Some MMJ applications require greater purity and potency, so it is desirable to remove inactive ingredients like fats, lipids, and plant waxes, as well as any chlorophyll and other water solubles.
When I class chlorophyll with the water solubles, it is not in the same vein as the term is used in inorganic chemistry and is more involved. Chlorophyll itself has a polar head and hydrophobic tail, so it is mostly non soluble in polar water, but can be removed from the plant and conveyed by water as micelle.
Water also dissolves and washes away the Chlorophyll binding proteins and exposes the Chlorophyll to the solvent used. Chlorophyll is highly soluble in alcohol and slightly soluble in butane.
For further discussion of that subject, please see: http://skunkpharmresearch.com/chlorophyll-pickup-in-extractions/
Processes that use a polar solvent and reflux or soxhlet to maximize extraction, also maximize and concentrate chlorophyll, which can be a problem for some people. The poison is in the dosage, so even for a salubrious ingredients like chlorophyll, some people can get too much of a good thing, producing digestive tract upsets, with attendant vomiting, cramps, and diarrhea.
See: http://www.nlm.nih.gov/medlineplus/ency/article/002893.htm for details.
In a nutshell, many water soluble non cannabinoid ingredients come along for the ride when a polar solvent is used and water is present. While it is easier to use a process that minimizes their extraction in the first place, if that is a moot point, because you already have an extraction with excessive non-active ingredients, here are some ways to clean them up?
Filtering:
After re-dissolving the extract in ethanol or hexane, it may simply be filtered to remove the material that is insoluble. We usually use coffee filters for this purpose, or if we have a larger amount, we use a Whatman # 1 lab filter, with a vacuum assist.
If we wish to filter it further, we run it through 0.45 or 0.2 micron syringe filters, which takes out any remaining plant material, as well as any bacteria present.
Winterizing:
When using non polar solvents like butane and hexane, some non-polar waxes, fats, and lipids are extracted as well. An easy way to get rid of them is to simply re-dissolve the non-polar extraction in 190 proof (~95.5% azeotropic) polar ethanol and stick it in the freezer for about 48 hours at -18C/0F, for the waxes to coagulate.
The waxes will precipitate out of solution as the temperature drops and clump together so that they are easily filtered out with a standard coffee filter, or a Whatman #1 lab filter.
Here is what a winterizing filter cake looks like, while still wet.
After filtering, the alcohol is evaporated or vacuumed off, to leave a pristine Absolute.
Winterizing ISO, Methanol, and Denatured alcohol extractions:
Even though Ethanol is polar itself, it can still be used to remove some of the undesirables they pick up, because it is not as aggressive a solvent as Isopropyl and Methanol. By re-dissolving their extracts in hot ethanol and then placing that in the freezer overnight, some of the undesirables will precipitate out and may be filtered out.
Removing minor green coloration:
Because butane is non polar and considered insoluble in water, it is the longest chain alkane that is still slightly water soluble at 0.0325 vol/vol (3.25%). That means that a liter of n-butane will actually hold as much as 32.5 ml or mgs of water (1000ml X 0.0325).
3.25% by volume is also enough water to bring along some water solubles like chlorophyll and leave an otherwise pristine extraction with a green tint, usually light and sometimes a gorgeous electric hue.
These light green hues are easily removed without the more involved and extreme measures that I will follow up with, and is as simple as putting a jar of the oil suspended in an ethanol tincture, in sunlight or a light from a high UV source, like a grow lamp.
The UV radiation in the sunlight will quickly break down the chlorophyll and the breakdown products are amber, so the green color disappears.
Alas, UV radiation also destroys cannabinoids, but fortunately at a much slower rate, and three or four hours in the sun is usually enough.
OH MAH GAWD:
Oops! Soooo, what if the extraction is really, really messed up, or if you just want to see how purdy you can make an extract?
Sometimes bad things happens to good oil, and evil spirits need to be exorcised, or sometimes the most economical process, or indeed the only available extraction process, extracts undesirables. Fortunately there are ways to remove undesirables, though at the expense of yield and some of the other terpenes, so there is compromise involved.
Alcohol/Hexane wash:
One way to clean up an alcohol extraction, is to reduce its volume to a manageable level given your resources, and pour it in a separatory funnel to about the one third level, followed by the same volume of n-Hexane and then of water.
We use an HPLC Reagent grade for this purpose, which we get from the local scientific supply store.
Shake well and then lift the lid long enough to burp any pressure, before setting it in a stand to stratify into layers. After it has separated, bleed off the water and emulsion layer. They contain both the undesirables, and the alcohol as well, with the cannabinoids left with the hexane.
Add water again and repeat the wash step until you are satisfied with the clarity, before evaporating off the hexane, to yield the pristine oil. More on hexane purging in the subsequent process description for serious scrubbing:
To put this process into perspective, I once collected all of my pipe bowl scrapings and roaches until I had about a pint of them, and dumped that into the container of black denatured alcohol, that I had been cleaning my pipes in.
I shook the mixture well and let it soak for a day to extract the material from the roaches and scrapings, before straining it through a wire strainer and then a coffee filter.
Because I didn’t want to mess up a separatory funnel with the black foul smelling mess, I poured the solution in a 1 gallon Ziploc bag, to which I added equal amounts of water and hexane.
After shaking it well, I hung it from one corner, to let it stratify, and after it had, I clipped off the lower corner of the Ziploc bag, and by pinching it, and controlling the bleed rate, I was able to bleed off the water, alcohol, and emulsion layer, so that only the now gold hexane solution remained.
I filtered the hexane and poured that into a Pyrex pie plate, which I blew air over with a fan to evaporate off. Attached are pictures of the amber oil that I extracted.
While the black color was gone, slight ashtray undertones could still be tasted, so further refining was necessary with activated charcoal, but we will cover that as a separate subject.
I am not suggesting this process for reclaiming ashtrays, but simply to make a point.
Hexane/Saline water wash:
Joe came up with this process, which has produced our most pristine creations. It involves re-dissolving the oil in a hot highly non-polar solvent such as hexane and repeatedly washing the solution with saturated salt water until it is mint quality.
Salt water washing uses a separatory funnel as above, but we start out dissolving the extraction to be cleaned directly into hot n=Hexane, and then washing the hexane solution with saturated salt water.
The magic trick is two fold. The saline exposes any proteins hydrophobic surfaces, making them insoluble in water, so that they precipitate out, and the saturated water has no room for anything but the alcohol, which aids that process.
We start out by making four or five liters of saturated salt water in a glass (or ceramic) container, by mixing sodium chloride (table salt) in hot tap water with a hand mixer until no more will dissolve. We buy the salt cheap by the bag, using salt intended for water softener use.
We perform the salt water wash of the hexane mixture, by simply pouring the salt water and hexane into the separatory funnel together in about equal parts and shaking well and burping, before allowing the mixture to separate out into layers.
After carefully bleeding off the bottom layer of water, we continue to replace it and repeat the wash process of both the emulsion layer and the hexane solution, until the emulsion layer disappears and the hexane has bell clear clarity.
At that point we stop washing and evaporate off the hexane. While we use HPLC grade hexane, light naphtha (Pentane & Hexane) will also work for this process.
Purging Hexane:
While n=Hexane is a delightfully non polar solvent, that enables us to do some amazing things, it has two more carbons and four more hydrogen atoms in the chain than Butane, and so due to the greater Van der Waal forces involved, is not as easy to get rid of as Butane.
The most effective way that we’ve found to remove the residual hexane, is either with multiple ethanol washes, usually around three, or thin film vacuum.
To wash with ethanol, redissolve the hexane honey oil in ethanol at a ration of about 10 to one and boil off the alcohol. When it is almost all gone, do it again, and repeat, until there is no decernable hexane odor.
For thin film evaporation, we place about .200 inch of it in a six inch Petri dish, which we place in a vacuum chamber and evacuate down to 29.9 mm Hg and ~80F for 30 minutes.
N-Hexane boils at about 69 °C/ 156 °F and has a high vapor pressure, so it is easy to evaporate, but harder to completely purge. Given our 30ppm taste sensory threshold and our 130 ppm odor threshold, we can detect its presence, long before we reach levels of concern.
Because it is a simple Alkane and relatively non toxic, hexane is used extensively in food extraction, but should not be viewed as being as salubrious as mother’s milk.
