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Isomerization: This method is out of "Dr. Atomic's Marijuana Multiplier," one of those early 70's doper pamphlets. This process assumes you have pure hash oil to begin with.
* Dissolve the hash oil in absolute ethanol or pure methanol in the ratio of
one gram extract to ten grams solvent. There must be no water in this
solution, as the next step is the addition of one drop of 100% sulfuric acid
per gram of extract.
* Add the acid slowly, drop by drop, stirring slowly and completely, with a
long glass stirring rod.
* Place a Pyrex pot containing the extract-alcohol-acid solution into the
refluxing apparatus and reflux for two hours. The acid will not evaporate
and will remain in the Pyrex pot. Allow to cool.
* Take the cooled solution, pour with an equal volume of water and 1/2 volume
of petroleum ether into the ether-extraction apparatus (separation funnel).
* Allow to settle, and drain the ether extract layer.
* This leaves an ether-extract-acid mix from which the acid must be purged.
To accomplish this, pour the ether-extract-solution into four volumes of 5%
sodium bicarbonate solution (1 gram bicarb. in 20 grams of water). This
will neutralize the acid, releasing CO2 and leaving a solution of sodium
sulphate.
* Allow this to settle into layers, then drain the ether-extract layer.
* Mix the ether-extract solution with an equal volume of pure water and let
it separate.
* Drain off the ether-extract layer.
* Evaporate the ether and what remains is hash oil in which all of the
cannabinoids have been converted into THC.
Hash Oil At Home - A Connoisseur's Guide To Home Oil Extraction
A booklet purchased in Amsterdam 1996.
(No attributions or dates are given.)
Safety Checklist
1. The entire manual should have been read and the procedures and precautions understood to safely extract oil.
2. Do not attempt extractions while under the influence or after the consumption of any intoxicants.
3. Do not use any cracked, damaged, or otherwise imperfect equipment and materials
4. Store petroleum ether in a cool place (refrigerator), upright with a cap on tight to avoid leakage. Always recap petroleum ether.
5. Do not drop, spill or leave open any empty/full containers of petroleum ether or alcohol at any time.
6. Do not use, pour or set petroleum ether near, or even close to, heat, flame or sparks.
7. No matches, cigarettes, open flames or heat source should be in the room to avoid accidental use.
8. Work only in well ventilated area. Use only a sparkless fan.
9. Do not allow anyone who has not read and understands this manual in the work area.
10. Do not inhale vapors or allow prolonged contact on skin
11. Clear working area of any objects which might fall, hinder work, or otherwise be hazardous. Keep out of reach of children.
12. Test the condensing equipment and set-ups before beginning the process. Test all hoses for leakage.
13. Keep an ABC fire extinguisher within reach
14. Keep all animals away from the work area
15. Do not do this process in any area where it is illegal.
Introduction
You now have in your hands a complete and comprehensive guide to home oil extraction using a quick, simple, efficient and safe method of extraction from plant materials. In these pages are instructions for making some of the most potent oil anyone has ever smoked. It's easy, because we tell you exactly how to make it, step by step, with common laboratory equipment. We will tell you what safety precautions you should follow, and how to obtain the necessary materials.
Your oil is extracted with petroleum ether, a common solvent that is easily obtainable. It is not a real ether, but the name comes from early chemistry days. It is a mixture of isomers of hexane (low boiling hydrocarbons). Isomers are molecules with the same type and number of atoms, but which differ in their spatial arrangement. Petroleum ether is very similar to the components of gasoline and must be treated with the exact same care. You must be extremely careful when you use petroleum ether for it is very flammable and can explode if the vapors are heated in a closed system (we will have more on that later). You will see that we emphasise safety throughout the book. If you follow these instructions you will be able to safely extract all the oil you want without fear of harm. Please follow them carefully. Since we do not recommend the use of flame or heating coil for the extraction, the danger of fire is greatly reduced. Please read the section on safety carefully, and have anyone who is to participate read it also.
The amount of oil you get, and the color of the oil will vary, depending upon the pot you use. Amounts vary from plant to plant. Quality remains constant. Unlike many oil machines on the market, we do not use alcohol for the extraction. Alcohol extracts the oil just as petroleum ether does, but not as efficiently. Alcohol also extracts chlorophyll plus simple and complex sugars, while petroleum ether does not. After the extraction process your plant material will look the same as before, but will not be potent since almost all of the active components have been removed.
Concerning the safety Checklist
Safety is of extreme importance when making oil. The extraction is safe, but in order for it to be so, one must follow all instructions and precautions. Carefully read the safety precautions in this manual to insure the production of high quality oil without injury to yourselves or others. Make sure that you read the entire text, paying special attention to safety precautions, and instructions for care and storage of petroleum ether. No matter how competent you feel, do not take anything for granted. Do not overlook any precautions, and do not allow anyone who has not read this book or does not understand all safety precautions to participate, interfere or be present during production. It is absolutely necessary to observe all points of safety. So do yourself a favour, and take the time.
The safety checklist will be referred to throughout the book, so it would be wise to read it over now. the checklist, as well as the entire manual, should be read and completely understood before beginning the process. We repeat, DO NOT IGNORE THE SAFETY PRECAUTIONS!.
