and flavonoids will be reduced.

I am assuming most homes have an average temperature of 20'C (68'F) to 25'C (80'F), thus, at sea level the partial vacuum range of ethanol is 55 mm Hg (73.3 mbar) to 70 mm Hg (93.3 mbar). That partial vacuum range puts the bp of ethanol between the temperature 20-25'C (room temp).

To achieve 55-70 mm Hg one needs to adjust the flow rate from the pump. The pressure gauge on the aspirator can be used to insure proper partial vacuum.

The nice thing about knowing the partial vacuum one needs to achieve is one can adjust the figures for higher elevations which changes the bp when under partial vacuum (verses bp under partial vacuum at sea level).


.................


The following quotes offer more evidence that the method I suggest might be totally free from hydrocarbons!

"METHOD FOR REMOVING HIGH BOILING SOLVENTS FROM DRUG FORMULATIONS BY VACUUM DRYING"
http://www.freepatentsonline.com/EP0971701.html

The present invention is particularly useful in preparing or formulating drugs which exhibit excellent pharmaceutical activity but are extremely difficult to recover from the high boiling solvent
medium in which they are synthesized or manufactured. The drugs dissolved in the high boiling solvents generally are not acceptable as injectable formulations because of the toxicity or other objectional characteristics of the high boiling solvent medium.




Here is information on how the redissovling of BHO into ethanol removes the residual butane. In this quote the BHO would be the high bp solvent (even though its not) and the ethanol is the "co-solvent" which has a lower bp (even though it's bp is higher than butane):



A technique has now been devised wherein a high boiling solvent can be removed from a drug compound dissolved in the high boiling solvent by vacuum drying in the presence of a low boiling co-solvent to levels below the detection limits of the high boiling solvent and low boiling co-solvent. While the method of removal of the high boiling solvent is not entirely understood, it is believed that the low boiling co-solvent augments the mass transfer rate of the high boiling solvent. It is also likely that there is some hydrogen bonding between
the high boiling solvent and the low boiling co-solvent, which in turn leads to a volatilizing effect. The method foes not depend on the formation of an azeotrope.

...And...

While the manner in which the addition of the low boiling co-solvent enables removal of the high boiling solvent is not entirely clear, it is clear that the solvent and co-solvent do not necessarily form an azeotrope. Rather, the evaporation of the co-solvent appears to transport the high boiling solvent out of the solution.

Because of its effectiveness as a high boiling solvent/low boiling co-solvent mixture towards a large number of pharmaceutical compounds, the combined use of dimethyl sulfoxide/ethanol is preferred.

The process of this invention is particularly useful in the preparation
of injectable pharmaceutical formulations, e.g., anti-neoplastic
agents which were previously impossible to formulate because of their extreme instability in common injectable vehicles. Examples of such drugs include carmustine, (BCNU), PCNU, lomustine, Taxol, camptothecins, anthracyclines, etoposide, bizelesins and carzelesin to
name a few.


Cheers

(Next up, proper temperature of decarboxylation of THC-A into THC)

[guest]

Does anyone know the FDA maximum detection limit for ethanol in pharmaceutical compounds for human medicine?

I would like to know the limit, even though I still think there will be less than trace amounts ethanol left in the extract. Ethanol is non-hazardous but I'd still like to know the FDA stance on it. I ask because in the patent in my previous post it seems implied that there could be an amount of ethanol left in the pharmaceutical compound which would be below legal detection limits.


FWIW, here are the detection limits for raw cannabis as medicine as required by Health Canada:
https://www.icmag.com/ic/showpiece?p=2210236&postcount=261






And here's some info on using propane as the solvent vs co2 SCE vs butane. Like I've said before, propane might be more ideal than butane for my purposes. I think I will make two different extraction, one using butane and the other using propane...

I really like that propane is supposed to leave no toxins in the extract. And when used with ethanol as the co-solvent both solvents are toxin free, organic solvents.
:)

www.edenlabs.org/supercritical_extraction.html

Propane-
There is a little known school of thought in the natural products industry which believes that propane is the ultimate solvent for extracting botanicals. Eden Labs has tested this theory thoroughly
and we have come to the conclusion that there is something to it. Although propane cannot be as widely manipulated through temp and pressure as CO2, it produces very similar results, sometimes
better. It has an amazingly small loading ratio 1-4 volumes and it can be recovered quickly. This means much faster production times. It leaves no toxic residues and it is an all natural, organic solvent. The material data safety sheet, MSDS, says it is harmless except for the fact that is flammable. Because it works at relatively low pressures, 80-150 psi, the technology costs much less than a full supercritical
CO2 system and can be very competitive in terms of quality and speed of production.

The downsides to propane is that it is highly flammable so precautions such as sparkless rooms with powerful ventilation are a must. The fact that is is not widely understood or accepted can also be an issue.


Butane/IsoButane-

In some cases where propane doesn't do the job, butane works better. It has all the pros and cons of propane and requires identical equipment for utilization.

[guest]

OK, wtf?

What is the current proper spelling of the following words? I have seen them spelled two different ways each. All from scholarly journals:

COOCH or COOH ?

THC-A or THCA-A ?


Also, I just spent the last 2 hours figuring out the real deal with decarboxylation. And guess what? It seems we should NOT be using heat to decarboxylate cannabinoid acids. We should probably be using alkaline bath only. I will post the info soon, I gotta go get a coffee! I have four full text papers from whence I get my info. I will upload all four papers here.

...Its really pisses me off as I learn how much BS we have been fed by the so-called cannabis gurus like Rosentahll, Cervanties, etc, they all tell us to use heat for decarboxylation and lumes or watts or PAR for light measurement, WTF?