The first clue of course, is that it doesn’t come in nearly as attractive a container, and the second is the MSDS information which tells us, that in excess, N-Hexane attacks our nervous system. The following is a typical MSDS Section 8:
Section 8: Exposure Controls/Personal Protection
Exposure Limits:
TWA: 500 (ppm) from OSHA (PEL) [United States] Inhalation TWA: 1800 (mg/m3) from OSHA (PEL) [United States] Inhalation
TWA: 176 (mg/m3) from ACGIH (TLV) [United States] SKIN TWA: 50 (ppm) from ACGIH (TLV) [United States] SKIN TWA:
500 STEL: 1000 (ppm) from ACGIH (TLV) [United States] Inhalation TWA: 1760 STEL: 3500 (mg/m3) from ACGIH (TLV)
Section 11: Toxicological Information
Routes of Entry: Absorbed through skin. Dermal contact. Inhalation. Ingestion.
Toxicity to Animals:
WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. Acute oral
toxicity (LD50): 25000 mg/kg [Rat]. Acute toxicity of the gas (LC50): 48000 ppm 4 hours [Rat].
As the saying goes, the poison is in the dosage, so leave us please keep N-Hexane’s potential nature in perspective, which includes never losing sight of it. Note also that oxygen in a breathing atmosphere greater than 75% pure will kill us dead!
A review of the hexane Material Safety Data Sheet shows that the oral rat LD50: is relatively high at 25000 mg/kg. At that rate it would take about 4.5 pounds to kill 50% of a population of 180 lb men.
Acute toxicity of the gas (LC50 rat): was 48000 ppm using 4 hours exposure data and the Threshold Limit Value for an 8 hour weighted average in breathing air is 500 ppm with a Permitted Exposure Limit of 1800 mg/M3 (~ppm).
The good news is that if you are out of the stink or taste, you are less than about .01% of TLV, but the bad news (?) is that although it is relatively non toxic, hexane still tastes like lighter fluid below toxicity levels, with our sensory threshold far below the Threshold Limit Value.
Not an unexpected taste treat, because as many of ya’ll know, lighter fluid is in point of fact light naphtha, which is a blend of pentane (5 carbon atom chain) and hexane (6 carbon atom chain).
Posted by Keith on May 23, 2013 at 2:50 PM
How effective would winterizing be on Isopropyl extracts? We are trying to remove the excess impurities and clean up our oil. Thanks
Posted by Skunk Pharm Research,LLC on May 24, 2013 at 10:18 AM
Winterizing with ethanol or methanol will remove some stuff from Isopropyl, but not much. The best way to clean up and iso extract, is with a non polar solvent like Hexane and a brine wash.
Posted by Jeremy on May 23, 2013 at 4:45 AM
Thank you Grey Wolf,
I did not think moonshine would be as clean as ever-clear. Thank you for your time.
Posted by Skunk Pharm Research,LLC on May 24, 2013 at 10:22 AM
I know someone making 194 proof using a 7′ compound refluxing still, so it is possible, but as you note, most moonshine isn’t that high a proof.
Posted by Bkdelux on May 21, 2013 at 7:33 PM
Man, I just want to say thank you!!! What a wealth of information this is. We’ve been extracting/purging into Pyrex on hot plate with great results but want a cleaner harder outcome. If we purge into Pyrex and then wash with 190 everclear and wash immediately with everclear we can go straight to jar and into freezer for 48 hours? Once we filter back onto clean Pyrex what’s best non-vac purge? Hot plate again at 130? Never purged winterized so how can you tell when fully purged?
We’ve been using a vaporizer pen with great results and a harder product does very well in our 510 pen with kanger cartomizer.
Thanks guys!!!
Posted by Skunk Pharm Research,LLC on May 26, 2013 at 7:47 AM
If you want a harder product without using vacuum, I would consider placing the alcohol mix in a thin film on a hot plate at about 125F.
Besides watching bubbles, I tell by taste and smell when the alcohol is gone.
Posted by jameson on May 21, 2013 at 6:19 AM
Hi thank you for all the work from the skunkpharm team.
Can a decarbed sappy oil that’s been winterized in ethanol still become shatter given enough time in a thin layer at ambient temp? or does it need to be under vacuum? Will 115f/28.5 hg be sufficient to become brittle Thanks and Peace
Posted by Skunk Pharm Research,LLC on May 22, 2013 at 6:42 PM
Decarboxylated oil won’t harden again. Shatter is carboxylic acid form.
Posted by Robert on May 17, 2013 at 1:25 PM
Where’s the resin come from…in a pipe or is it the trichromes>?
Posted by Skunk Pharm Research,LLC on May 18, 2013 at 6:47 AM
The resin is manufactured by and contained in the trichomes.
Posted by samyaza on May 17, 2013 at 5:08 AM
Hello all.
I have a ( rather ) stupid question. What would happen if I did so :
Let the plant material slowly extract in pure alcohol for a while, filter it and then add a lot of water ( maybe salted ? ) in it. How would the water-soluble alcohol, the water insoluble cannabinoids and the water itself behave ?
I suppose the alcohol + the cannabinoids would dissolve in the water at the beginning, but when the alcohol concentration will get very low after adding so much water, would the cannabinoids still be soluble ? Could they salt out in any manner ?
Posted by Skunk Pharm Research,LLC on May 18, 2013 at 6:05 AM
The cannabinoids are not totally insoluble in water, so my guess is that it would mostly make an emulsion.
Posted by samyaza on May 19, 2013 at 12:15 AM
So, the emultion could be filtered and dried ? Ethanol is a bit dangerous to evaporate at home because it’s flamable. You need to water-cool the vapors. If the emultion is mostly solid and poor in ethanol, it could be easier and quicker to extract à fatty, waxy paste. I may try to recycle molted material also. Cheap, safe recycling must be interesting.
Posted by Skunk Pharm Research,LLC on May 26, 2013 at 8:01 AM
The emulsion is washed of cannabinoids or discarded, but isn’t typically filtered and dried.
No solvent should be evaporated indoors without proper ventilation.
Posted by bob on May 16, 2013 at 4:55 PM
WHat other solvents do you rreccomend instead of hexane for refining oil with iso and water?
Posted by Skunk Pharm Research,LLC on May 17, 2013 at 8:51 AM
Pentane works well too. More expensive and easier to purge, but not as hydrophobic.
Heptane will work, but is harder to purge due to its longer chain and higher Van der Waal forces.
Posted by Brandon on May 13, 2013 at 7:53 AM
Do I need to winterize before I do a hexane/saline wash? Or does the hexane leave all the undesirables in the alcohol? Would it be good to winterize the alcohol anyway, just so i can keep using the same alcohol as long as possible?
Thanks
B
Posted by Skunk Pharm Research,LLC on May 14, 2013 at 1:45 PM
We winterize before the hexane wash.
Posted by Bill on May 8, 2013 at 2:17 PM
Does hexane remove terpenes as does ethanol? And is it true that ethanol removes terpenes? If I was to re dilute the extract in warm hexane and do saline washes as stated above will any terpenes remain? I have proper fume hood and lab glassware to try this method safely. Thank you
Posted by Skunk Pharm Research,LLC on May 9, 2013 at 5:23 AM
Terpenes are aromatic Alkene hydrocarbons, soluble in both simple Alkane hydrocarbons like Hexane, as well as a simple Alkane alcohol, like Ethanol. They are all 100% miscible in one another, including alcohol and Hexane.
The terpenes are mostly lost when evaporating away the solvent, especially the lighter monoterpenes, because they are alcohols, ethers, keytones, aldehydes, esters, and carboxylic acids, with high vapor pressures. They also form azeotropes with the solvent.
The terpenes are also not 100% insoluble in water, so the saline wash also depletes them. An extract that has undergone a brine wash in Hexane, has little monoterpene flavor left, and tastes mostly like the diterpene cannabinoids.
The best way that we’ve found to preserve the lighter terpenes, is to do a clean extraction in the first place and vacuum purge away the solvent at low temperature.
Posted by stratosss on May 5, 2013 at 2:46 PM
Do you think it might be possible to use slightly dilute isopropanol for winterizing? The thought being that iso+water could be adjusted to achieve 3.9 polarity index so it is the same as azeotropic ethanol.
Posted by Skunk Pharm Research,LLC on May 7, 2013 at 5:19 PM
Sounds like you have a good idea. I have found that 3-5% water is a good rule of thumb for winterization.
