Closed-Loop Concentrates Vacumn Temps and Times

HG23 said:

Great post, thanks for that info GW. I will have to see what adapters I need in order to setup a nitrogen bleed system on my AI, I don't see a kit or anything on their website. Do you have any suggestions?

I'm not knowledgeable on what is under the skin of the different AI ovens, and understand that they aren't all created equal. If you pull the side panel or outer cover off of your oven, does it have hoses or solid fittings?

If hoses, replace them with 3/8" or larger stainless fittings and tubing. Replace valve as necessary and suggest looking at one brand like Swagelok for mating parts and assemblies, rather than mix and match.

Hook the N2 hose from your bottle regulator to the oven vent/backfill line, and set pressure at 15 psi. If you wish to sometimes backfill with atmosphere, add a tee and another valve venting to atmosphere.

Was there ever any update on that boiling point chart for cannabinoids? I remember it was under dispute.

Not on vapor points, but we did agree that 157C for THC boiling point at atmospheric pressure appeared to be flawed.

Our literature search on vapor points under vacuum was unsuccessful, so we are hoping to share more light on that by empirical testing, once our oven RSA is again available.

A

I am also interested in Skunk Pharm's cotton candy technique as it relates to purging. I have see Xtracted Labs in WA post pictures of their prepurge (cotton candy) and say it tests in the area of 40PPM before entering the vacuum oven. That, in combination with your above techniques should significantly shorten necessary time in the vac oven compared to what I'm doing now which is 2-3 flips a day and pulling as much of a vacuum as I can right from the get go. Has Skunk Pharm done any testing in this area?

It was more than our 50ppm shutoff, so we process it further, but I don't remember the number.

We just relocated and upgraded our GC with a new column, so I just added it to the list of tests to run. It would have to be a series of different samples to circumscribe the error of the sample, but we can get an idea of the general scatter.

It has never really made much sense to me to let the oil sit very long on the heat once it's quinescent under vacuum. I always see people extoling the length of their purge time and have started to wonder how much time we are wasting with 48-100 hour purges.

If you ignore C or F and look at it from the standpoint of Kelvin, you can have a better perspective of percentage of temperature rise.

Consider that the terpenes sublimate off at a relatively steady rate below their boiling point, but boiling is faster vaporization than sublimation.

If we heat the oleoresin up enough for bubbles to readily break surface tension and start to pull a vacuum, the boiling point of everything is lowered. You can lower the absolute pressure only low enough to boil the butane until most of it is gone, before finishing off in the range that you are also boiling the monoterpenes, to minimize the time spent in the high loss range.

Another thing that has been on my mind is solvent distribution throughout a slab. Watching the bubbling in my oven, the distribution is clearly uneven and probably relates to thickness as well as other factors. Since only a gram or so of oil is tested for residual solvent, it's still kind of ambiguous because the batch or slab could have been huge. Unscrupulous individuals might simply break off a gram from a thin edge of a thick slab or simply spread a small portion out extra thin to send for testing.

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justintime420 said:

seems like the most recent thread to ask this question. Its about stability I know the time it has decarbed has alot to do with how stable it will be. That being said has anyone else had the experience of everything turning to pull n snap and not stable shatter?

Yes, high terpenes, residual solvent, including water, or decarboxylation will all affect viscosity and brittleness.

we pour out at -10in/hg so no scrapes. 95 degrees on the oven multiple flips 3-4 when each side is "finished" roughly 60-90 gram slabs in the oven for about 48 hours. We dehydrate our material for 3 hours at 95 I know this decarbs it but its only for a little bit right?

Above 120F is where it starts to accelerate.

its mostly to get everything super dry and minimize our water pickup as well as lighten the color of the extract. I keep saying its the material i work with (sugar trim) but wanted to make sure it wasnt on my end.

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justintime420 said:

Thanks again gw! Tried some properly stored material from 6 months ago properly stored and turned out much better than "fresh" material that I found out was improperly stored

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thcnology said:

GDubaya Money Haha I must say since I first posted this thread I don’t know 3 months ago now I have really learned a lot about this extractor but more importantly your technique. I've ran close to 2 hundred pounds through it now just testing and everything has greatly improved… quality number 1, speed number 2… all due credit and much respect to you. I went ahead and placed the Parker filter out front of the Caresaver as well as got in touch with Isaac at VICI and have had his filter on the discharge. He said a few months back when I purchased he hopes to have these filters serviceable soon to save us all some money but so far haven’t need to replace. I’m using Instrument grade gas but feel with having this attached I’m actually cleaning it to a Research grade every cycle so… added bonus maybe? Anyway, I can't thank you enough for pointing me in the right direction, I probably know more about the use of this machine then the guys that sold it to me… and to anybody that may be thinking of buying one be sure to ask in advance about the SLA they will actually commit to or genuinely guarantee.