[c-ray]

or enzymes, like decarboxylase for instance
you are right about heat though, it drives off the terpenes and that is a travesty, we want to preserve as much of the terpenes as possible

[d'artanian]

COOH = Carboxyl

[d'artanian]

THC-A = Tetrahydrocannabinolic acid
THCA-A and THCA-B :The structural difference between the two isomers is a carboxyl group at C-2 or C-4

[guest]

Hey gerber,

Thanks bro. Are you saying the correct spelling of COOCH is COOH? Then do you know what COOCH is? (Forgive the questions, I could look it up but I was already at the library once today and now I'm being lazy)

OK, so THCA-A is THC-A-2-COOH? (Or similar?)

Thank you

[guest]

Hey C,

Let me clarify, too much heat is not wise. A little heat IMO should not be too much cause for concern. See below.

That's an interesting point about enzymes. Do you know that they will decarboxylate cannabinoids acids? I have only read about using heat or alkaline solutions.

Good point about the terpenes, however, many (most?) have a high bp and many will not boil off at lower temperatures, for example, below 200'F. The main reason I believe too much heat is not wise is due to the amount of THC-A lost to vaporization before it has a chance to become THC. Cannabinoid acids have lower bp. The losses are quite dramatic, and I was quite surprised at what I found...

If one does want to use heat one should not exceed 122'C (251.6'F). Below 122'C and the resulting cannabinoid (THC and CBD) level increases (even after heating for 50 minutes). While from 122'C to 145'C (293'F) the resulting cannabinoid level is decreased from that of 122'C. The decrease is due to evaporation (boiling off) of cannabinoid acids.[1]. (Note that these figures where not necessarily attained from water as the solvent; using a closed glass reactor, but they are still applicable as a range. It would seem in an open reactor the bp would be higher...)

In a paper (I need to read) by Turner and Mahlberg [2] they used 37'C (98.6'F) and 60'C (140'F) for several hours in an open reactor. This is good because both 37'C and 60'C are low, I assume few terpenes will boil off at 98.6'F.

....
I think I may use a warm water alkaline bath at 38'C (100'F) for two or three hours.

With that method most of the THC-A and THCA-A [3] should decarboxylate directly into THC.
....

Due to C-Rays good point about boiling off terpenes (and flavonoids) at lower temperatures it seems not using too much heat is wise, as stated above. Instead one can use water bath with NaOH to bring the water pH to =>10. IIRC, this bath is also supposed to ismorize CBD to THC. It also removes chlorophyll from raw cannabis.

I spent two hours in the biology library today trying to figure this out. It seems I succeeded, I hope, and that's annoying me. If I found the answers in two hours why did not the book gurus do their due diligence? Douche bags...

Here is a winzipped folder of 6 journal articles. Some are not exactly on topic, but close so I thought some of you might be interested:
www.filedropper.com/decarboxylate


"Determination of cannabinoid acids by HPLC of their neutral derivatives formed by thermal decarboxylation"
Author(s): T. Veress, J. I. Szanto and L. Leisztner

CONCLUSION

When preforming the thermal decarboxylation of cannabinoid acids in either the presence or absense of organic solvents in an open reactor, an optimum temperature at which the volocity of the decarboxylation would be high enough and simultaneous evaporation of neutal cannabinoids would not occur could not be found. Consequently, it is not possible in this manner to obtain an amount of neutral cannabinoids equivalent to that of the cannabinoid acids from which they were decarboxylated. ...



Info about decarboxylation with alkaline solutions:


"Natural cannabinoids: Templates for drug discovery"
Author(s): Ganesh A. Thakur, Richard I. Duclos, Jr. And Alexandros Makriyannis

Classical cannabinoids (CCs) are ABC tricyclic terpenoid compounds bearing a benzopyran moiety (Fig. 2) and are insoluble in water but soluble in lipids, alcohols, and other non-polar organic solvents. These phenolic derivatives are more water soluble [AFAIK that's good] as their phenolate salts formed under strong alkaline conditions


"Structure-Activity Relationships of the Cannabinoids: An Overview"
Author(s): Raj K. Razdan, Ph.D


In an earlt SAR study, Edery et al. (1971) postulated the need for a free phenol for cannabinoid activity.



[1] "Determination of cannabinoid acids by HPLC of their neutral derivatives formed by thermal decarboxylation"
Author(s): T. Veress, J. I. Szanto and L. Leisztner

[2] J. C. Turner and P. G. Mahlberg, Journal of chromatograhy, 171 (1979) 504.

[3] "Isolation of THCA-A from hemp and analytical aspects concerning the determination of THC in cannabis products"
Author(s): Franz E. Dussy, Cornelia Hamberg, Marco Luginbuhl, Thomas Schwerzmann and Thomas A. Briellmann


What is my fellow C-Wers take on this topic?

Thanks all

[Lundin]

hey gojo:teeth:

you are talking to the right guy allright

google jabir

[guest]

Hummm,

So all of E. Rosenthall's three different figures for decarboxylation are correct, though too high IMO for decreasing terpenoid and flavonoid losses.


Hey MS,

Nice to see ya. Heading to goolge now.

[c-ray]

here's a juicy little tidbit from a gw pharmaceutical patent
http://v3.espacenet.com/publicationDetails/biblio?DB=EPODOC&adjacent=true&locale=en_EP&FT=D&date=20030108&CC=GB&NR=2377218A&KC=A
Surprisingly, it has been found that application of temperatures greater than those used for steam distillation can also speed the conversion of inactive constituents of natural products into compounds which are biologically active and can be separated in high purity by heating and condensation under defined conditions. For example, the principal active constituents of Cannabis sativa and Cannabis indica are the cannabinoids - tetrahydrocannabinol (THC) cannabidol (CBD). Cannabinoids such as cannabigerol (CBG), cannabichromene (CHC) and other cannabinoids are present in small quantities in harvested cannabis plants. The majority of cannabinoids are present in the plant as the corresponding carboxylic acids. The carboxylic acids themselves have little or no biological activity and in the production of cannabinoids for medicinal use it is necessary to convert the cannabinoid acids into free cannabinoids before extracting with solvents or other procedure.

