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#11
Old 03-22-2018, 05:20 PM
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Ethanol does a great job at extracting terpenes, but it is hard to retain them without switching to a lower BP solvent. I like to do a saline scrub of ethanol extracted material in pentane. It removes water solubles, and purges much more easily. If you take your time, you can drop out some chunky THCA crystals. I have made some impressive terp sauce from extracting terpy material with ethanol and moving to a lower BP non-polar solvent.
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#12
Old 03-23-2018, 10:39 PM
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Quote:
Originally Posted by HashoftheTitans View Post
Ethanol does a great job at extracting terpenes, but it is hard to retain them without switching to a lower BP solvent. I like to do a saline scrub of ethanol extracted material in pentane. It removes water solubles, and purges much more easily. If you take your time, you can drop out some chunky THCA crystals. I have made some impressive terp sauce from extracting terpy material with ethanol and moving to a lower BP non-polar solvent.

Could you give a link to this process or a step by step here? Are you saying that your using hexane to separate the terps/cannabinoids out of solution in ethanol? I step by step would be amazing, thanks.


edit: so i looked into what you are referring to; liquid liquid extraction. i assume you're using a seperatory funnel. what is your ratio for hexane vs ethanol?
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#13
Old 03-23-2018, 11:49 PM
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Would love some more details about the process as well. I found these interesting in some web searches:

https://www.scribd.com/doc/7389231/L...ar-Attractions

https://patents.google.com/patent/US3575818
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#14
Old 03-24-2018, 01:37 AM
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Have anyone tried adding water to their extracted ethanol solution until all of the hash oil precipitates into little emulsified bubbles then filtering out the precipitate from the water/ethanol solution? I have, but so far the only gear I've used to recover cannabinoids from precipitated water/ethanol solution successfully is internal biological equipment.
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#15
Old 03-24-2018, 03:37 AM
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Quote:
Originally Posted by HashoftheTitans View Post
Ethanol does a great job at extracting terpenes, but it is hard to retain them without switching to a lower BP solvent. I like to do a saline scrub of ethanol extracted material in pentane. It removes water solubles, and purges much more easily. If you take your time, you can drop out some chunky THCA crystals. I have made some impressive terp sauce from extracting terpy material with ethanol and moving to a lower BP non-polar solvent.
Quote:
Originally Posted by coldcanna View Post
Could you give a link to this process or a step by step here? Are you saying that your using hexane to separate the terps/cannabinoids out of solution in ethanol? I step by step would be amazing, thanks.


edit: so i looked into what you are referring to; liquid liquid extraction. i assume you're using a seperatory funnel. what is your ratio for hexane vs ethanol?
Cannabis Alchemy by D Gold (the link will open by using the trick in my ICMAG Signature)

Notes: the low boiling point (30-60C) petroleum ether referenced is mostly pentane with some hexane, pentane or hexane will work.

Separating the layers with a jug is an improv on the use of a formal separatory funnel.

https://calgarycmmc.com/E-books/E%20...0D.%20Gold.pdf

Step 6: Purification
Oil produced using this method is quite potent, but still contains substances which give the oil its taste, smell, and color. These are sometimes very pleasant to smoke, and they are sometimes left in the oil. Removing them, however, greatly increases the potency, but decreases the yield proportionally.

The oil from the extraction is dissolved in five times its weight of alcohol and poured into an equal volume of water in a large glass jug with a screw-on cap. All solvents used are cold or cool. A volume of petroleum ether equal to half the volume of the water used is added. The screw top is tightened and the jug is inverted. The jug is turned upright immediately, and a few seconds later, when the mixture has run down the sides of the jug, the screw cap is opened slowly to relieve the pressure. The inversion of the jug is repeated about twenty-five times, which releases the pressure each time, and then the jug is allowed to sit for about half an hour. The mixture of liquids will separate into three distinct layers. The bottom layer will contain water, alcohol, and the substances in the oil (tars and resins) that are not soluble in petroleum ether. The thin middle layer is an emulsion of waxes, ether, and air bubbles. The top layer is the purified oil dissolved in petroleum ether.

The jug is fitted with a two-holed rubber stopper, glass tubing, and rubber hose. Two pieces of glass tubing are fitted into the two-holed rubber stopper. (Injuries when cutting and fitting glass tubing are frequent—cut ends are always fire-polished and hands must be protected when any force is used in fitting the tubing.) One piece of tubing need only protrude from the stopper an inch on each side. The other tube is positioned so that when the stopper is tightly fitted to the jug, the tube extends into the mixture to a half-inch from the bottom of the ether/oil layer. The other end of the tube is attached to a length of rubber tubing to transfer the ether/oil solution to a collection jug. The end of the tubing must be lower than the end of the tube in the ether/oil solution in order to obtain a siphon action. A short piece of rubber tubing is fitted to the short glass tube, and air pressure is applied to start the siphon.

The glass tube is spaced a bit above the emulsion layer; any ether/oil solution not removed will be recovered later. The ether/oil solution in the collection jug is saved. Another volume of fresh petroleum ether is added to the extraction by inverting, separating, and collecting the ether solution, which is added to the first ether/oil solution. This process is repeated until the ether layer remains clear after inverting. This indicates that the ether-soluble oil is totally extracted from the alcohol-and-water layer.
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Best to Worst Canned Butane List
https://www.icmag.com/ic/showpost.ph...6&postcount=28

Cannabis Alchemy by D. Gold
https://calgarycmmc.com/E-books/E%20B...0D.%20Gold.pdf

Hash oil techniques and solvents for non BHO hash oil?
https://www.icmag.com/ic/showthread.php?t=338633

Solvents listed as to polarity
https://www.icmag.com/ic/showpost.ph...&postcount=162

The Truth Machine by James L. Halperin (free read provided by the author)
https://coins.ha.com/information/ttm.s
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#16
Old 03-24-2018, 08:17 PM
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I recover my ethanol extract down to a syrupy consistency. Then, I mix in 3 parts pentane (I prefer pentane over hexane because of the lower BP and its less toxic) to the oil. I like to scrub with saline solution and with water from PH 4-9 to drop out water solubles with my last wash at PH7 to neutralize the solution. I like to scrub in a reactor, and then move the solution to a sep funnel to separate out the last of the water. Then you can roto down to super-saturation levels of solvent and you can put it into vessels for crystallization or pour into a thin film for slabs.
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#17
Old 03-24-2018, 08:29 PM
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Quote:
Originally Posted by HashoftheTitans View Post
I recover my ethanol extract down to a syrupy consistency. Then, I mix in 3 parts pentane (I prefer pentane over hexane because of the lower BP and its less toxic) to the oil. I like to scrub with saline solution and with water from PH 4-9 to drop out water solubles with my last wash at PH7 to neutralize the solution. I like to scrub in a reactor, and then move the solution to a sep funnel to separate out the last of the water. Then you can roto down to super-saturation levels of solvent and you can put it into vessels for crystallization or pour into a thin film for slabs.
Fantastic info! Thanks for sharing! Just curious, what kind of reduction of yield do you see with this process vs a straight purge from syrup?
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