Posted by scottschwake on April 18, 2013 at 2:14 PM
Hi GW,
I do a super cold qwiso with dry ice and get amazing results very inexpensive. I use a large stainless salad bowl and a large stainless stew pot. First place a little crushed dry ice in the salad bowl place stew pot on top. Now fill void around stew pot with more dry ice and pile up the sides as high as you can pack it hard. then wrap it with towels. put 18 pints of 99% iso in the pot and let stand until iso turns viscous. I like to wait until it is as thick as motor oil I put a few pieces dry ice straight into the iso to speed this up. Then add 1 lb frozen material and stir up to 5 minutes with a few chunks of dry ice in the mix. Note after 5 mins. in wash no chlorophyll. Then one filtering through cheese cloth to get the course debries then 3 times through commercial coffee filters to get the fine sediment.Then I cook it down in a rice cooker until it stops bubbling. Amazing results every, time leaf and shake turn out clear reddish great tasting very potent oil every time. anyone else doing anything like this?
Thanks
Posted by Skunk Pharm Research,LLC on April 19, 2013 at 6:14 AM
Thanks for sharing bro! We’uns haven’t tried dry ice and Iso, but sounds like we should!
Posted by Gregory Karl Davis on May 15, 2013 at 4:24 PM
Yes, absolutely thank you! for posting this informative expose’ wow
Posted by ketabyte on April 16, 2013 at 11:48 PM
My first winterization:
I ran my bubble into a pyrex pie dish that was sitting in a hot water bath.
I then poured my everclear into the pie dish then set in freezer.
I know I should have let it sit longer but I noticed a mishap.
I purged the tane in the hot water bath too long and let it dry, then added the everclear. MISTAKE
What I should have done was blast into a pyrex measuring cup, added the ethanol while the tane was purging, stirred ALOT gently, then stuck to freeze overnight.
What I did was panic, pour out the ethanol (that didnt mix), and scrape my remainder out then, which was almost nothing afterward.
If I plan to remove said chlorophyll, lipids, fats, etc. What should I blast my tane column into (vessel)?, how much should i allow the tane to purge? whats the lowest grade of ethanol i can use? how much ehtanol should i add?
Posted by Skunk Pharm Research,LLC on April 17, 2013 at 7:33 AM
If you heat the ethanol up, the oil will dissolve more easily.
I use about a 10:1 ratio for winterizing.
Posted by Jeremy on May 21, 2013 at 6:16 AM
Hello Grey Wolf,
I can not get Ever-clear in my state but I can get top notch moonshine.Can I use moonshine to winterize my BHO?
Posted by Skunk Pharm Research,LLC on May 22, 2013 at 6:41 PM
190 proof moonshine will work or you can order Everclear shipped to you from http://www.winechateau.com/
Most moonshine is from a pot still and is less than 120 proof.
Posted by Skunk Pharm Research,LLC on May 23, 2013 at 1:14 PM
ubmitted on 2013/05/23 at 1:13 PM | In reply to Jeremy.
190 proof moonshine will work and you can order Everclear shipped to you from http://www.winechateau.com/
Posted by Tyler on April 14, 2013 at 4:33 PM
Hey SPR,
I slowly heated my extracted matter until it was soft and whip-able. Question: will prolonged heat ruin my extraction? It was over a low heat for a few hours while i waited for it to stop bubbling. Bubbling I understood was the butane evaporating. Am I misunderstanding? I was worried about the effects of prolonged heat so I removed it.
Posted by Skunk Pharm Research,LLC on April 15, 2013 at 8:33 AM
When you heat oil to purge the solvents, it also decarboxylates the oil at a slow rate and produces CO2 bubbles. The solvent bubbles are random sized and some are quite large, while the fizzy CO2 bubbbles are small and of uniform size.
Decarboxylating an oil, makes it softer and more runny, but not necessarily bad for the purpose that it was made. We typically decarboxylate all of our oil for oral application, so that it will pass the blood brain barrier and be orally active at the CB-1 receptors.
Some of the heat that converts THCA to THC, also converts THC to CBN, a sedative, so a decarboxylated oil is typically more sedative than a shatter.
We also routinely vaporize decarboxylated absolute amber, but also make some oil especially for vaporization bragging rights. We typically do not decarboxylate that oil, so as to maximize THC content, and minimize CBN.
Posted by joe on April 10, 2013 at 3:40 PM
Hi, I’ve been winterizeing my b.h.o. for some time now with everclear 175. In search of a cleaner product I tried ISO 99% and everclear 190 .Both gave me similar worse results, first when pouring my higher grade alchohols into my butane/oil solution (I let the tane burn off almost completey but not enough to get hard) ,when using the 175 everclear there is an instant seperation of butane and alchohol and once all butane is gone there will be debris in the alchohol solution. This doesn’t happen when using the ISO or the 190 everclear..the poduct comes out WAAY DARKER . The only thing I get in my filters when filtering the higher grade alchohols is a very white slime, .I usually freeze my soultion 14 hrs before filtering..any thoughts would help ..thanks
Posted by Skunk Pharm Research,LLC on April 11, 2013 at 10:17 AM
I would freeze for at least 48 hours before filtering and take it down to -18C/0F. I’ve still had waxes precipitate out after 24 hours.
Using heat will darken the solution. If you can cold boil it in a vacuum at 115F, it will stay light colored.
Posted by Kevin on April 9, 2013 at 8:08 AM
Hello Skunk Pharm Research, I had a question regarding my bho melting and sticking together to the wax paper it was stored on. I winterized my oil in an attempt to separate the oil from the paper however after the 99% IPA evaporated out today it still has a similar texture as before, is there anything I can do to salvage this oil?
Posted by Skunk Pharm Research,LLC on April 11, 2013 at 7:47 AM
Parchment paper works better than wax paper. You might try sticking it in the freezer and seeing it it separates easier frozen.
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Posted by Jeffrey smith on March 26, 2013 at 9:33 AM
Ive been experimenting with winterizing my BHO extracts, Which winterizing solvents preserved the best flavor and aroma in your oils out the 3, Hexane, ethanol, and Iso propyl alcohol?
Posted by Skunk Pharm Research,LLC on March 27, 2013 at 6:24 AM
You can winterize a hexane extraction, but you can’t winterize with a non polar solvent. Ethanol is better for winterizing than Iso.
Posted by Jeffrey smith on March 27, 2013 at 1:43 PM
Is there a certain “grade” or Purity” ethanol that you would recommend?
Posted by Skunk Pharm Research,LLC on March 28, 2013 at 8:12 AM
95.5% azeotropic ethanol works well and can be found in many liquor stores as Everclear 190 proof.
Posted by johnnyzxc on April 3, 2013 at 11:05 AM
i can only get 94% GLOBAL here in quebec alcool. will this work just as good to winterize?
more expensive than just buying straight 95% ethanol.
Posted by Skunk Pharm Research,LLC on April 4, 2013 at 6:44 AM
94% ethanol will work OK for winterization, but I would check the Global MSDS to make sure alcohol and water is all that is present. I seem to remember having done so once, and it was OK, but was unable to find one just now.
Posted by Looking for info on making RSO - Page 9 on March 25, 2013 at 2:05 PM
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Posted by Is there anything you can do with bad ISO hash? on March 15, 2013 at 7:31 AM
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Posted by arun on March 14, 2013 at 11:01 PM
I have extracted green leaves with ethanol. how can i remove the green color in the extract..plx help me for this
Posted by Skunk Pharm Research,LLC on March 15, 2013 at 8:52 AM
Some green color can be removed by setting the ethanol and oil mixture in bright sunlight, but if there is very much you will need to dissolve the extraction in a non polar solvent like hexane and wash it with brine.
Posted by johnnyzxc on March 14, 2013 at 12:16 AM
Do i need to heat the Ethanol first to dissolved the purged BHO? or can i spray the BHO directly into the ethanol and freeze for 12 hours then filter, then purge. i did not purge out all the butane and i can see a seperation of oil and ethanol in my jar. Is this normal?
Posted by Skunk Pharm Research,LLC on March 14, 2013 at 3:34 PM
Ostensibly you could spray directly into the alcohol, though I never have.
If you redissolved the BHO in ethanol, it is normal for the waxes to separate from the alcohol solution.