Thus when preparing extracts of cannabis by extraction with ethanol or supercritical CO2 it is necessary to preheat the cannabis in order to decarboxylate the cannabinoid acids to free cannabinoids.

Surprisingly, it has been found that by contacting cannabis biomass with gas at a temperature of 125-450 C and particularly in the range 145-225 C the carboxylic acids are converted into free cannabinoids which are vaporized, and can be condensed. The process of the invention can therefore avoid the need for a separate decarboxylation step, since extraction of cannabis with heated gas at a temperature of 125-450 C, and particularly in the range 145-225 C, results in decarboxylation and vaporization of the active cannabinoids in a single step. The process of the invention is particularly advantageous for preparing extracts of cannabis for this reason. The rate of decarboxylation is a product of temperature and time. At 145 C 95% of cannabinoid acid is decarboxylated in approximately 30 minutes.

my question is are there natural enzymes present in the bud and/or trichomes and how can we activate them without using excessive heat?
or howabout can we extract the essential oils first separately, then extract the cannabinoids and decarboxylate them (without the essential oils), and finally recombine?

[d'artanian]

Thanks bro. Are you saying the correct spelling of COOCH is COOH?
perhaps a typo? but I do not know the context
I believe that there are no known substances/ with the formula COOCH. correct me if I'm wrong. maybe they mean HCOOCH3, metylmetanat, an ester. esters is written as R1COOR2 or -COO-

[d'artanian]

my question is are there natural enzymes present in the bud and/or trichomes and how can we activate them without using excessive heat?
cure buds:kind:

[guest]

Hey C,

One can use alkaline bath with no heat to decarboxylate cannabinoid acids. Heat isn't needed. I don't know what effect it would have on flavonoids and terpenoids, I would like to look into it.

After the alkaline bath using butane or propane would probibally provide the easiest way to get the most true essence of cannabis with a wide range of flavonoids and terpenoids.

You could also use fractional distillation under vacuum if you know the bp of flavonoids in question. Alchemist made the good point one can do the same with Co2 SCE, that is extract different chemicals. I bet the best way to get the most terpenoids and flavonoids is to use a luke warm water alkaline bath for an hour then use butane or propane extraction under pressure. Then using ethanol to further remove butane, plant waxes, etc, to better experience flavonoids, etc. I don't know if the full flavonoid and terpenoid profile has been anayized that is why I think the shotgun approach with butane or propane could be the best option, at least right now.

HTH

[TheForSaken]

howabout can we extract the essential oils first separately, then extract the cannabinoids and decarboxylate them (without the essential oils), and finally recombine?

Are you asking if we could steam distill the bud to get our essential oil.
Then fractional distill the essential oil under vacuum in order to keep the heat to a minimum in order to not degrade the oil.
Then collect the different boilling point fractions, individually.
Disregard the fractions you don't want and combine the fractions you want to keep as you wish?
Has this been attempted? Only solvent you would require is dh20.
Regards
TFS

[guest]

Hey TFS,

Do you mean as a fragrance? Or possible medical extracts? Without cannabinoids? Why use steam distillation? To make the fractional distillation easier and simpler?

I know there has been a lot of work with extracting terpenoids, but I have not looked into it. I think C-ray said Sam Skunkman has been doing research he keeps secret.

I got your PMs, sorry I didn't respond yet. I will tonight or tomorrow. They were helpful thanks.

[TheForSaken]

Yes as the fragrance, all plants have an essential oil. Many of which are very medicinal. Essential oils are concentrated plant extracts.
I can elaborate on super cheap, super ghetto DIY steam distillation apparatauses;)
Once you have the essential oil, you have all the goods in liquid form, which is the only way one may move on to the distillation.
The essential oil will contain many different compounds all with their own different boiling points.
Very easy to seperate them all.
No problems on the pm's, just wasn't sure if you were getting them.
Peace
TFS

[guest]

Hey TFS,

What temperature does steam distillation operate? I haven't looked into stem distillation. If too hot I would think that's something to stay away from, no?

If you didn't want cannabinoids (I don't think that was what C-ray was referring to) why not use butane under pressure (less heat than steam, no?) or if price is no big deal Co2 SCE? Why do you prefer steam distillation?

I'm aware of essential oils and what they are, I was curious why you suggest steam distillation as it seems less than ideal due to (I assume) high(er) temperatures.

[guest]

In my understanding butane (or propane) extraction under pressure might be the best extraction method for cannabis, at least one most people can could afford, to extract a wide range of flavonoids, terpenes, etc.

I'm curious, what do you consider to possibly be the best extraction method within financial range for most of us?

[TheForSaken]

Steam distillers operate at boiling water temps.
I suggested to give it a go simply because the only solvent used is water throughout the whole prosess.
But after re-reading this thread, I noticed c-ray mentioning that through steam distillation, one can not get to the goods that one seeks.
Sorry for the derailment.
TFS

[guest]

C-ray,

I don't think I fully answered your question. If you don't want to use butane extractor like a Tamisium, you can do as you ask as so (but its more trouble IMO and required strong chemistry background):

After doing a simple extraction with a solvent like petroleum either you could chelate THC-A separate with column chromatography, then when fractionally distilling under vacuum the THC-A will decarboxylate. You could also use column chromatography to separate any CBD, which could be isomerized using the fractional distillation unit. If could you find out how to elude the specific flavonoids and terpenoids using column chromatography you would have separate extracts (as eludes). Then if you know the bp of said flavonoids and terpenoids you could further purify the extracts with fractional distillation under vacuum. And finally for to make very pure extracts once again use column chromatography. Then combine at will.