One thing that still alludes me… or bugs the hell outta me really and can’t seem to find a good solution to... is when I'm pulling the extract out of the collection pot...I always have an amount on top that is a melted waxy residue. Tried a lot of things with adjustment of water jacket temps, amount of vacuum on collection, and timing of vacuum on collection.

Always it varies a little of course from extraction to extraction but I'd say somewhere from 10-20% comes out like that… always on the top… the rest underneath and down the sides and bottom is more like a powder. The texture underneath reminds me more of like a pork rind than a muffin in my opinion but... I then remove this whole collection but when later I'm whisking I end up with some parts of this melted now frozen rocky material or semi-frozen waxy goo that was on top that won't whisk and the rest being this now pulverized pork rind like golden powder that I believe we're really looking for. I then run all this whisked material through a wire mesh spaghetti strainer/colander and shake this dust onto the parchment which then goes into the oven...and sure enough shatter can be had in 1-8 hours depending on thickness. The rocks or “goobers” for lack of a better term… now left behind

I've tried including them in the oven with the beautiful golden powder but then seems a longer cook time or waxiness then random spots of buddering appear… so for now I've just been setting aside.

It makes me wonder what exactly this “goop” is... or if I'm screwing something up… or if this is something we all are experiencing?

And... I hate discarding it...I suppose of course it could be cooked to something... but any immediate thoughts/ideas in Ol’ Gray Wolf's vacuum of knowledge that spring to mind before the fall of this Ol’ Mans next harvest?

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thcnology said:

Just some notes I've been taking...

These come from a variety of sources do much respect and all credit due.

Super golden Light 70 hours at 102 degrees. Darker 75-80 hours at 104 degrees.

Our extraction method ensures the same care for quality as our growing practices. We freeze the

cannabis to preserve its flavor and medicinal qualities and then run the full plant, in strain-

specific batches, through a closed loop extractor. After reclaiming the gases used in the

process, we purge the product of any residual gas particles for 12-72 hours, or even longer if

necessary. Stay tuned through the year as we move towards live plant resin extracts.

Parker C-082 Filter
Parker 303 Filter

Originally Posted by surfguy1936 View Post
hey Gray wolf so i have the C-082 filter already on my recovery pump, so with that would i be

able to clean out the tank if i just run it through. Because I have seen liquid go through the

little glass screen on it a couple times
Any of the filter dryers will work, if they are large enough and aren't already saturated. We use

an E-032 as an inlet guard for the pump and add another filter to dry out the butane.

The 082 will work until it gets saturated with water. I use the 032 for pump protection, and

would use the largest that I could accommodate for drying and periodically dry it out in a 200F

oven as needed.

We actually have a Robinair refrigerant pump and filter dryer, which pumps in a circle from the

tank, through the filter dryer, and back to the tank. It has a replaceable element, which can be

baked out to regenerate.

we used a mixed gas....

the heating vessel circulates water at 90 degrees and my recovery tank is just in an ice water

bucket. about a 45 min full recovery time for 4.5# of mixed gas
You might try dropping the 90F to 80/85F. Amazingly, the color starts at about that level.

We use 85F and get light extracts, but much more and they darken.

1. Always let sit in your oven for 30 minutes prior to pulling a vacuum. This will greatly reduce

the muffining effect and your oils will use gravity to make its own thin film.

2. Time > Temperature. Set that shit at 103, let run for 6-8 hours. Then release vacuum and let

set for 30 minutes. Take it out and flip it. Repeat. Patty flipping is just common sense for the

most part. You really don't have to go 'thin film' necessarily if you do this properly. Once your

patty stops looking like the toxic avenger and those oil on water rainbow bubbles stop bliping,

your shit is pretty much done. An extra 30 min for good measures.

3. Fabricate a dry ice sleeve around your column of your closed loop. -40c will help freeze some

plant fats and waxes (waxy membrane around trich head) and not allow them to pass through your

screen. Too much plant fat and wax will make your shatter (autobudder) over a short period of

time.