Posted by johnnyzxc on March 24, 2013 at 10:26 PM
I normally winterize using ethanol and i can see cogulation within 5-6 hours of a deep freeze.
this time i decided to use 99% ISO when it’s in the freezer i checked after 5 hours and nothing has solidified. will it take alot longer to winterize using 99%iso than ethanol?
i hope i didn’t mess up my oil =(
Posted by Skunk Pharm Research,LLC on March 27, 2013 at 5:00 AM
It won’t work as well as ethanol for winterizing and we use 48 hours minimum as a soak time in the freezer.
Posted by Erik on April 14, 2013 at 7:41 PM
If ethanol is unavailable, would Iso or methanol be better winterization? Assuming non-polar extraction of course! (most likely butane)
Posted by Skunk Pharm Research,LLC on April 15, 2013 at 8:25 AM
Iso will work somewhat, but methanol would work better due to the difference in diaelectric constants. Iso is the least polar, ethanol next, and then methanol.
Posted by Johnnyzxc on March 24, 2013 at 8:44 PM
I sprayed bho into a measuring cup let some of it purge and then I poured in 99% iso to winterize it. It’s been in a deep freezer for 5 hours already and I don’t see any waxes or solids. I’ve used ethanol before and I would have seen this by now. Did I do something wrong???
Posted by Skunk Pharm Research,LLC on March 27, 2013 at 4:59 AM
Iso doesn’t work as well at winterizing as ethanol and it usually takes us about 48 hours for complete wax precipitation.
Posted by MedicalCannabis Spain on March 5, 2013 at 6:42 PM
Respect as always.
Posted by CO2 Extraction and MMCs - question on how things work - Page 2 on February 24, 2013 at 8:50 AM
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Feel free to share our information with other sites, or other sites with us.
Posted by C on February 22, 2013 at 9:44 PM
WOW just wow, I’ve known about both winterizing and water washing for quite a while but have never taken the time to do it. So I took some full extracted “RSO” style 12 hour everclear soaked oil and washed it. Yuch what a lot of stuff. For the cancer patients I always left the stuffin because as far as I know it could be any combo that is making it destroy the cancer cells so, ,,,
but I decided to try this out for some pain patients to vaporize. wow.
I made a trichrome extract from straight sieved clean trichromes and it was clear and strong but when winterized that same oil is amazing.
My question now o wise ones is , 1) can sap oil be turned into shatter or is it always more liquid because it is so pure?
2) Is the “wax” BHO caused by the unfiltered out plant waxes?
3) Thanx bunches!!!
Posted by Skunk Pharm Research,LLC on February 23, 2013 at 4:45 AM
Oil can be retained in the shatter form by using low heat.
The plant waxes seem to play a part in producing “Wax”, but are not the whole answer. Not universal agreement on the subject, but it appears to me that water is forming an emulsion with the wax and oil, which turns into wax and oil hydrates.
Posted by C on February 25, 2013 at 8:26 PM
thanx ,I’m very curious as to what all the different things r that wash out. What is a low heat? 120 f,130,140,
or even lower? thanx again this is very new to me and I really appreciate the know how help.
Posted by Skunk Pharm Research,LLC on February 28, 2013 at 9:53 AM
Any water solubles and chlorophyll will be removed.
Low heat depends on the context and whether there is a vacuum present or not. 115F works in a 29.9″ Hg vacuum, while 125/140F might be required without a vacuum. It is also different for an oleoresin and a solution. In what context do you have in mind?
Posted by C on February 28, 2013 at 11:49 AM
Thanx for the responses,
First it would be in solution and as it evaporates turn more into an oleoresin. So if I run it at 140 F until it gets smaller and then put it under a vacuum at 115 F for the remainder ( using Hexane )
Then redisolve the oil in everclear and winterize it,then evaporate under vacuum again at 115 F then pour out and evaporate any solvent left will the final product be shatter ?
or will the 140 F temp cause to much decarboxalation?
I’m sure all the oil I have made so far is sap because of temps I’ve been getting the solvent off at. Good strong oil just kind of hard for people with muscle shakes etc to use easily. I’m thinking that the shatter is prolly the easiest form for them to vaporize with. Though the decarbed sap is great for medibles.
thanx and hopefully I’ll get to meet you in person sooner than later. I’ve been reading and rereading this site for a while now and I am so glad I found it. Thank you so much okay enough of that words aren’t near enough peace.
Posted by Skunk Pharm Research,LLC on March 9, 2013 at 3:43 PM
Sorry H&HN, I got behind with classes and this got buried on a back page.
If you are running under vacuum, there is no need to go above about 115F. 140F will produce a softer, partially decarboxylated oil.
If you use a large evaporation surface and keep the films thin, you can boil off and purge relatively fast. We don’t do large quantities, so a 6″ Petri dish works well in our vacuum desiccator, at 115F and 29.9″ vacuum.
At our saturation level, we pour in about 3/16 or so of liquid, and end up with a film 1/32″ to 1/16 ” no more than 1/6″ thick, after cold boiling off the alcohol, and the residuals are purged.
If it is a fresh frozen extraction of young material, it will produce a flint hard brittle extract, that fragments at room temperature when bent, and as the material gets older, or as more heat is applied, it will become more decarboxylated and softer as well as darker.
Posted by Walldawg on February 18, 2013 at 7:27 AM
So i have just started ‘polishing’ some extracts i have been getting and I have a few questions…
I am having an issue “polishing” my matter… i am working on a small personal scale and i experienced success with nice amber absolute my first two polishes and then i tried to polish another wax and it is looking really good until right at the last second when under vacuum pressure and light light heat from a heating pad it waxed back up… I am using 100% acetone as my solvent and making sure it is fully removed before trying. I have narrowed this down with my understanding to a few possible issues…
A. Is it the heat? if the heat, i used the same amount in my first two tests and it was successful but i know it can react differently with each matter
B. is it the solution? is 100% acetone from a supply store different than a lab quality acetone? Should i switch to iso? i couldn’t find ethanol where I live.
C. Is it the matter: this seems like the most likely to me but it really confuses me because the first two tests i did were a success and the material was worse off and had a visible amount of plant material in it via a blow out (but was a ridiculously good deal). so this reason also confused me because the cleaner golden looking starting concrete matter isn’t cleaning up nicely.
D. Could it be possible because the second batch of matter that was cleaner looking was bright gold wax so it might be that it has a less amount of plant waxes and undesirables but was actually just whipped and beaten to shit to much by the processor? (it also has a strange taste, harshness, smell {unpolished i am referring to here}} it will affect its ability to turn into an absolute consistency?
So i guess i want to know on a small scale is it best to do what i am doing or what recommendations safety issues can you advise me of before i try my finished product.
Posted by Skunk Pharm Research,LLC on February 18, 2013 at 9:34 PM
My first thought is Botrytis mold causing your issue. Try dissolving and filtering with a 0.45 or 0.22um syringe or vacuum assisted filtration unit. Check compatibility of your plastics beforehand to prevent dissolving them and the membrane. Cellulose nitrate and PTFE membrane are my recommendations.
Joe
Posted by Lance on February 16, 2013 at 12:27 AM
How long do the alcohol/hexane, saline/hexane washes normally take to separate fully? I’ve followed all the steps and can’t seem to get the layers to stratify with any ease. Do you recommend doing the alcohol/water/hexane wash first without any salt, and then do another step with just saline and hot hexane? or does it work if they’re combined into one step, with the salt and vinegar at the beginning? Do you usually have to wash the same oil a bunch of times to get it not black? Last thing, what do you think about using Petroleum Ether ACS/ Reagent Grade 30-60 boiling point from pharmco-aaper in place of hexane? its much cheaper. Any recommendations would be very helpful!
Thank You,
Lance
Abstract Extracts
Posted by Skunk Pharm Research,LLC on February 17, 2013 at 11:09 PM
If you are having emulsion issues decrease or eliminate the alcohol. I would add a little vinegar to heavily salted water. You still need some interaction between the layers to get stuff to partition. You just need to be able to drain off what you can tell is water soluable. As you decrease salt in the mix you get more alcohol diffusion into the water and then you can bleed that off too. When the alcohol is gone add more salt back to the solution to decrease emulsion and drain off the water. This may take several washes. I use hexane because its not soluble in water or alcohols and is reasonably non hazardous. Pet ether has safety issues that need to be addressed and ether is polar so it is soluble to some degree with water and no doubt soluble in alcohols. Which in this case wouldn’t be desired.