But, all that said, IMO using butane to extract near the majority (or majority) of terpenoids and flavonoids is definitely easier. Then clean it up with ethanol and vacuum evaporation.

Anything past a high quality extractor like a (eg. Tamisium) will probably require chemist skill (at least a little), for example, fractional distillation under vacuum.

[guest]

Hey again C,

With the method I am suggesting one can keep heat at or below 110'F. That seems ideal for optimum flavonoid and terpenoid profile.


Temperature:


First step: Alkaline bath with luke warm/tepid water for an hour or two ~80'F

Second step: Butane extraction under pressure ~100-110'F

Third step: Redissovling BHO into ethanol co-solvent ~0-5'F

Fourth step: Vacuum evaporation ~68-80'F (local room temperature)


Aloha Nui Loa

[guest]

Due to the length and complexity of this thread I thought I would post a short summation of what I have found so far.

I went back and re-read what the chemist told me. That the co-solvent (ethanol) has to have a higher density than solvent (butane). And butane has to have a lower bp (boiling point) than the co-solvent. Fortunately, both requirements are meet with what I am proposing. Below I detail the physics behind the solvent/co-solvent interaction.


Here's a quick run down:


This method should yield a extract of absolute purity. A similar method to what I am working on is used by big Pharma to created injectable drugs from a DMSO compound redissolved into ethanol as co-solvent. My extract will be chalk full of terpenoids and flavonoids, while reaching around 90+% THC (to total cannabinoid profile). While I believe the extract will be free from solvents, if it does have any they will be trace levels below limits for intravenous drugs and it would only be ethanol.

The final extract should be as pure as Co2 SCE, that is, free from hydrocarbons, while retaining a wide(r) profile of terpenoids and flavonoids thus IMO possibly making my proposed extract better than Co2 SCE. The great thing is as you will see, no chemistry background is needed. I've done all the legwork, I even have a 'shopping list' I will post for people. All told, one can spend $800-2000 (depending upon size of extraction apparatus) to produce extracts probably as good, or better in some ways than Co2 SCE which costs 20-30k.

An important issue is the density and bp of the co-solvent. The co-solvent (ethanol) needs to have a higher density than the solvent (butane). When BHO is dissolved into ethanol any residual (and less dense) butane 'trapped' (not precipitated) in the BHO will be released and rise to the surface of the (more dense) ethanol. And because butane has a lower bp than ethanol the butane will fully boil off first! At this point there is zero butane left in the EC and from here its all about boiling off the ethanol, which is non-toxic :)

Ethanol density = 790 kg/m^3

Butane density (liquid at bp) = 601 kg/m^3

Butane density (gas at room temp) = 2.52 kg/m^3

HTH

[c-ray]

have you researched what a diy co2 extractor would cost, I'll bet it's far less than $20k

(ps. I'll be waiting for you @ post #219 of this thread with victory doobie in hand)

[d'artanian]

Steam distillers operate at boiling water temps.
I suggested to give it a go simply because the only solvent used is water throughout the whole prosess.
But after re-reading this thread, I noticed c-ray mentioning that through steam distillation, one can not get to the goods that one seeks.
Sorry for the derailment.
TFS
perhaps superheated steam (http://en.wikipedia.org/wiki/Superheated_steam), can do the job?

[d'artanian]

perhaps superheated steam, can do the job?

sorry, forgot that the bp. THC is 200C at 0.02 torr. it'll be difficult to keep the vacuum with a steam source in the system

[guest]

Hey c,

No I haven't looked into DIY co2 SCE. It sounds dnagerous to work with that high pressure in a DIY fashion. I'm no engenieer and would prolly blow myself up. Haha.

Thansk bo, ill meet you at that post. For reals though, someday we will all chill and get hiiigh :)

[guest]

On the topic of Thin Layer Chromatography (TLC)...

I have developed a very good method to use TLC for testing cannabis samples for semi-quantitative (comparative) and quantitative results. Its not much different than traditional methods, just more streamlined IMO.

Anyway, there is a thread at icmag where someone asked about TLC. So I wrote up a little into for TLC. I hope you all find it useful.

I plan to use TLC for qualification and quantitation of butane and ethanol in samples of my final extract. That way I will know for sure if its a good method!

The TLC method I've been working on is easy and I'm setting it up with chemistry newbies in mind. Its inexpensive too, after minimal startup costs. So anyone of you can spend $100-200 for supplies to carry out many tests.

Scanning spot density is the best TLC method, one can use Photoshop to do the same, or the free JustQuantify, or the great JustTLC (makers of JustQuantify).

A standard is >98% pure cannabinoid in question. Without a standard one can't tell how much cannabinoid is present in a sample, ex. % THC (by weight). If one does have a standard then they know the quantity (weight) of the cannabinoid in the standard. Thus by comparing spot densities one can calculate the weight of the cannabinoid in sample.

IIRC, JustTLC has been proven as accurate as HPLC if done correctly. There is a independent study on the JustTLC site with evaluates and states JustTLC for use in analytical research.

If one has no standard then one can get a baseline (average) of X samples. Then test samples and save ones which surpass the baseline. Of those, run comparative test to see which has the greatest density spot. The sample with greatest spot density = strongest sample.

Using fast blue BB reagent one can test for many cannabinoids. With use of a reagent we can use spot color as cannabinoid qualification, no need for Rf vales.