4. Do not touch your shatter with your oily ass fingers. This will cause autobuddering. Do not

fold in more than once to make a patty, or you will increase your chance of autobuddering.

5. Use a buchner funnel/lab filter and passive vacuum system to completely dewax your oils. You

have to either keep adding butane or bury the funnel in dry ice to keep your tane chilled -40c.

If you smell the wax you get off of using dual solvent winterizing process, you will notice it

smells better than your oil. If you use a single solvent for dewaxing, hte wax has no smell;

therefore, full terpene retention in the oils. Use a buchner funnel only if you want 100% wax

free shatter. You can get a good 80% out by using dry ice and a 25micron screen. You can't see

how much wax is present in your shatter until you dewax it You typically lose about 15% yield

doing this.. but if youre a connoisseur, i say go for it.

6. Stop smoking wax. Seriously. You are smoking a bunch of unnecessary plant materials in your

product. The stuff that makes you feel like you got kicked in the chest... thats WAX.

https://www.youtube.com/watch?v=E8pIiq1t5fU

7. Never turn your vacuum pump off while in the oven. Yes AI ovens have a vac-lock mechanism but

the problem is that as they hydrocarbons boil out of the oil, they release a very very very small

fraction of vacuum in your oven; thus, slowing down the purge; thus requiring you to add more

heat and longer times that make your oils dark. You simply get more action by leaving the pump

running throughout the whole purging process. This will yield you lighter oils.

8. Never let your collection vessel exceed 80degrees F when recovering your tane. Always leave

about 5% gas in your collection vessel to act as a carrier solvent for your oils. This will speed

up the cleaning and scraping times, but will lose you 5% gas (a few bucks) but lets face it..

time is money.

9. Learn how to calibrate your AI oven. It came with the instruction manual and the guys at AI

will gladly assist you in breaking down the PV/SV and what it means to your oils.

10. Safety first. Gas mask, lab coat, gloves? check. walk in lab hood that pulls 2700cfm? check.

Proper fire suppression and explosion proof equipment? check. Do not cut corners here. Lots of

people die OVER SOME WEED because they want to make money


Originally Posted by Roji View Post
Im starting to question the need for such industrial machines for these relatively sensitive procedures we do . Is there any reason we need such bulky and heavy duty units? I'm wondering if a top load plain old vacuum chamber with stackable heated shelves fitted inside would be functionally similar to these new fancy highly technical ovens for a fraction of the cost. My ten gallon vac chamber has 1.33 cubic feet. Decent amount of room.
Am I missing something here? Are heated sides really necessary after we have gone to heated shelving?
Why are you even asking rhetorically?

KISS:

Simplest single walled box with front facing door that can hold a vacuum without imploding, there's no high heat from radiant heaters to weaken it... a full size plexiglass window for a door, like the top of a stock pot vacuum chamber, would be slick.

Several aluminum shelves with adhesive backed, full coverage silicone heaters stuck to the bottoms (two or three hundred watts per shelf should be more than enough imo)

PID temperature controllers with solid state relays for each heater in a little external box

The gauge and valve 'manifold' composed of a couple of cross connectors can also be completely external with just one hole in the chamber for the vacuum plumbing entrance, or two if you want to backfill with nitrogen, etc.

Silicone heat mats, each with it's own sensor and PID controller. The only way to get perfect tracking is to directly monitor the oil temperature, IR temperature sensors should do, since this is a low temperature specific oven. They start at about $150 each,

http://www.omega.com/subsection/fixe...ermometer.html

Just mount a sensor pointed down above each heat mat.

If you place soft padding/insulation under each heat mat, the mat will tend to conform to the uneven (concave) outside, bottom surface of many Pyrex dishes. I doubt you'll find any dishes that are perfectly flat on the bottom, and it would be necessary to ensure good contact with a solid heated shelf.

For the silicone heat mats (they're called heaters,) 1.25 watt per square inch is plenty, and should be able to withstand full power in free air. Here's a Temperature versus Wattage in fiberglass heaters graph, http://www.omega.com/toc_asp/framese...ro_flexheaters

The 1.25's are the SRP Series from Briskheat, Briskheat sells direct, Grainger's also carries them, so does this place,

http://www.oemheaters.com/c-541-srp-...-wsq-inch.aspx


That, and the box and you're good to go. The window should be large enough to allow full viewing of all levels so you can adjust the action on the fly...