Joe
Posted by Lance on February 18, 2013 at 6:29 PM
Right on thanks joe! Theres not very much alcohol, most was evaporated off. We did use vinegar with the saltwater, and it did finally seperate but not very well, probably because we used petroleum ether I guess. Thats very confusing to me though because I always knew petroleum ether to be non-polar, it definitely isn’t mixing with a pure water layer. Have you ever seen the books Marijuana Chemistry or Cannabis Alchemy? They both recommend doing this process with petroleum ether…I don’t get it…? Thank you for your help, you guys have obviously put your time in on the subject!!
Peace,
Lance
Posted by Lance on February 18, 2013 at 6:42 PM
Sorry one more question. Just curious about the safety issues you mentioned with pet ether, at least anything more than possibly blowing yourself up with fumes. I assume you might me talking health risks, which worries me since I just got 5 gallons to work with
Thank you again
Lance
Posted by Skunk Pharm Research,LLC on February 18, 2013 at 9:02 PM
I was referring to explosive peroxide crystals that form with ethers. Apparently though the EPA advises that pet ether is not ether and not a peroxide forming solvent. The Lower carbon chains are still soluble or form emulsions. So same fire safety measures and general safety practices. Try high bp varieties like 60-80 for less issues. Happy extracting
Joe
Posted by Skunk Pharm Research,LLC on February 18, 2013 at 8:26 PM
Ethers aren’t all water soluble just those that don’t have many carbons. Ether is a carbon chain that has an oxygen atom connecting it in the middle. That oxygen is polar and is attracted to water. The hydrocarbons all want nothing to do with water. If there’s enough carbons it will form an interface with water if not the carbons get dragged in. The more charged ions (salt) in solution the less pull the water has.
Posted by Jake on February 13, 2013 at 6:49 PM
For the saline wash, is the hexane necessary? That is, if liquid (warm) oil was introduced to hot salt water, could that be agitated sufficiently to remove chlorophyll? Could the desirables be removed by lowering the temperature to around 0 degree c and filtering out the semisolid oil? Or does chlorophyll precipitate out of solution at low temperatures as well?
Posted by Skunk Pharm Research,LLC on February 14, 2013 at 8:36 AM
Oil is slightly miscible, but not nearly enough to wash it without the aid of another solvent. It mostly just clumps together and floats on top, with some forming an emulsion.
Separating the molecules with a solvent, allows the water molecules access to the water solubles and those things that fall out of the hexane solution.
Chlorophyll actually isn’t water or hexane soluble, though it is in alcohol and is readily transfered by water as micelle, because the molecule has one polar hydrophylic end and one non polar hydrophobic end.
GW
Posted by marie on March 7, 2013 at 4:45 PM
I have a question regarding chlorophyll extraction from my bho. I have made bho a number of times with desirable results. This last time didn’t come out so well, it came out pasty with a jade green color. I am assuming that I have chlorophyll in my extract based on my readings. I don’t have a vacuum or anything lab-like at hand, the information you provided is sound but a bit over my head. In reading your answer to Jake’s question, came my own question: would I be able to break down oil with regular 70% isopropyl, evaporate alcohol, then do hot salt water wash to bring extract to desired state and rid it of chlorophyll if indeed that is my problem?
Posted by marie on March 7, 2013 at 5:16 PM
I want to add that the process looked successful, this change in color and consistency took place when I reheated extract over warm water a few days after extracting with butane. Until then the result was an ideal amber color with a glass like consistency. when it warmed up and became gooey I started stirring. Ten minutes later, a thick, green, pasty clump was the ending product. This was a large yield with great starting material so I’m hoping to be able to rescue what I have. Could warming it over the water have resulted in this even though I’m positive none came in contact with it? Thank you for your time and know-how.
Marie
Posted by Skunk Pharm Research,LLC on March 9, 2013 at 2:16 PM
Pretty sure you can save it simply by winterizing it, but if that doesn’t work, we have more tricks.
We average about 8% loss of the raw oleoresin weight, when we winterize our own indoor strains, but a much greater loss sometimes processing donated outdoor grown material. How was yours grown?
I didn’t ask for the details of your process, because the Jade paste sounded like a one time thang with no changes in process. Might you tell me more about the material that you are using, and how you are processing it?
Posted by Skunk Pharm Research,LLC on March 9, 2013 at 2:07 PM
Pasty Jade green BHO sounds like the presence of plant waxes, water solubles, and some chlorophyll. The slight green tint is usually due to overwashing, or grinding the material too finely using a grinder such as a food processor or coffee grinder, which produces a lot of fines.
Plant waxes will cause cloudyness, so I would first recommend that you simply winterize the BHO extraction to see where you are at first. That may solve your problem.
Alas no, there has to be a non polar solvent involved to do a brine wash, so unfortunately that won’t rid you of the chlorophyll and water solubles.
Without the wax, you may still have a light electric green, but at those low levels it shouldn’t be harsh, so you might check it before processing it further. Processing it further to get rid of the light electric green, will cost you some of your terpenes, including some of the cannabinoids.
Posted by Andrew on April 21, 2013 at 10:59 PM
I’m no expert on bho, having only done a handful of small runs, but I’ve definitely turned a batch of beautiful translucent shatter bho into the kind of dull jade butter described above.
The bho was made from high grade pollen and the initial end-result clarity was top-notch, so I’m assuming the oil was low in plant fats/chlorophyll.
The transformation from shatter to paste occurred suddenly after about a week of gently reheating the oil via water bath in preparation for each use (so usually once daily). The oil wasn’t ever intentionally “whipped,” only agitated when pulling out warm stringy dabs.
Each time after use, when the oil was allowed to cool back to room temp, it would return to shatter, until one day after about a week, pulled it off the water bath and it instantly got cloudy then opaque as it cooled.
So I can attest to repeated heatings causing buttering up.
(On second thought, if using warm water baths like this frequently, could the steam from the bath be slowly hitting the oil forming emulsion?)
Posted by Skunk Pharm Research,LLC on April 24, 2013 at 3:04 PM
It may have been both the heat and steam. Old dry material doesn’t appear to autobudder as frequently as newer stuff.
Posted by Nathan on February 5, 2013 at 8:14 AM
Hey! I am into IPA washing of cannabis. And I’ve been using a syringe for filtering for a while now. But after seeing the syringe you folks have, Im wondering how I can get my hands on one! Any help would be appreciated. looking for glass.
Posted by Skunk Pharm Research,LLC on February 6, 2013 at 1:21 PM
I got our last batch off e-bay. Before that, some were gifted to us, and Joe had one or two that he dug up somewhere. Several have since been dropped and broken, so I may be off looking again soon.
GW
Posted by Sppete13 on February 17, 2013 at 8:27 PM
I have a question…. How do you operate the syringe filter?
Do you: a) dip the filter tip into the solution to be filtered, then remove filter and squirt filtered solution into desired purging vessel. b) take the plunger out of the syringe and fill syringe w unfiltered solution and push thru the filter directly into purging vessel?
I opted for “b” and it was very very difficult to push the solution thru….
Posted by Skunk Pharm Research,LLC on February 17, 2013 at 10:25 PM
Wet the filter with some clean ethanol or other solvent first. Suck the solution to be filtered into the syringe with a stainless meat injection tip. Trade tip for pre wet filter and push into a new container. Or pre wet then try as you did before. If it is still difficult dilute it more and try again. Also make sure your filter and the housing are compatibile with your solvent. Also think about filtering with a larger pore size first. Then follow up with a smaller size.
Joe
Posted by Little Trees on February 4, 2013 at 6:25 PM
Great guides here. I have a couple questions: Where can I get that vacuum fitting for vac assisted filtering? I tried searching around on some lab equipment supplier sites but couldn’t find what appears to be a very simple setup that you have.
And when you’re doing larger batches with the ethanol do you use a still for evaporation/recovery?