Hey! Now I think about it one could very easily use TLC for qualification of hydrocarbons in the sample! This means one can tell if/how pure their sample (ex. BHO) is. For example: one can test to see if there is presence of butane in the sample (qualification). And using a butane standard, one can tell how much butane is present in the sample (quantitation). All one needs to know is the TLC mobile phase and visualization reagent for butane and ethanol.

[guest]

TLC = should be no need for GC/MS or HPLC. Very small amounts of butane can be identifed with TLC.

[Springs]

Saaweet! That sounds frickin great, how high up on you to do list is this? :good:I cant wait!:D

[guest]

Hey bro,

I'm doing it today :) I can't believe I didn't think about testing for butane with TLC before! I was planing on using GC which can get pricey and not legal in all but 13 US states. I need to find out the mobile phase and reagent, etc, needed for butane. Should have research done in a couple of hours, I hope.

One could also test for specific petrochemicals or fungicides, etc. Stuff we don't want to smoke. So if buying for med purposes one doesn't have to trust the seller.

I would to try and figure out a way to test bud to see if it was grown with chemicals or not. I doubt it possible without tracers which would make the method impossible (can't add tracers after its harvested).

I plan on doing a pictoral once I am ready and make a thread. For now ill post some TLC info here.

Here some links that may help people understand what this stuff is all about:

-Quantitative TLC:
www.chromatography-online.org/quant/contents.html


-"Quantitative Chromatographic Analysis"
by Raymond P. W. Scott
http://www.chromatography-online.org/quant/Quantitative%20Analysis%20by%20TLC.html


-Video tutorial for TLC:
http://www.chem.zenkyo.h.kyoto-u.ac.jp/operation_eng/operation_16/operation_16.html

[guest]

Making or ordering standards:

One can use TLC (with effort) to make pure standards of THC (for example)! That is great because it enables one to use true quantitated results with TLC on the cheap! See this thread:
www.chemicalforums.com/index.php?topic=10949.0

Although, if making ones own standard than using HPLC to create standards is generally much preferred. But HPLC are expensive. All I would need to do is figure out what solvent to use to remove the silica, and maybe a second purification step, but its possible, tho not simple. Once one has their standard they need to test it to insure its purity, two tests are ideal.

That is how Sam Skunkman got his THC standard for his GC, he made his himself using HPLC. I know other people who have done this. I have a great paper detailing how to make standard of THCA-A using HPLC. One can adapt that paper for other cannabinoids if one has an HPLC.

Standards are expensive, and sometimes not what they claim (ex. Sam said Sigma THC standard was only 87% THC, IIRC). That is why he made his own, he could not find a good source. Over 2k for very little is common most of the time. Check out this company to order reference standards. Tho I doubt they will ship to the US without lots of documentation:
www.lipomed.com

BTW, this brings me to Dr. Hornsby (sp?), I have very strong doubts about the quality of his standard, or at least the calibration of his GC. I think his figures are inflated a lot due to poor standard. For example, some guy here claims the Dr. tested his budder (from QWISO IIRC) and it came out like 90+% THC! Haha, yea right! That is proof enough for me. IIRC the icmag member who got the budder tested is the guy who came up with budder, or a friend of the creator of budder.

[Green Supreme]

Hornby uses HPLC. Peace GS

[guest]

Hey bro

How ya going? I'm not sure, are you positive? I have read posts about his testing with GC and C-ray told me the Dr. did all GC testing for Med Canada.

Thanks as always

[guest]

Hello,

Due to much interest in TLC I wrote a little something. I wrote it quickly so forgive typos or slight omissions.

You want the salt, fast blue bb salt as regent, it shows all the neutral cannabinoids. You don't need a license.

Use silica. Dip the plate, do not spray.

I will upload my digital mini-library on TLC, HPLC and GC; all on the topic of cannabis. Mostly TLC but the best manuals by the UN and NATO also have great directions for testing all kinds of drugs with TLC, GC, HPLC, etc. I can probably upload 5-10 full text journal article plus manuals from the DEA, UN and NATO.

I think people will learn a lot from them.

Here is a quick into, this might have typos or slight omissions, I'm tired. If so ill fix it tomorrow:

1. Extract cannabinoids

2. Sample super critical solution with micropipett.

3. Spot plate with micropipett. Two applications per spot can be good. This is the stationary phase.

4. Put plate into 'developing chamber'. This is the mobile phase. In the chamber is the hexane:ether mix (4:1), a little in the bottom. Along one side of the chamber is the filter paper, it is wet with developing solvent (synonymous with mobile phase). The filter paper and solvent are to fill chamber with fumes to facilitate the mobile phase. The developing solution will run up the plate. Dragging invisible lines of cannabinoids with it. Once wet mark reaches top line of plate (0.5" from top of plate) its done. Pull out and allow plate to dry. This can be speed up with very light warm air from hair dryer, but allowing to dry in a vacuum desiccator is much, much more ideal and quicker too

5. Before applying the visualization reagent one should make the silica plate alkaline first, better results with cannabinoids. So mix up as below and quickly dip the plate into the alkaline solvent. Allow plate to dry as before.

6. After plate is dry dip in reagent (1% fast blue BB salt in water). Allow to dry as before.

7. After plate is dry dip in preservation solution. Same as the alkaline solution. Allow plate to dry as before.

8. Scan plate with flatbed scanner and upload to JustQuantify for free spot density scanning and assay. If you place a few different samples on one plate it makes comparisons easier and more accurate.


Done!


