Soxhlet Extraction method...

sworth

Well-Known Member
I've been looking into the "Soxhlet" extraction method today (thanks riu!)

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

Thinking I may buy on, but just want to see if anyone has tried this?

Oil is my favoured method of using up my trim etc. at the moment, and this is great as it re-uses the iso-propyl alcohol.
It even look good!
I hope I'm not now going to find out why it's not so popular...;)
Thanks, as ever, in advance...
 

sworth

Well-Known Member
Wipe some on a paper, a drop on a pipe...it can be a little messy...somewhat like myself after consuming its concentrated stonedness...;)
 

oakley1984

Well-Known Member
this method of extraction is not suited to do high quality extractions

in 99% of cases hot solvents and mj dont mix welll... you end up with liquid plant, not concentrated cannabinoids
 

george xxx

Active Member
I've

this is great as it re-uses the iso-propyl alcohol.
It even look good!
I hope I'm not now going to find out why it's not so popular...;)
Thanks, as ever, in advance...
It uses equipment not readily available to most people. You can extract cold. Use heat to remove and reclaim the alcohol.


This guy's recipe is readily available on the web.

Honey Oil
Written By: Bud Oilerman

Equipment and Materials To Make Marijuana Honey Oil
Written By: Bud Oilerman
1. Marijuana stalk, leaf and bud can be used. Make sure your marijuana is dry. DO NOT GRIND UP YOUR WEED. Start off this recipe with 4 ounces of weed. You can use as little as one ounce or as much as you want. Simply cook just leaf and produce a wicked honeyoil. Try to use buds for special occasions. The best place to get free weed is off of someone who just finished a grow room and has a whole bunch of trimmed leaves and stalk lying around.
2. Isopropyl Alcohol 99% pure. Make sure it is 99% pure Isopropyl Alcohol. The alcohol ranges from $5CDN to $13CDN per 4-litre plastic jug. Any pharmacy should have Isopropyl Alcohol 99% on the shelf. When using 4 ounces of weed as mentioned above you will need 2-litres of Isopropyl Alcohol 99%.
3. Empty 4-litre plastic milk jugs (4). Three jugs you cut the top off so you turn them into a pail. The other one you cut the bottom off so you can use it as a big funnel. Sterilize each one with hot water and clean thoroughly. DO NOT use soaps or cleansers to clean. No foreign debris in the jugs.
4. Empty 2-litre plastic coke bottles (2). Cut the tops off so you can use them like a funnel to pour into the bottom part of the bottle. Make sure the pieces are very clean. Again, just use very hot water to clean with and NO soap or cleansers.
5. Ordinary coffee filters. You'll need at least three filters to start with. You will be using the top of the cut up coke bottle and the filters together.
6. Refrigerator freezer or an IceBox to freeze all the ingredients.
7. Clear plastic tubing to fit the lid on a pressure cooker. 6 to 7 feet. Determine the size you need by reading the next item below.
8. Pressure Cooker of average size. They can be found at any second hand store. Can pay as little as $10CDN for second hand. Or you can buy one new. Pressure cookers have one or two holes in the lid, usually two. Take off the top fittings from the holes in the lid and insert three feet of clear plastic tubing in each hole. Maybe use some tubing from an aquarium. You can get cheap tubing from any hardware store. Pay attention to what size tubing you need for your lid. Please ensure when inserting the tubing into the top of the lid that it is secured airtight somehow. This is really the only pain in the butt part of it all. There are fittings you can get from the hardware stores or plumbing stores to help you. The alcohol will be going through the tubing while under a vacuum pressure. If you are not too handy at this, seek a friends help. Test your pressure cooker with boiling water. Positively NO LEAKS at the lid please. The open ends of the tubing will run into a collection pail so you can reuse your Isopropyl Alcohol over and over. The main purpose of a pressure cooker is to recycle your Isopropyl Alcohol and control dangerous fumes. You can just have the Isopropyl Alcohol evaporate away so you don't have to use tubing but this isn't recommended, it's highly flammable.
9. Electric Frying Pan that the pressure cooker will sit in.
10. Water to put into the electric frying pan to slowly heat the pressure cooker.
11. Small Pane of glass for drying out a finished product.