Posted by Skunk Pharm Research,LLC on February 7, 2013 at 11:46 AM
As I recall, ours came from American Scientific a few years ago, and yes we do recycle ethanol. http://skunkpharmresearch.com/alcohol-reclaim-still/
Posted by dysomniak on January 16, 2013 at 1:28 PM
So, I have some hexane, a vacuum chamber, and a sep funnel on the way. What I’m planning to do is extract with ETOH, then add HEX and separate. I may also winterize and/or do additional washes with ETOH/H2O/NaCl as needed. (this basic procedure was suggested to me by a chemist friend with quite a bit of experience in this *sort of* thing, but not this *specific* thing)
I’m wondering if you experts think there’s any value to starting with an NP extraction and then redissolving in ETOH if I’m going to be going through all the rest of that, or if you see any other flaws in my plan.
Posted by Skunk Pharm Research,LLC on January 19, 2013 at 9:46 AM
It sounds like you have an understanding of what you would like to do. If you want to do a np extraction before winterizing it should work just fine. You should however review our pages on these subjects to make sure you have picked up all the nuances of each before starting. Good luck and let us know how it goes!
Joe
Posted by dysomniak on January 20, 2013 at 1:00 PM
Thanks so much for the reply, I’ll make sure I let you know how it goes.
” If you want to do a np extraction before winterizing it should work just fine.”
I imagine it would, I guess I’m mainly just wondering if there is any reason I *should* do an NP first, considering I plan to end up with a hexane solution at the end anyways. In other words, is there any reason NOT to start with an ETOH extraction?
“You should however review our pages on these subjects to make sure you have picked up all the nuances of each before starting”
I’m working on it. At the moment “nuance” may be a bit too much to hope for out of me, but I’ve been doing some reading and I think I’m staring to wrap my mind around how this stuff works. If I’m not mistaken in the “Alcohol/Hexane wash” procedure described above the addition of H2O to the ETOH solution creates a microemulsion from which the HEX can readily dissolve the desirable substances?
Posted by Skunk Pharm Research,LLC on January 21, 2013 at 8:46 AM
My preference would be to extract with any number of solvents, winterize, decarboxylate, NP, decarb, NP, separatory funnel brine/EtOH/ Hexane wash, then drive the hexane off with EtOH when concentrating your final product.
Posted by Skunk Pharm Research,LLC on January 21, 2013 at 8:56 AM
The micro-emulsion helps to draw out charged and polar compounds that may remain in the extract. Some contaminates may be too hydrophobic to be in brine but once they get into the emulsion precipitate. If you vary the salt concentration or start low and move to a high concentration it will be a little more effective.
Joe
Posted by A guide on advanced BHO making. - Grasscity.com Forums on January 7, 2013 at 9:56 PM
[...] [...]
Posted by jakenm on December 15, 2012 at 6:16 PM
I’m posting this here because I think I could get some good feedback from sfr, but there isn’t a dedicated section on cold water extraction so here goes- Is there a way to limit the pick up of plant waxes in the cold water extraction process? My bubble is to a point lately that it vaporizes almost completely leaving almost no residue, and tastes much like a dab of oil, but also leaves a slight waxy coating on the lips and tongue as some oils do. I’m also considering using your method of winterizing in ethanol to remove those waxes at some point, but would first be interested to know if there is something I can do differently in my cold water process to limit the pickup of plant waxes in the first place
Posted by Skunk Pharm Research,LLC on December 16, 2012 at 9:32 AM
Alas, I know the waxy taste of which you speak, but no ideas on how to minimize it with ice water extraction. Almost 100% of our icewater extraction is just an interim step toward oil.
When I research ice water extraction myself, I find http://www.fullmeltbubble.com/forum/index.php a good resource.
Posted by Tyrelle Raymer on December 18, 2012 at 1:21 PM
So you make oil from bubble? I always wanted to try this. Pass through column?
Posted by Skunk Pharm Research,LLC on December 19, 2012 at 6:06 AM
I made all of our oil extraction with ethanol, but you can extract with a column or thermos using butane. You must pay close attention to filtration using a column, less it clog.
A proud new local Mk III Terpenator owner just ran an experiment extracting dry sieve using a 12″ column, which turned out well, so we will be doing more experimentation in that arena.
Posted by pandawashere on December 15, 2012 at 4:40 AM
Awesome writeup! Quick idea about a speed winterization… after solution is dissolved in solvent load into paint sprayer (would want it to be new never used for paint…) spray out with N2O as the air source onto a piece of glass. This results in super frozen cannabis resin almost instantaneously
Posted by Skunk Pharm Research,LLC on December 15, 2012 at 4:56 AM
Hee, hee, hee, good idea!
Posted by nate on November 28, 2012 at 8:21 PM
Please e mail me I have a specific question thanks
Posted by Skunk Pharm Research,LLC on November 29, 2012 at 4:31 AM
My e-mail addy is graywolf@skunkpharmresearch.com
Posted by sally on November 28, 2012 at 5:09 AM
I don’t put any water in when I purge. I take it from the butane machine then put on pyrex on a hot plate. Cook until butane is gone. The trim is also dry…
Posted by Skunk Pharm Research,LLC on November 29, 2012 at 5:41 AM
You don’t have to add water, as the plant material still contains some, unless powder dry, but the principle source for us has been atmospheric humidity. It freezes out in the form of ice at the edge of the evaporating pool, and then melts into the oil during purge.
The way we got around it, was to use a deep catch and evaporation container, sitting in warm water, so that the ice formation was eliminated.
Posted by sally on November 27, 2012 at 7:46 PM
Hey GW,
When I purge on a hot plate after running thru the extractor with butane, there is a this bottom layer stuck to my pyrex that is white. I scrape with putty knife first and then the last thin layer with a razor blade and it is white. Do you know what this is or why it is turning white close to the pyrex?
Posted by Skunk Pharm Research,LLC on November 28, 2012 at 4:17 AM
Sounds like water.
Posted by garrett on November 26, 2012 at 2:52 AM
I have never heard of winterizing nor performed it on my bho…should I be worried about my health with all the non-winterized stuff I have been puffing?
Do I winterize after I purge?
Does adding ethanol affect taste or mess with terpenes?
I appreciate this website immensely, so THANK YOU in advance for all your hard work!
Posted by Skunk Pharm Research,LLC on November 26, 2012 at 6:42 AM
Convoluted issue;
Are the waxes removed by winterization toxic? No.
Can they be turned into something toxic or carcinogenic if subjected to the pyrolysis of burning! Yes.
Can they coat your lungs? Yes.
Will removing them make the oil safe to burn? No, because the cannabinoids can also be converted to carcinogenic substances through incomplete combustion.
Combusting cannabis oil is not a good idea, so we prefer vaporization, at which point the issue becomes residual wax coating of your lungs, if the waxes are not first removed.
Winterizing will remove the residual butane as well, when the alcohol is evaporated off. You can skip that first butane purge step. We wash our oil out of the extraction pot with ethanol, and then stick that directly in the freezer for winterization.
Winterizing with alcohol also reduces some of the lighter mono and Sequiterpenes, when it is purged, but still leaves nice floral undertones.
We winterize most of our oil and yet when you first open a jar of oil and stick your nose in the opening for a deep sniff, it explodes with floral over and undertones, and with a little practice, you can easily tell what strain it came from, due to its distinct odor profile.
The raw oleoresin that they are made from, have even more, but you can feel and taste the wax left behind in your lungs and mouth upon exhale. A matter of taste and choice….
Posted by Alex on February 16, 2013 at 6:25 PM
Correct me if I interpreted that incorrectly, but are you saying that [in my case] after spraying into the pyrex resting above the hot tap water, one doesn’t need to apply a low-heat purge [in my case, i would have no vacuum and have yet to purchase a hot plate] and can instead directly scrape the oil and dissolve in ethanol for the winterization process?
Posted by Skunk Pharm Research,LLC on February 17, 2013 at 8:28 AM
Yes, the balance of the butane will exit when you purge the alcohol.
Posted by tilopa88 on November 19, 2012 at 6:26 PM
Thanks for the info. I just did a simple hexane process that ended up a little too green (because I left the plant matter in the hexane for 2 days), and reading your cleaning article have this question. You say you can clean your product by dissolving it in 95% ethanol and then filter out the Chlorophyll (green stuff). But if chlorophyll is completely soluble in ethanol how can it be filtered with a coffee filter or other filters? And if I did this would I not be filtering out the THC? I’m assuming THC is not soluble in ethanol?
Posted by Skunk Pharm Research,LLC on November 21, 2012 at 5:38 AM
If you already have a Hexane extraction, there is no need to redissolve in ethanol to get rid of the chlorophyll, as simply washing in brine will accomplish that end.