Procedure for making the oil
Before starting the extraction process, make sure you have read the whole book twice, carefully. Be sure you have studied the section on safety. Do not allow anyone to assist, observe or interfere unless they have read and understand the safety precautions.
The following steps are for initial extraction.
REFLUX
To set up the reflux you need one ringstand, one condenser, one round bottom flask, two clamps and silicon grease.
Place the ring stand on a stable surface. Put one clamp on the flask's neck and clamp it to the stand. Leave enough space underneath the flask to place a pan of hat water and to be able to remove the pan to add fresh hot water. The water should be at neck level on the flask.
Now carefully clamp you condenser into place (use a small amount of silicon grease to give an airtight seal). Be careful with the condenser, as it is probably the most expensive piece of equipment you have bought. Connect the hose that carries the cold water to the BOTTOM nipple on the condenser. Connect a second hose to the top connector on the condenser, and let the other end drain to the sink. Carefully fill the condenser with cold water. Make sure your connections are tight. Also, never seal the top of the condenser when refluxing. When you are refluxing, pressure is kept at a minimum by the condensing of the hot vapors, but some pressure exists. If vapors escape, reduce the heat by adding some cold water to the hot water in the pan. Do not begin heating the flask until all equipment is set up, and all petroleum ether is put away.
1. Remove flask and place material to be refluxed into it. Leave about two inches of space between top of material and the bottom of the flask's neck.
2. Take the petroleum ether from the refrigerator and add enough of it to the flask containing the plant material so that the petroleum ether just covers the material.
3. After you have put the petroleum ether back in the refrigerator, connect the flask that was just filled to the bottom of the condenser. The flask should be secured by a ring clamp to the ringstand. Make sure the condenser and flask fit well. Use silicon grease for a tight seal.
4. Turn on the cold water attached to the condenser
5. Put warm water in a bowl and place it so that the flask is submerged to about the level of the petroleum ether. Use book(s) to elevate the hot water bath in order to adjust temperatures without adjusting the height or position of the flask. The reflux process will begin as soon as the petroleum ether starts to boil. The water bath temperature should be around 35C or 110F. UNDER NO CONDITIONS SHOULD YOU HEAT THE WATER WHILE REFLUXING. Always get your hot water from another room or use hot tap water. Do not use water that is too hot to touch - it will be too hot for safe refluxing and could be dangerous.
6. A steady even boil not reaching into the neck of the flask is what is desired. If it is boiling too fast (boiling into the neck of the flask) remove water and cool it to reduce the rate of boil. If it is not boiling slowly and evenly, add warmer water to the bath.
7. Allow refluxing to continue for 45 minutes.
FILTERING THE PLANT MATERIAL
1. After refluxing is completed you may remove the warm water and replace it with ice water. This cools the ether, so it will not evaporate too quickly during the filtering process.
2. Fold filter into a cone shape. Hold filter in top of pyrex beaker.
3. Remove flask from condenser and bath. Carefully pour petroleum ether through the filter (be extremely careful not to spill any ether). DO ALL WORK IN A WELL VENTILATED AREA AWAY FROM ALL FLAMES, SPARKS OR HEAT. The filter catches all small pieces of plant material and seeds. Do not get plant material in the filtered solution.
4. Take petroleum ether from the refrigerator. Pour a small amount of petroleum ether into the flask with plant material. Shake well and pour through filter into the beaker with the rest of solution. (This insures that you are not losing any oil). Put the petroleum ether and the refluxed solution (covered) in the refrigerator.
5. Not all of the plant material will come out of the flask when you pour for filtering. The remainder may be removed with tweezers, forceps or by gently shaking the flask upside down. Be careful not to scratch the ground glass if you remove the material with any tools. Wrap the treated plant material in paper towels and place it outside in a well ventilated area where the petroleum ether may evaporate safely. Do not place it near fire, heat source or sparks. This material will dry within an hour and should be disposed of properly.
OPTIONAL FOR FURTHER PURITY
If you are a connoisseur of fine oil, and do not mind a few minutes extra work, and a few dollars more of equipment, then you will want to further purify and concentrate your oil
First, immediately following the filtration, mix about 2-3 grams of finely ground activated charcoal to your extracted solution and stir well. Make sure the solution of petroleum ether and oil is cold before starting this process. Re-filter this mixture. If all the charcoal has not been removed, repeat the filtration. It might be advisable to use regular lab filtration paper for this step. After filtering out the charcoal, you will notice the solution is less colored. (Don't worry, all the oil is still there. You have only removed the impurities.)
Secondly you should water-wash the solution. the essential oils are not water soluble while some impurities are both soluble in water and petroleum ether. Since petroleum ether and water do not mix together you can place them in the same container together and shake well and they will separate. The water soluble impurities in the petroleum ether will dissolve in the water, and then the two solvents will separate, leaving the oil in the petroleum ether and the impurities in the water.