Preparation For Extracting Hash Honey Oil From Marijuana
Written By: Bud OIlerman
1. Place the dry weed and jug of Isopropyl Alcohol 99% into the freezer. They can be in plastic containers. Do not grind up or rip up the weed. Just put it into the freezer.
2. Now prepare a juice weasel. Simply cut the jugs as described above. Check out all your plastic jugs for debris, hair, etc. Make sure they are clean.
3. Take weed and alcohol out of the freezer after a good hour or two of freezing. The colder they get, the better the reactions will be.
4. Rinse the weed with the frozen Isopropyl Alcohol 99%. Just put the weed in a jug with holes at each end. Simply pour the alcohol over the weed quickly and collect the alcohol/THC liquid mixture you will be left with. The alcohol/THC liquid mixture should look golden brown or yellowish in color. Don't throw out the weed you just washed. Again the weed and alcohol that was just used should end up in two seperate containers. One with washed weed and one with the Iso/THC mix.
5. Repeat this rinse cycle a good three times. DO NOT let the Isopropyl Alcohol 99% soak in the weed. You just want to do quick rinses while the alcohol and weed are still very cold. Otherwise you loose the nice golden yellowish clear color and the oil turns green from chlorophyll.
6. Place a doubled up coffee filter in the funnel you made from the coke bottle.
7. Now filter the rinsed out alcohol/THC liquid mixture by pouring it through the double coffee filter funnel and into the coke bottle. This gets rid of any sediment.
8. Throw away the double filter and use a single filter for a second pour or filtering. Never filter over a kitchen sink. Fire can go right down the drain and become very serious.
9. Now warm up the alcohol/THC liquid mixture to room temperature. This makes it easier to cook with.
10. The final product should look clear of debris and light brownish/yellowish honey in color. You have collected all the THC into the Isopropyl Alcohol. You are now ready to get rid of the alcohol and have just the THC left

Cooking Marijuana Into Hash Honey Oil
1. Run an extension cord to a discrete place outdoors. the best method is to cook in the trunk of an old car in the backyard. The biggest reason for outside cooking is to help deal with dangerous alcohol fumes from the evaporation process. Cooking can be done inside on an open stove burner in a stainless steel pot, however the fumes in the air can ignite quite fast. A pressure cooker helps keep fumes in. A safer way to cook indoors is to use a pressure cooker on your stove. Very low heat. The pressure cooker helps recycle your alcohol for use again. So you see, it can be done indoors but at your own risk. It can be done with or without a pressure cooker. OUTDOORS PLEASE.
2. Fill your electric frying pan half full of water. 3. Place the filtered solution of alcohol/THC liquid mixture into the pressure cooker and place the lid on. Check the lid and make sure the fittings are tight. 4. Put the pressure cooker full of the alcohol/THC liquid mixture onto the electric fry pan half full of water. The warm water will evaporate the Isopropyl Alcohol.
5. Have the hoses running off your pressure cooker lid drip into a collection jug. You are recycling your alcohol. Do not place the tubing inside the jugs, have the tubing drip into them. If the tubing is right inside the alcohol in your collection jug and the pressure cooker drys up, a reverse vacuum will occur and your alcohol will be sucked back into the pressure cooker. This will happen at the end of the cooking process. A tight seal for the tubing on the pressure cooker lid is needed because a vacuum is created during cooking and is an essential part of the process so it must be working properly. If your seal is OK then the process goes real smooth. Again it is not recommended but the Isopropyl can just be evaporated in the air. OUTDOORS PLEASE.
6. Now turn on the heat for the electric frying pan to around 190 degrees Fahrenheit. NO HIGHER. VERY LOW HEAT. You are about to evaporate the Isopropyl Alcohol out of the THC.
7. Watch the process. It should take an hour to complete give or take fifteen minutes. The alcohol will begin to run out of the tubing at a steady rate. Just let it evaporate. Very low heat. Do not get impatient. Not too often, but every once in a while, lift up the pressure cooker lid and look at the progress being made. All you are really doing now is evaporating away the alcohol so you will be left with a high concentration of THC in oil form.
8. The alcohol in the tubing will stop being a steady stream and start to be airy with bubbles telling you no more alcohol is left. Another way to see if all the alcohol is evaporated is just look inside. The oil should be almost like a hot tar. If you tilt the pressure cooker around the oil will move like a slow liquid. 9. The process is now done cooking and should have 90% of your Isopropyl Alcohol returned in the collection jug. One can use the Isopropyl Alcohol over and over again.


Finishing Making Marijuana Honey Oil
Written By: Bud OIlerman
1. While the pressure cooker is still warm, pour the finished honey oil onto something like a pane of glass. The honey oil still needs to evaporate a little more alcohol out of it. Just for an hour or so. Keep your eyes on the honey oil, as you don't want it to get rock hard. You'll like to be able to pick up the honey oil by a knife and have it drip slowly into a glass vial for storage. Don't mind the texture being a consistency to pick it up with a knife but it won't drip off into the glass vial, it needs just a little heat from a gas lighter to get the honey oil to flow.
2. Marijuana Honey Oil will store forever in glass jars.
3. Yields are 1 gram to 3 grams of honey oil per ounce of leaf/stalk or 5 grams to 7 grams of honeyoil per ounce of bud.
4. The old weed you rinsed can be soaked in Isopropyl Alcohol instead of a quick rinse. Soak it for 2 or three hours. Use the same cooking procedures. This will produce a lesser quality green marijuana oil that everyone is used to seeing.
5. Smoke it in a pipe, on a rolling paper with weed, on charcoal, off a pin, off a hot knife, or whatever you think is cool. Personally, try to a bent the end of kitchen knife to sit on a small torch. Stays on the torch all day.
6. The honey oil is well worth the effort. One hoot and you are wasted.
 

sworth

Well-Known Member
Yeh thanks George, I've made oil a few times now. The main advantage with the soxhlet extraction is being able to use only 200ml of iso-propyl, and refilling the apparatus with fresh herb as one goes along...
I'm going to buy a set for my next harvest. The plan is to give a quick wash of iso, straight through a sieve, which will be my "grade A" and use the soxhlet kit to get the rest out.
I'll update my results.
The only thing guaranteed is my being entertained with my experiments! ;)
 

MikeGanja

Well-Known Member
Sworth and others, are you still using soxhlet apparatus for your extractions? Do you recommend the method? Pros/cons?
 