The reason for redissolving in ethanol and then freezing, is to coagulate the waxes, so that they can be filtered out.
Posted by sally on November 2, 2012 at 5:42 PM
I will check with my husband and have him inspect. I have a question about the Appion G5 twin. The gauge on it broke after about 20 runs. It seems to still be working and we use our own gauges. The Appion seems tempermental……. Sometimes it shuts down during our runs. Is there something we can do to preserve this machine and care for it a little better during runs and after runs are completed?
Posted by Skunk Pharm Research,LLC on November 3, 2012 at 7:13 AM
The gauges on the Appion are a joke, so I ignore them and use a good compound refrigeration gauge, that goes from 120 psi, down to -30″Hg.
My first thought is that the Appion has a pressure limit switch, that shuts it down if you exceed its limits. That will happen if you build up excessive pressure, or start drawing liquid.
I would have to look at your system set up to have any opinions on which it might be.
As far as taking care of the Appion, beyond following the Appions manual, we no longer try to pull our pots below -22″ with the Appion, instead switching to a two stage pump at that point, to reach -29.5″Hg. The Appion is not only super slow at those vacuum pressures, but it wears out the upper end seals prematurely, because they are running essentially dry of lubricant at those low pressures and butane concentration.
I had to install one $250 upper end rebuild kit in our unit, shortly after buying it, because I developed our process using it. We have hundreds of hours on it since that rebuild, with no indication that it’s performance is deteriorating.
The difference between 29.5″Hg and 22″Hg is about 25% of the volume of the pot in vapor, and with a 233:1 ratio between butane gas and liquid, the cost is less than a penny for our largest pot.
Posted by sally on November 1, 2012 at 6:56 PM
Grey Wolf,
We seem to have problems with the fitting between the colum and the pot leaking. Seems to need to be replaced every 5 runs. Any suggestions?
Posted by Skunk Pharm Research,LLC on November 2, 2012 at 5:35 AM
Are you refering to a triclamp connection?
If so, we haven’t had to replace any of ours in over a hundred runs, so I suspect you have either a mismachined gasket surface, or are not using a compatible gasket material.
What material is your gasket? We use either Teflon, or Buna N, depending on which one.
Is the machining on the two mating gasket surfaces smooth and undistorted? Any nicks or gouges?
GW
Posted by will on October 15, 2012 at 2:16 PM
I would also be interested to know what that milky white liquid is as it has shown up in several of my isopropanol extractions. I can’t imagine its bad but I’d be interested to know what it is and what causes it to form
Posted by Skunk Pharm Research,LLC on October 15, 2012 at 4:58 PM
It is caused by water.
GW
Posted by concentrait on October 15, 2012 at 4:20 AM
for winterizing, if its more like a normal house freezer, should it stay in the freezer longer since its not 0 F? also a milky white liquid formed when the everclear was nearly all evaporated, what is this and is it bad?
Posted by Skunk Pharm Research,LLC on October 15, 2012 at 4:34 AM
The lower end of most household freezers is about 0F, but longer at a higher temperature will work. In fact, if you just set it aside for long enough, it would drop out most of the waxes at room temperature.
GW
Posted by Sean on November 7, 2012 at 11:59 AM
Hi GW,
Thanks for your help – earlier this year in a forum you graciously informed me of the hexane /saline wash, in an attempt to remove neem oil from a few harvests.
My first and current batch has seen nearly 5 gallons of saline, however there still is an emulsion layer that appears between the water and hexane when my separatory funnel bleeds out nearly all the water. Initially my first reaction was thinking I wasn’t dissolving enough salt into the water to be effective, which seems partly correct, and I started using roughly 500g / liter. However, is it possible that my lack of winterizing the solution in advance is causing the necessity of so much washing? Or, do you think the emulsion layer will eventually stop showing up if I just keep bleeding it out and washing with enough saline? The solution has been filtered with a coffee filter but I was waiting for the emulsion layer to disappear before finally running it through the syringe filter.
Thank you very much for any insight, as I have a few more harvests in line =)
Sincerely,
-Sean
Posted by Skunk Pharm Research,LLC on November 8, 2012 at 7:56 AM
Hi Sean, forgive me for not remembering the forum you mention and if I led you astray on Neem oil. The procedure will remove a lot of undesirables, but is doubtul if a saline wash would be effective in removing hydrophobic oils from hydrophobic oilss.
Not sure what the emulsion is, unless there is some alcohol present. Did you use alcohol anywhere in your process?
GW
Posted by Rob on October 1, 2012 at 10:26 AM
When doing the Hexane/alcohol wash how do you prevent an azeotropic mixture from forming between the hexane and the alcohol? Or how do you reclaim the pure hexane? I tried your method and after distilling off the hexane (stuff’s too expensive for me to just evap, and not really eco friendly either) it is cloudy indicating that it has formed an azeotrope.
BTW, I love your site, it’s nice to see others doing the same type of extractions as I am and seeing how they handle the different aspects of the process.
Keep up the good work.
Posted by Skunk Pharm Research,LLC on October 1, 2012 at 5:18 PM
We prevent an azeotrope by adding salt and vinegar to the solution. There will be some comingling at the interface with the alcohol/hexane simply because the one end of the alcohol molecule is non polar (CH3-OH). I just pee it off slow out of the sepratory funnel and generally end up with a little alcohol left or a little less hexane. We attempted to recover hexane with a distilling condensor but couldn’t get it dialed in such that we didnt smell hexane fumes escaping.
I hear Greywolf has been tinkering with a stainless rotory evaporator for recovering hexane. I think we are still in the developement stages so it may be a little while before you see anything posted on our site.
We are all waiting with baited breath……
Posted by Rob on October 1, 2012 at 9:58 PM
About how much salt and vinegar do you use per… say 100ml (or some other arbitrary volume)? I’ve had good luck with my distilling setup (liebig condenser) I solved my leaking problem by Dow using high vacuum grease.
Posted by Skunk Pharm Research,LLC on October 1, 2012 at 10:23 PM
I would have to look at my lab notebook at the chemistry lab to know for certain. But I believe it was around 100g salt / liter. It was pretty time consuming to dissolve. You could probably use less. Salt makes the alcohol insoluble and exposes hydrophobic surfaces of proteins and causes them to precipitate.
What are your polishing goals if I may ask? I could help paint a better picture if I have a better view.
Posted by Rob on October 2, 2012 at 8:37 AM
My wife has Primary Spinal Stenosis (narrowing of the spinal canal) and I make her extract to smoke and for making a transdermal topical. I use a soxhlet with hexane to extract the crude and am triying to find a good procedure to wash the crude to get a purer oil. I am doing your “winterizing” procedure right now and am excited to see how much wax/lipids/etc precipitate out. And the geek in me just wants to fiddle around and try to make it as pure as possible.
Posted by Skunk Pharm Research,LLC on October 2, 2012 at 4:24 PM
I predict that you will be amazed at what drops out winterizing in ethanol and delighted with the results.
Good job tinkering!
GW
Posted by Rob on October 2, 2012 at 9:52 PM
OMG you were so right about the winterizing just finished distilling the extract. My procedure next time is going to be soxhlet extract with hexane, distill till “dry” then disolve in EtOH, freeze, vacuum filter, distill till “dry” disolve in hexane then distill and evap to leave my absolute. The reason I’m redisolving in hexane is on the equipment I have I couldn’t get the EtOH to stop bumping even with boiling chips so It’s just easier for me to use hexane as the last step. This last batch of extract now looks just like yours at the top of this page, thanks so much for being willing to share your knowledge/experience with me over the last few days.
Rob
Posted by Skunk Pharm Research,LLC on October 3, 2012 at 4:11 AM
You’re welcome! Ohmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!!!!1
Posted by Rob on October 4, 2012 at 7:56 PM
One more question for you, is your absolute after winterizing always a liquid (viscous, kinda like gear oil)? Even a room temp my absolute is a liquid, just wondering if this is the norm.
Rob
Posted by Skunk Pharm Research,LLC on October 4, 2012 at 8:42 PM
It is if it is decarboxylated as well. Undecarboxylated, it is a stiff resin, that ranges from stiff taffy to hard at room temperature.
Posted by Rob on October 4, 2012 at 9:18 PM
ok this batch was decarboxylated, I’m looking at getting my wife an Omicron vaporizer, should I decarb or not for this kind of application?