Of course you can also toss your oil on parchment in there, right on the heat mat. You can even mix Pyrex and parchment, why is radiant heat still even being considered?

Water Jacket Temp 85 degrees

102 degree Heat Mat BestVac

We pull at 50% clear to 100% milky, usually 12-7 days immature.

All rh levels are below 20%

also, pulling a hard vac really quick can often result in waxing. best to pull partial vacs and let the butane escape slowly. if anything, slow and steady is the better way.

So I have some facts not after digging. We have been speaking frequently with the owner of a WA company that works very closely with extracted.

The gas depends on the material. For example propane is used for older cure material. When propane is used the vibrant colors and light terpenes are retained because of the ultra low boiling point of the solvent.

They run Extraction Tek systems and csresavers. Way over priced systems they told me each set up cost 25 grand. The do not use tamesiums

They use very large pumps to bring purge times way down.

To achieve the muffin the use a warm water circulator around the pot during propane extractions and pull a super hard vac. This and a few other steps will yield the stable muffin.

We use an ETS just like xtracted, FOA, lunchbox, etc. The prepurge muffin is just hard vacuum while the collection pot is cooling after a hot water circ. The pour prepurge is accomplished one way by heating you hot water circ to 90-100F...The oil will be a VERY low residual solvent syrup that hardens immediately. I don't like the pour because you can get oil all over the pot and spend precious extraction time scraping (potentially causing nucleation).

They also do propane butane blends. It has a lot to do with how you handle and prep your material as well. We have broken the code and now producing the same caliber oil as xtracted good luck everyone.

I read 8 pages of this post, no one mentioned that shatter comes from non agatated oil. If you scrape then scrape razor, then scrape again etc, you get butter. If you blast into Pyrex let it purge to a point where it's sludge, then with a flexible spatula scrape corners and whole pan with as few smooth strokes as possible. Then let gravity run the oil from spatula to parchment , you can guide it with a razor. Once it is on parchment let it sit in oven for 30 before pulling vac. I start at 95deg Fahrenheit, and each flip I go up 1degree. After flip let sit for 20-30 before vac again. After a few days I usually end up with solid shatter. If warmed up a bit it can be flexible...no idea why pics won't post but hopefully this helps a few people...yes I don't have many posts on here...but that's cuz I really don't care to have one more thing to keep up with.

https://www.icmag.com/ic/showthread.php?t=289808&highlight=propane+shatter&page=3

I've been running an ETS with 99% pure propane from General Air out of Dillon, CO for a little over 6 months now, and I find that the yields are lower, but the product is far lighter when pulling it out. I've been purging at temperatures in the 80's and have had some awesome results, but this comes after whipping the material at 125 degrees until it turns creamy. Toss it in the 80ish degree oven, and it muffins up and turns to a glorious crumble. My best crumble test result was 96.3% THCA from some Blue Dream trim. For some reason, though, even though when I first pull it out of the collection vat and of the oven it smells great, when it comes to dabbing it, it leaves room to be desired as far as terps is concerned. Maybe they're evaporating when I'm whipping at 125?

If this same whipped material is purged at 110ish or higher, I've found it makes the material a more earwaxy material, rather than a flakey crumble. A small bit of brightness seems to be compromised when making it the wax instead.

I've tried to make shatter with propane as well, and have had decent luck. Without whipping, I've purged the hash at around 100 degrees, and gotten some rather stable and bright shatter. The issue for me has been that the shatter I make with propane auto-budders HARD after about 2-3 weeks. Had some dispensaries call and complain of this, though the auto-budder is still rather tasty. Highest test result with propane shatter was a 97.9% THCA 303 Kush.

I've thought about taking my once-run material and steam distilling it for remaining terps, then adding it to the material while I'm whipping it. Would that work with material that's already been run? Sometimes the cannabis still smells good when I'm unloading the column, so I've gotta guess there's still some goodness in there.

Tried doing some live-resin with propane, had KILLER results. Some Island Sweet Skunk for Hashish House in Pueblo turned out to be a yellow-wet-sand look, and had the best terp profile of anything I've ever blasted with the ETS. I guess they're selling it 100/g out here in CO :/ Did a shorter soak, no whipping, and a purge at about 85 degrees. About to start playing with another several loads of live resin from them this morning, any advice?