Below is needed to test cannabinoids:

Chemicals:

Petroleum ether (extract solvent)

Hexane

Ether (mix with hexane as 4:1 hexane:ether as mobile phase)

Fast blue bb salt (visualization reagent - add 1% to water)

0.1M sodium hydroxide (Alkaline solvent and Preservation solvent)


Materials:

Glass jars 1L, 0.5 L, 0.25 L

filter paper

5mg spatula

Microscale

A few eppendorf (1.5 ml each)

Eppendorf holders

Capillary micropipett (3ul)

1ml pipett

Pasture Pipett

50 ml test tubes

5 ml vials

Motor and pestal

Test tube vibrator or ultrasonic vibrator (optional)



US sources of chemicals:

I get fast blue bb salt here:
http://www.sciencelab.com/page/S/PVAR/10413/SLF1114


Carolina chemicals:
(They sell many kinds of kits)
http://www.carolina.com/category/physical+science/chemistry/chemicals.do?KickerID=int_t_hom_chemicals


Science Lab (same place I get reagent):
http://www.sciencelab.com/page/S/CTGY/10405


Here is a good ebay site:
http://stores.ebay.com/AVOGADROS-LAB-SUPPLY

[guest]

BTW,

One does not need all the materials I listed, like pipett, some jars, eppendorfs, etc. I made the list a bit bigger than the bare minimum. But, if one has the money my previous list can allow one to process more samples simultaneously and give one greater flexibility.

Here is what I think might be bare minimum:

Silica plates

Glass/pyrex jars a few sizes up to 1L.

Tweezers

Spatula (5mg)

Microscale

Many disposable capillary micropipett (3ul)

Filter paper or blotting paper or paper towel

5ml vials

50 ml test tube

Motor and pestal

[Green Supreme]

Perhaps he has changed then. I once challenged his methods in person when he stated his numbers came from hplc. Peace GS

[guest]

OK, thanks bro. Yea HPLC would have the same potential problems with quality of standards.

If you don't mind, could you add some context? Why did you think to challenge him in the first place?

Thanks a lot

[d'artanian]

Hey Gojo. TLC is awesome for a home setup. But try to avoid using hexane, since it is very carcinogenic. cyklo-hexane, heptane or pentane may be used as an alternative

you may also have difficulty identifying butane and other hydrocarbons with a lower bp. than the mobile phase, since TLC-plates must be dried.

[guest]

Hey gerber,

Yea hexane is not the nicest solvent, but its ok with fume hood, or outside. I have a few other mobile phase solvent mixtures, but none are 'safe' per say. I will look into replacing hexane with what you suggest, tho I have some doubts they will work well with ether.

To your point about the bp, yea I thought about that. I am considering doing TLC in a large cold cooler and using vacuum desiccator in same cold environ. I thought about using the walk in freezer but no one will have that at home, so I think a cooler may work.

I need to figure out what extract solvent, mobile phase and hopefully visualization reagent to employ.

What do you think? Any ideas for chemicals for butane TLC?

Thanks bro

[d'artanian]

ether should work with pentane and cyclohexane, since they are soluble in each other and have similar vapor pressure as ether. heptane can be somewhat difficult to use, because of the vapor pressure

the mobile phase must evaporate before one can detect the presence of alkanes on TLC. so this is very difficult. but if you've decided, so you had to use liquefied gas as a mobile phase, in a freezer as you mentioned

for determination of butane in a BHO matrix, I would really recommend a GC.

[guest]

Hey bro,

Yea the vacuum desiccator might work for drying the TLC plate (I hope, we will see). This is the only time I wish butanes bp was high ;)

I want to use TLC even tho I know GS/MS is preferred. The problem is no one has a GC and so they can't test cannabis products in all but a handful of US states, and most everyone in those states doesn't know how to use a GC, or where to get a accurate test (which is much harder than it sounds)...

The only reason I want this to work is so anyone can test their extract at home and rather inexpensively, thus lots of people could get better (safer) meds.

If it turns out I can't get it to work I will just test my extract with GC/MS. Assuming others follow my exact methodology the GC/MS results should be valid for their extract too.

Thanks for your input. Ill let you know what I find.

[guest]

Hmmm,

Well after some thought about what Gerber wrote, and discussion with some chemists I am pretty well convinced one can not use TLC to detect butane. I shortly considered using a large cooler kept cold for butane TLC, but that seems like a non-starter.

I am still hoping to find some method for testing at home, but it looks like GC is one of the few options. Thus, I will test my solvent-free extract to see if it's truly solvent free (at least totally free from butane). If my new method I'm working on turns out as well as it should I plan on writing a very detailed PDF paper on the 'how-to'. Then if one follows my methods to the letter they could be reasonably sure their extract is solvent free too.

Ok off to bed! The vicoden and flexeril is really kicking in...yawn, i don't like this type of pill high.

[Lundin]

Tamisium

[guest]

Word. Do you like it? What size? I know the 1oz size has been redesinged a bit.

Would you suggest a Tamisium to others? Thanks for that pic

[Lundin]

oh
its just a picture i saved before their site removed it

i can understand why they removed it. here it is...

[Alchemist]

here's a juicy little tidbit from a gw pharmaceutical patent
http://v3.espacenet.com/publicationDetails/biblio?DB=EPODOC&adjacent=true&locale=en_EP&FT=D&date=20030108&CC=GB&NR=2377218A&KC=A


my question is are there natural enzymes present in the bud and/or trichomes and how can we activate them without using excessive heat?
or howabout can we extract the essential oils first separately, then extract the cannabinoids and decarboxylate them (without the essential oils), and finally recombine?




Great Idea!!! that s the ticket right there

strip the essential oils , then go back after the cannabinoids with a slightly higher density! voila


You guys are way ahead of me on all this stuff! But I will catch up, soon i hope!

Thanks to everyone for posting here, this thread is turning into the definitive extraction resource!

Hey GS, that beeline stuff sounds great, i might order some as im back on my bong now while my vape is getting fixed.