Posted by Skunk Pharm Research,LLC on October 5, 2012 at 5:06 AM
It will work either way, depending on the cart. Since you are vaporizing, it also isn’t necessary.
We use a 510 cart with the wick removed for the carboxylic acid forms, and leave the wick in for decarboxylated. The issue is that the decarboxlated will leak or run out of the cart when it is laid on its side, unless kept suspended in the wick.
Posted by Liam on September 9, 2012 at 2:37 PM
So out of the above outlined procedures, which parts need i do to polish my qwiso extractions into an absolute using everclear? Or at least remove some more of the undesirables ive been picking up (relatively little). Also I’m considering making the switch to pure isopropanol for my qwiso extractions, will i need to make any changes to my current method or is there anything i should keep in mind?
Many thanks to everyone whos contributed this wonderful information to skunk pharm, keep it up!
Posted by Skunk Pharm Research,LLC on September 10, 2012 at 5:26 AM
Thanks for your good thoughts!
An Absolute is made by winterizing a non polar extraction with a polar solvent, to remove the mostly non polar waxes and lipids.
Isopropyl is a polar solvent, so it doesn’t extract as many of the non polar elements, and technically can never be an Absolute, but can be cleaned up with Ethanol some, by simply re-dissolving the QWISO extract in hot Ethanol and then sticking in the freezer.
Often you will find that everything won’t re-dissolve in the Ethanol to start with (redish waxes), and after about 48 hours, when you filter it, some more things may drop out. That is because Ethanol is not as aggressive a solvent as Isopropyl is. Isopropyl will strip in 20 seconds, what it takes Ethanol 3 minutes to accomplish.
The best way to totally clean up a QWISO, is to redissolve in a non polar solvent like Hexane, and water wash it using brine and a separatory funnel, to remove the water solubles and the chlorophyll.
As far as switching from 99% to pure Isopropanol, I doubt that you will be able to tell the difference in either the process or the end product. There is more water than that still left in the plant material, unless you have it desiccated powder dry, which is counter productive.
GW
Posted by ExtractorMarc on August 18, 2012 at 1:53 AM
Thanks for the good info as always guys! I’m just having a tough time visualizing the Alcohol/Hexane wash… Any way to further clarify it or perhaps make a video? I have a gallon of reagent grade n-hexane, and shitloads of food-grade 95% ethanol (as well as iso and a bunch of other good shit, and all the required labware) so I’m really interested in this process to clean up my bho extractions.
From what I understand, I dissolve my bho in the n-hexane, and then add saturated saline solution to the mix in the sep.funnel, let it stratify, bleed off the saline (which would also contain the impurities, no?), add more saline, rinse lather repeat until no more impurities precipitate with the saline, and then boil off the n-hexane.
Another thing is that (living in CO) my vacuum desiccator won’t go above ~21-22inHg so I’m guessing I need to purge more and longer as well?
And would the final product be an absolute or would I still need to winterize it, or should winterization be done before the hexane/saline washes???
Again, thanks fort the info guys, keep up the AMAZING work!
Posted by Skunk Pharm Research,LLC on August 18, 2012 at 8:22 AM
Thanks for your interest and good thoughts!
Adding videos is on our project list, but we didn’t like the quality of our first attempt, so are approaching it more cautiously this time.
As we have a full plate wrapping up existing projects like the new skunk lab and Mk II Terpenator, don’t look for any until next year.
Your understanding is correct; but add “shake well”, after mixing the brine and hexane mixture, and before allowing to stratify.
Your vacuum gauge is reading relative pressure, but the actual absolute pressure would be the same. If you are using a pump capable of vacuum levels below 29.9″Hg at sea level, it will ostensibly pull the same relative pressure at any elevation.
The definition of an absolute, is a non-polar extraction, that has been winterized using a polar solvent, to remove the mostly non polar waxes.
We winterize before washing.
Peace, GW
Posted by ExtractorMarc on August 18, 2012 at 9:44 PM
Cool, thanks for clarifying everything! Can’t wait to give this process a try!
Keep up the good work!
Posted by Skunk Pharm Research,LLC on August 19, 2012 at 5:29 AM
Thanks for the good thoughts and good luck!
GW
Posted by scottie15 on August 17, 2012 at 1:44 PM
I do not know which forum is ‘Greywolf’s’ forum of choice, otherwise I would post this there.. but I came across a research paper from the University of Toronto where they use acids to precipitate chlorophyll out of canola oil (Canadian rapeseed has alot of chlorophyll). The acid/solvent ratios are close to that of the isomerization process, so I wonder if this same process can be used with hash oil without damaging the cannabinoids.
https://docs.google.com/viewer?a=v&q=cache:vwzM16J-XTsJ:www.cyut.edu.tw/~ijase/2005/IJASE%25203-2-1.pdf+remove+chlorophyll+canola&hl=en&gl=us&pid=bl&srcid=ADGEEShYZ-lbdR6c4qVNwcFk1THJDN5uH-ti3J3MKHIG3MGTXwLpsjOiKUG83tBsRe3eMJN3IO4cvj6TMJ3NWRtNLsryFRGl11SffNSvn0MgcHT7OtBwkTClpThGLFyZHEEdbLKXTbBO&sig=AHIEtbRXHV8blDgK-8n8BoctGDaAgvsSOA
I figure you guys’ll make sense of this more than I. Much appreciation for all the knowledge you are putting out there.
Posted by Skunk Pharm Research,LLC on August 18, 2012 at 7:20 AM
Thanks for the link Scottie! It look like an interesting process and my guess is it would produce a phosphate ester. Alas, I’m not a chemist so I will ask Joe, our resident organic chemistry brain trust, to review the process and make more educated observations and comments.
GW
Posted by for_science! on August 3, 2012 at 11:53 AM
Grad student here, working on a terpene extraction process for an entomology study! I just wanted to thank you, I’m trying to clean up chlorophyll and wax in my samples before putting them through a GCMS.
If I incorporate your steps into my method, is there some way I should acknowledge you if this gets published?
Posted by Skunk Pharm Research,LLC on August 3, 2012 at 12:18 PM
We understand if you are not comfortable with acknowledging Skunk Pharm in you research paper. The stigma may affect your career in the future. We would appreciate a comparative analysis of your extracts chlorophyll content before and after you perform the procedure. Our GC is not in operation currently and we would love to know quantitatively the effect of our procedure.
Posted by leo on July 2, 2012 at 3:22 PM
and how would i treat these differently? I am both interested in both using them for extraction and polishing up crappy butane products I come across.
Posted by Skunk Pharm Research,LLC on July 3, 2012 at 5:12 AM
Here is how we use them for extraction. Note the different soak times.
http://skunkpharmresearch.com/qwet-extraction/
http://skunkpharmresearch.com/qwiso/
You would use them the same for polishing, Iso just doesn’t work as well as Ethanol for that purpose, because it is more agressive.
Posted by leo on July 2, 2012 at 3:05 PM
I have easy access to 99 % iso but not ethanol. can these be used interchangeably ?
Posted by Skunk Pharm Research,LLC on July 2, 2012 at 3:18 PM
They can both be used for extraction, but not interchangeably.
Posted by jump117 on July 1, 2012 at 12:43 PM
Hey Skunk Pharm!
Posted by Skunk Pharm Research,LLC on July 1, 2012 at 1:14 PM
Glad you stopped by jump. We have been a fan of your work.
Posted by Skunk Pharm Research,LLC on July 1, 2012 at 8:48 PM
Hi brother Jump! Welcome to the Pharm!
Hope you will share some of your expertise with us! Your Absolute Amber, is an Absolute Art form!
GW
Posted by ommp pay it forward on April 6, 2012 at 10:19 PM
This is very exciting to see done. Thanks SkunlPharm for your reasearch.
Posted by Skunk Pharm Research,LLC on April 7, 2012 at 4:58 AM
Thanks, it is exciting for us to do too brother EK! Especially in retirement, without the pressures of survival clouding direction.
GW
Posted by hrpuffnstuffs on March 16, 2012 at 8:56 AM
Such an informative and knowledged filled site, everyone interested in concentrates need to take a look at this!
Go skunk pharm go!
Posted by Skunk Pharm Research,LLC on March 16, 2012 at 11:34 AM
Thanks for the good thoughts and bon appetite!