MikeGanja

Well-Known Member
You are probably right. I didn't want to start a new thread on the same topic but 2 years is a long time.

Soxhlet extraction sounds great since it recycle the alcohol.
 

Fadedawg

Well-Known Member
Soxhleting using a polar solvent extracts the chlorophyll. Soxhlets work best with a non polar solvent like pentane or hexane.

Soxhleting makes killer coffee...........
 

skepler

Well-Known Member
I did my first soxhlet in the 70s, and was happy with the results. But it is heavy on the chlorophyll. I am much happier with QWISO. One could reclaim the ISO by capturing it in a bowl in the soxhlet setup, but it would have to be warmed or heated, I try to avoid that, and how much water is picked up from the atmosphere in the process? A concern for the next use which may capture more chlorophyll with water in the alcohol.
 

MikeGanja

Well-Known Member
Ok, thank you for explaining. I read an article about the extraction in "Cannabis Alchemy" (Ronin 1989). The author suggests soxhlet extraction after 3-4 hours of refluxing a solvent. They use alcohol as a solvent in the example and the soxhlet is followed by a distillation and finally a purification by separating the good from the bad with ether. Now I understand why I need ether in the final step. Unfortunately lab grade pentane, hexane and ether is hard to in my country.

Soxhlet for the iced coffee gives me a reason to buying this beautiful apparatus. :)
 

Fadedawg

Well-Known Member
I love the old books, but alas, some of them leave much to be desired in details, because they were intended to sell books, rather than teach. At the time they were in the outlaw fringe and not published by the mainstream presses, so worth a premium for their size.

Gold, aka Larry Todd, did list petroleum ether as one of the reflux/soxhleting alternatives, which may be more readily available than the HPLC grades of Hexane we typically use.

Not the same as Di Ethyl Ether commonly referred to as ether and on watch list.

Where do the companies using HLPC's getting their Hexane where you live?

In Cannabis Alchemy's case, the information on THC Acetate suggests that he wrote about some things that he didn't fully vet or understand.

For instance, he went to great lengths to set up an inert atmosphere chamber and used a formula whose chemical ratios suggests it came from heroin production.

We make our the same way they make aspirin from salicylic acid, as taught in Portland State biochemistry lab class, simply by using the same formula and adjusting for the difference in molecular weights. You can compare the formula in your copy of Cannabis Alchemy, to the one us'ns Joe posted at http://skunkpharmresearch.com/thc-acetate/ and .

PS: Hee, hee, hee, you can't have too many toys...............
 
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MikeGanja

Well-Known Member
I am not a professional chemist so I thought all ether was the same. :) It´s the Di Ethyl Ether that's not available. I searched the web for Hexane and I did find a product currently sold to the consumer market to be used as a solvent/cleaner for residues of glue and paint. The product safety document says it contains "petroleum nafta" without benzene. CAS number 64742-49-0. Is this product the same as petroleum ether and low grade Hexane?

Some HLPCs companies where I live are getting their Hexane from companies like Sigma-Aldrich. None of them delivers anything more exciting than filter papers to consumers.

Thanks for the link, very interesting!
 

Fadedawg

Well-Known Member
I am not a professional chemist so I thought all ether was the same. :) It´s the Di Ethyl Ether that's not available. I searched the web for Hexane and I did find a product currently sold to the consumer market to be used as a solvent/cleaner for residues of glue and paint. The product safety document says it contains "petroleum nafta" without benzene. CAS number 64742-49-0. Is this product the same as petroleum ether and low grade Hexane?

Some HLPCs companies where I live are getting their Hexane from companies like Sigma-Aldrich. None of them delivers anything more exciting than filter papers to consumers.

Thanks for the link, very interesting!
Here is the MSDS for that mixture:http://www.docs.citgo.com/msds_pi/19041.pdf
 

MikeGanja

Well-Known Member
Thanks, this product is available so I can test the extraction. Would you recommend the Soxhlet extraction with Hexane as a solvent for a fairly safe and economic extraction with good result or do you prefer the QWISO, butane extraction or anything else?
 

Fadedawg

Well-Known Member
Thanks, this product is available so I can test the extraction. Would you recommend the Soxhlet extraction with Hexane as a solvent for a fairly safe and economic extraction with good result or do you prefer the QWISO, butane extraction or anything else?
I prefer a Butane extraction because it does a good job and is easiest to purge. Pentane would be my first choice for soxhleting.
 
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