The container used for this mixing of solvents is a separatory funnel. This is a clear, pear-shaped container. Simply pour the petroleum ether in the top to the half full level, and add several inches of water. Now close the cap, point the barrel away from your face and shake lightly. Open the stopcock to release any pressure that has accumulated inside. Close the stopcock and repeat the process, releasing the pressure between each shaking. Repeat until opening the stopcock releases no pressure. Now place the funnel on the ring clamp and remove the stopper. You will notice an interface. The bottom level is water, and the top petroleum ether. As the interface moves down, reduce the flow until the level reaches the bottom, and then quickly turn it off. You have now separated the two liquids. Using this clean and pure solution, go on to the distillation.
DISTILLATION
To set up the distillation, you need 3 ring stands, 5 clamps, 2 round bottom ground glass boiling flasks, 1 elbow connector with vacuum outlet, 1 elbow connector without vacuum, one condenser, silicon grease, plastic tubing and aspirator assembly.
Set up the ring stands in position. The flask with the filtered solution (flask A) requires the elbow connector without the vacuum outlet (nipple). The flask and the elbow joints should be independently supported by clamps connected to the ringstand. After attaching and positioning these to the ringstand, attach the other flask and the elbow with vacuum outlet (nipple) to a separate ringstand. Make sure that both flasks are tightly connected with the elbow joints and that each part is independently supported by separate clamps. The condenser should then be connected to the center ringstand. Allow sufficient room beneath flask B to remove the ice bath in order to add more ice if necessary. Once you have found an appropriate height for the positioning of flask B, you may connect the condenser to flask B. Now you may position flask A and connect it to the other end of the condenser thus closing the system except for the vacuum. You will have to adjust the positioning of flask A and the condenser to get a tight fit and to stabilize the distillation set up. N.B. THE CONDENSER MUST BE ON A SLOPE WITH FLASK A AT THE HIGHER END. Connect the hose from the water source to the lower nipple on the condenser which should be the same end as flask B. Connect the hose for the draining off of the water to the upper nipple. Connect the aspirator to the sink faucet and then connect the vacuum hose from the aspirator to the water trap. Then connect the water trap to the nipple on the elbow joint. Now turn on the water to be sure that the system is connected properly. Once the water is flowing smoothly, almost, if not all air should leave the condenser. Before proceeding make sure that your system is connected properly and is stable. (For diagrams etc see a chemistry textbook or similar on distillation).
To prepare for distillation, place ice bath around flask B up to the neck bottom. This cools the distilled ether and keeps it from being further moved into water trap by the vacuum.
Then place the warm water bath(35C or 110F) around flask A, about 1 inch from bottom of flask neck. The petroleum ether will quickly begin to boil. Do not allow the solution to boil so vigorously that it boils up into the neck of the flask or condenser. If it does, reduce the temperature by adding cold water to the pan. As hot vapors rise they pass through the adapter and into the condenser. Here the vapor condenses into droplets which collect and roll down to flask B where the ice water keeps it cool and a liquid. Note: This is only petroleum ether, not oil. The oil stays in the heated solution because it's boiling point is much higher than petroleum ether. Only ether boils away and only its vapors travel into the condenser. Eventually the ether will be entirely separated from the oil. As the evaporation process continues it causes the temperature of the solution in flask A to drop. This will slow the process of distillation somewhat but do not raise the temperature of the water bath. Just continue using hot tap water.
As the volume decreases in flask A you will notice the color of the solution darkening. As the ratio of oil to petroleum ether increases, the oil will become increasingly visible. the oil will become more concentrated and form a thick residue in the bottom of the flask. When all the ether has appeared to have boiled away, continue distilling for 5 to 10 minutes to ensure pure oil. Remove the warm water. Turn off water on aspirator slowly. Remove ice water bath and flask B. Pour ether back into original container and place in refrigerator for future use. It may be necessary to use the separatory funnel to remove any water that is mixed with the ether.
Replace empty flask B back in position. Remove flask A making sure all visible petroleum ether is gone. Allow to cool. Add about 25ml of ethanol or isopropyl alcohol to flask A with the oil. Replace flask A in position, turn on water, and repeat the distillation process. This removes any toxic impurities that may be present. When all the alcohol is gone from flask A, heat 5 to 10 minutes more to insure the purity of your oil. Dispose of alcohol in flask B.
At this time you have oil inside flask A. To remove it, first make sure all the ether and alcohol has been removed, then place lower portion of the flask into boiling water. The oil will become very thin and can be poured from the flask. You can pour the oil directly into a vial or onto aluminum foil, where it will cool and can be transferred in a more solid form.
There will be some oil left in the flask You can leave it there where it will mix with the next batch, or you can recover it if you do not plan to make any oil in the near future. If one wishes to remove the remaining oil, carefully pour 10-20 ml alcohol into cooled flask and carefully swirl it around and dissolve all remaining oil. Pour this into a round bottom corning ware dish. Place it in a well ventilated area and let it evaporate. After the alcohol evaporates, using a rounded rubber spatula, scrape out the oil and place it with the rest.
Now you have your oil and are dying to test it. WAIT!. First clean all the equipment with petroleum ether and dispose of the ether used. Disconnect all glass ware and empty all containers.
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