[guest]

As promised,

Here is a list of journal articles and manuals from my collection I included in the file "Testing.zip". I encrypted the folder with the password (not incl. quotes): "TLCrocks"
http://www.filesavr.com/testing_1

TLC:


"Analysis of Selected Pharmaceuticals by Quantitative TLC"


"Separation and Identification of the Consitiuents of Hashish by TLC in Forensic Analysis"


"Evaluation of quantitative TLC using Staining Reagents" ---> paper about and review of "JustTLC"


"Silica-Gel TLC Protocols"


"TLC Test Protocol". --> GREAT manuel, excellent pics and explanations



GC:


"Gas Chromatographic Determination of Tetrahydrocannabinol in Cannabis"



Multi tests - TLC, GC, HPLC:


"The Analysis of Controlled Substances"


"Identification and Determination of Cannabinoids"


"Simultaneous Separation and Identification of Hashish Constituents by Coupled HPLC-MS"


"Recommended Methods for Testing Cannabis" ---> Untied Nations manuel from 1987 (info still valid)


"Detection of Cannabis in samples of different sources" ---> The TLC method on page 6 is what I plan to use.* I might replace hexane.



**I reuploded the winzipped files concerning decarboxylation and I encrypted the folder with the password (not incl. quotes): "TLCrocks"
http://www.filesavr.com/decarb

[d'artanian]

My main idea[1] is based upon the physics of the solvent and co-solvent. I am assuming all butane will boil off before ethanol, thus, an absence of ethanol should indicate an absence of butane.

A second feasible idea[2] is to redissolve the final extract into a solvent. Then add
Potassium permanganate or potassium dichromate to compound. If one smells a foul odor then ethanol (alcohol) is probably present (this doesn't mean butane is present).

A third idea[3] is to use fluorous phase TLC chemistry to identify ethanol (see below). I know very little about fluorous phase chemistry, but that's fine, this method IMO is a non-starter. Its too much chemistry work for most people.

hey Gojo.
the first idea of your sound sensible.

but the problem with the second idea, as it is described, is that permanganate and dichromate, are very strong oxidizing regents, and will react with many of the components in the sample.
by oxidation of ethanol, we get vinegar, which has a strong and unique odor.
But ethanol also smells quite strong, and even small amounts of alcohol in a sample, one can easily smell when heated. so therefore I see it as unnecessary to work with these oxidizing, carcinogenic (!), and environmentally harmful substances.

idea 3 I have not read through all of the links. but I can say that the fluorous stationary phase usually it's used for seperasjon of PFC (http://en.wikipedia.org/wiki/Perfluorinated_compounds).

[Lundin]

Hey MS,

I don't see anything below the last sentence above. Did you post a link? Sometimes I can't see links with this computer. Could you please repost it or PM it to me?

Thank you

http://tamisiumextractors.com/tamisium-extractors.htm

[Green Supreme]

A post by Skunkman Sam I feel deserves notice here. Peace GS

http://www.icmag.com/ic/showpost.php?p=2329794&postcount=8

ps. and the thread it came from http://www.icmag.com/ic/showthread.php?t=120677

[Green Supreme]

This fellow at ICmag seem like he may have a good grip on CO2 extraction. Peace GS

http://www.icmag.com/ic/showpost.php?p=3110959&postcount=77

the thread it came from http://www.icmag.com/ic/showthread.php?p=3110959#post3110959

[hypnotoad]

http://forums.mycotopia.net/botanicals-cactus-misc-entheogens-psychedelics/53045-diy-soxhlet-extractor.html

DIY extractor. Hmmm...

[Lundin]

thank you for posting that! lets upload the pictures here so people can get some inputs on how to make something similar

[Sicarii]

I made something similar once for a school science fair. I made perfume mind you not cannabis extracts (and I'm sure that's why I didn't win;)) I used glass bottles tho and just cut the bottoms off of them. it worked pretty well, but the bottles were attached together with something that eventually dissolved(I don't remember all the details as I was like 10 :)).

I just may have to try to make another one of these.
thanks for sharing
peace sicarii

[Alchemist]

GS, thanks for all the links! I have an account at ICMAG but never go there much. some great posts over that way

[c-ray]

this looks like it could be fun:

http://www.globalgilson.com/productdisplay.asp?model=GA-18

http://www.globalgilson.com/images/product/large/GA-18.jpg

The GilSonic SiftMaster (GA-18)

• Fast, efficient separation of dry, flowable materials.

• Exclusive AutoSift self-adjusting controls.

• No.18-No.635 sieve range (1,000µm-20µm size range).

The GilSonic SiftMaster applies the proven efficiency of sonic separation to rapid continuous production sizing of flowable powders. Both power level (amplitude) and pulse frequency of the unit are quickly "tuned" for individual material types. Gilson's AutoSift electronic control monitors and adjusts material flow for maximum output with clean separation. Dual-position tap de-blinding keeps meshes clean. Once feed and product collection are set, no further operator attention is required. The device is ideal for low-volume continuous production of many materials including powdered metals, ceramics, minerals, ores, chemicals, cements, etc. Sealed all-stainless contact areas are easily accessible for food or pharmaceutical cleanups or for other low contamination applications. The unit is also suited to research or pilot plant applications.

Normal sifting devices use movement of the screen surface to throw material and rely on the limited force of gravity to return particles against sieve meshes. Difficult fine or low density powders do not separate efficiently. By contrast, SiftMaster has a stationary sieve surface. Particles are lifted and forcibly tried to meshes by an oscillating air column that may be tuned to 2,400-3,600 tries per minute. Downward thrust by the air column acts as a "gravity-assist" to permit sifting many particles that will not separate by conventional means. For easier materials, the "assist" yields increased throughput and efficiency. Gentle sonic action assures screen wear and particle degradation are reduced.