The ETS is capable of holding pressures of up to 300psi, and I've seen it get as high as 160 when I'm using it. I heat my propane tank before I release it for a soak, I've tried soaks for anywhere from 5 to 30 minutes, and I still get awesome colors. I think the collection pot is an 8", pretty tall and tough to get into.

Dispensaries like the PHO because it's bright and smelly, making it easy to sell.

Try this method for shatter, and see if never exposing it to vacuum deeper than -29.5" Hg solves the waxing up problem.

Thin film, 110-115F @ down to, but no lower than -29.5" Hg. Purge until the boiling slows to a crawl, only takes about forty-five minutes to an hour with a few grams. I raise and lower the muffin a couple of times at the beginning.

My opinion is taking the vacuum below the boiling points of the many of the oils components is disrupting the matrix.

Yeah, that's why we say wax sucks, smells good just sitting there, but dabbed it's just not there anymore...

Thanks for sharing about the propane results, I don't think I've seen any PHO at my local MMJ dispensaries. At the moment nobody in SoCal is denying what they're selling is BHO, so I don't know why they wouldn't brag about it being PHO if it was...

Btw, I came home from the Cannabis Cup with three shatters from Paper Planes, and now the third is also turning to wax...dudes get your definitions correct, you're confusing solidity with stability, here's a pic, they were all originally in parchment folds where they deteriorated, and now continue to deteriorate... I actually paid for this...why I really want to be able to continue on making my own oil for my own personal use.

The fastest way that I've found to purge propane or butane, is for the surface tension of the puddle to be low enough for the gas molecules to readily escape from strike angles shallower than 90 degrees. With the strains we tes
ted, that temperature fell somewhere around 110/115F.

Not to be confused with the oven temperature setting, as it was measured at the puddle surface itself.

The terpenes we are targeting are well below their boiling points, but sublimating off, faster under vacuum, so we want to limit how long we pump.

Heat also changes the nature of some terpenes, through processes like decarboxylation and oxidation, so another reason to minimize how much and for how long.

It is common to distribute a mixture of propane (C3H8) and butane (C4H10) (LPG) for combustion purposes.

Propane is more suited to colder environments since it evaporates at -44oF (-42oC) at atmospheric pressure. Butane evaporates at 33oF (0.6 oC) at atmospheric pressure.

The vapor pressure of a mixture of the two products are indicated in the table below:

Vapor Pressure (psig)
Mixture Propane (C3H8)
(%) 100 70 50 30 0
Butane (C4H10)
(%) 0 30 50 70 100
Temperature
(oF) -44 0 0 0 0 0
-30 6.8 0 0 0 0
-20 11.5 4.7 0 0 0
-10 17.5 9 3.5 0 0
0 24.5 15 7.6 2.3 0
10 34 20.5 12.3 5.9 0
20 42 28 17.8 10.2 0
30 53 36.5 24.5 15.4 0
40 65 46 32.4 21.5 3.1
50 78 56 41 28.5 6.9
60 93 68 50 36.5 11.5
70 110 82 61 45 17
80 128 96 74 54 23
90 150 114 88 66 30
100 177 134 104 79 38
110 204 158 122 93 47
1 psi (lb/in2) = 144 psf (lbf/ft2) = 6,894.8 Pa (N/m2) = 6.895x10-3 N/mm2 = 6.895x10-2 bar
Note that the evaporation temperature is not the only parameter that influences on evaporation of the propane butane mixture. Evaporation requires heat and if the heat transferred to the liquid gas is limited - the liquid cools down and the evaporation is reduced.

Larger consumers requires heat exchangers fueled with hot water, electric heater or combustion of the propane butane mix itself to supply the evaporation heat.
Smaller consumers requires propane butane mix containers with efficient heat transfer from the surroundings. By example - composite containers provides less heat transfer compared to steel containers and may cause problems at lower surroundings temperatures.

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sr_bho said:

Hi all,
There's been some cool tech notes here and tips. Always nice to see what's happening with others and good luck thcnology with your new hobby. From personal experience it the best!!

Here's one i just thought of - Do you really need to fill the tube full of material? i.e. if the tube was only 3/4 full, would that affect the extract process in a close loop system?
Logic tells me it wouldn't matter?? Anyone tried?

Cheers

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coldcanna said:

@gray wolf- What is the life expectancy of butane in your system, I imagine there must be some degradation of it overtime where you must dump and recharge?

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