Setup conditions for a given material are all established in minutes by simple manual adjustments while observing sifting action through the observation window.

When switched to AutoSift mode, an electronic sensor monitors material passing wire cloth mesh. When incomplete separation is sensed, AutoSift cuts power output. When clean separation is restored, power is automatically increased again. Highest throughput with sharp separation is assured. Sensors are continuously cleaned by a built-in air supply stream. Wire Cloth Units are changed through a front opening in less than a minute. SiftMasters may also be stacked or operated in series.

The SiftMaster is supplied on casters with 6ft (2m) of flexible hose that may be cut as desired to fit feed inlet and oversize/undersize outlet ports with clamps provided. For additional hose and clamps, order GAA-14 Kit. A freestanding, stainless steel 1.5ft3 (45qt) Feed Hopper is available as GAA-12. Round stainless steel containers for storing or collecting powders all have two welded-loop handles and matching cover.

[Green Supreme]

One of these http://www.rmsross.com/derocker.html

on one of these http://www.iowagold.net/HOWTOPAGES/how_to_build_and__run_a_sluice.htm

Peace GS

[spaceman]

hardcore!!

[Parabola]

siftmaster... the name says it all

[c-ray]

cold ethanol quick wash:
http://www.treatingyourself.com/vbulletin/showthread.php?t=44323

[Bram]

yes, i been wanting to play with 99% ethanol for awhile now. I noticed with my potka how it didnt pick up chloro's, but captured the full flavour. I think you can do longer then 3 mins tho. I would let my vodka sit in the freezer after adding the leaf into it for up to 7 hrs, and still no green at all.

[c-ray]

everclear is 95%

[Bram]

ya, but i would have to go to alberta to get that i think. havent seen that in the stores here. time to find some rednecks.

[c-ray]

I bought some at a duty free store in BC once upon a time

[spaceman]

we will try the ethanol wash next.,.,

[nuggdigger]

190 proof..soon come:pimp:

[c-ray]

https://rowellsapushistory.wikispaces.com/file/view/Moonshine-Still.jpg/62367540/Moonshine-Still.jpg

[Green Supreme]

Saw this recently and it has the gears turning. Peace GS

http://heartmagic.com/EssentialDistiller.html

[memyselfandi]

that looks real cool, pure oil. is it possible ?

[c-ray]

I thought those were for essential oils mainly?

[Green Supreme]

Was thinkin about using alcohol. Peace GS

[Lungus]

If you can get someone to go into states for you they could bring back some Everclear grain alcohol. It's 190 proof, great for making extracts.

[nuggdigger]

ahmm..ahmm..ahmm

im so sorry gs..
there is a story behind that..
a case came from the land of guns and oil..
it was brought nonprofit..no delivery costs..10 discount for caselot included..
it was stated/noted that bottles were called for..but only about 1/4 of them..
namely in the order of those who asked..
gs..vapor..pb..and then to be offered to other senior members..
as far as i know two bottles went close to k-man and that is all i know..
the last time i gave a reminder i was told to f.o.
i reiterate..im so sorry..
i now have to make another trip..lol!
peace

[Green Supreme]

No malice bro. Peace be with you. GS

[Harvester]

Thinking out the Co2 methodry, I am wondering why the $30k expense? Isn't it on the same principal as butane extraction, but at a significantly higher pressure?

Co2 is cheap and free of suspicion I think it's like $30 to have a big tank filled last I checked. It takes about 1000 PSI to keep it as a liquid, which is safe to use with many materials as long as they are assembled properly, however I would think one would lean towards stainless steel for it's food-safe properties.

This might be something worth doing. I know I could get the fabrication part of it correct, but the design would need a little research to be sure of function and safety. Would have to be sure that the Co2 stays a liquid while washing the materials, and also have to make sure that there is a controllable and safe manner in which to relieve the pressure and collect the goods.

I wonder what other type of seemingly 'inert' gases could work. I know that the old refridgerant R-12 was a liquid at 300psi or so and it also carried mineral oil...But even the new 'eco-freindly' refridgerant gases aren't something I would want to dispense into the atmosphere... I am guessing that the cost of these commercial units is greater due to being able to re-capture and re-use the Co2.

I did find this link. If guys can run liquid Co2 directly to a paintball gun (skipping the gaseous state), then we ought to be able to find a way to make that same paintball gun ooze out honey oil...lol.

http://www.vmempire.com/liquidco2.htm

H

[c-ray]

stick with CO2, .. it is possible to use refrigerants like r134a at low pressures for essential oils but you will need to do your research to find the right refrigerant if you want to extract resins

[Alchemist]

bioexx (sp???) extraction in eastern Canada uses a coolant similar to freon to extract. The main draw of this is that it has great solvent power at low temps (30c) and when oils or other lipophillics are extracted from a biomass with remaining protein, the protein is suitable for high quality animal feed as the low temperatures do not denature the proteins. I don't know of their current status as far as human products go, but most natural health products folks don't really view this as being as sustainable and non-toxic as the co2 alternative.

[c-ray]

Peter Wilde is the name of the guy who invented fluorocarbon extraction for anyone who is interested in fluorocarbon based solvent extraction, there are some patents that describe it all.. I agree with the Alchemist though, doesn't seem like it would be really clean like a good CO2 extract

[Green Supreme]

This never happens to hash makers. Peace GS

http://www.youtube.com/watch?v=gzUd8KICcrk&feature=player_embedded

[Green Supreme]

Ya of course my shit's purged properly. Peace GS

http://www.youtube.com/watch?v=zovD6TPywYg&feature=related