GrapeStreet Frost Hash

This is my photolog of an extraction process I've been tinkering with. This is my third run with this method. My knowledge comes mostly from members of this site.


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oldskoolgrower
AugustWest
Hashmouf
Edit: Smoove - I can't believe I forgot! Reading the Martini Hash gave me the initial idea. Totally deserves the credit.
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Cheers, guys. Thanks for being. This bowl's for you.


"Purple Kush"

On to the journal.

Set Up

4 Pyrex dishes - $5.00+/ea. = $20.00
The square ones seem to be easier to scrape. Straight edges, straight razor...makes sense.

99% Isopropyl Alcohol - $2.00 (x2)


Reusable coffee filter - $1.78
A normal paper coffee filter will not let resin glands pass through. And a bowl to set it in when I'm not using it.Razor - $0.33/ea. (10x$3.29)


25mL Pipet- $10.75

Turkey Baster - $1.00
Attached to the pipet with tape to provide controlled suction, though a more permanent solution would be better; if alcohol get up into the baster, the unit must be cleaned and rebuilt.

17g Afgoo Includes buds and trim. stems separated for another experiment.


"The Set Up"

Total Setup Cost - $36.82
Total Process Cost - $4.00/oz. (?)

Frost Hash

Chop - Pulverize your buds. I used a small food processor.




Wash - Place the bud pulp into the coffee filter, set it into a pyrex pan (small one) and pour about 8oz of Isopropyl (1/2 of a 16oz. bottle) over the buds. Soak as much as possible and let the alcohol drain into the dish.



Repeat - For the second wash, I agitate the buds by swirling the filter and use the rest of the iso in that bottle.

For the third wash, the second bottle is slowly poured off into the third dish, then press down with the back end of a spoon to strain the pulp dry.


"Wash trays in order: 1, 2, 3"

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Note: I scoped the pulp with an optic loop at this point and while much of the THC is gone, there are still small glands clinging to the leaves, so I'll be running another batch with this same bud tomorrow, reusing the alcohol from this run.
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Freeze - Alcohol can't freeze when put in the freezer, but oil can.

I placed the dish near the front, propped up on one end by some hamburger meat so the liquid collected in the "v" of the lower side's tilted corner.


Notice the resin solute in the "beach" near the top and increasing towards the deep end.

The dish is in the freezer, and I'm hittin' the sack. Tomorrow, I'll separate the waste from the resin and purge.

Edited by GrapeStreet, 18 July 2010 - 04:21 AM.

Not the easiest method ive seen, but wondering whats up with puttin it in the freezer.. ill wait

waitin for more

Yes!!! hahaha you are quick man, i think it was...yesterday you said you were gonna put up a guide w/ pics hahahaha. Im very interested to see the final results here!!! My qwiso stem n shake collection is nearing a quad here, about another 7-8 grams and im gonna try this if it works!!

Can't wait man. I've got a batch of standard QWISO drying right now, myself. Should be good stuff too. Think I got the wash perfect with this batch.

Anyway, very excited to see this. Always looking for better ways to get fried, and I know you know your shit. How did your first two runs go? Above average quality?

The first two runs were ok, though I didn't have 4 trays so it ended up being 2 tiers quality.

The good tray was a nice medium amber color, close to the consistency of kief. Very high potency, scoping revealed few contaminants. When packed, it kept its lighter color and a marbled consistency, breaking apart into chunks and sheets.

The first time, the second tray ended up being green-black, smelling horrible, and smoking worse. The whole tray was discarded.

The second time, the second tray was darker and when it was scraped, it formed the quintessential black gum hash that I'm used to. Black, but brown when thinned or stretched. Smoked well, bubbled when melted. It's the kind of hash that makes your bowl burn slow and smoke forever.

I don't have my nice metal packer anymore, just my 1 drum, no caps plastic packer (does its job). Think I'm going to order one today. I find it the best tool to isomerize the hash. I know my potency would be higher if I could go through that process as well. Maybe next round. For this round, I'm thinking of baking it in the pyrex after it's been purged.

Camera's charging. Then I'll finish up the phlog.

This is the first wash after cooling overnight. The separation of solid material on the bottom is more pronounced.




Decant - Using the pipette, I removed the alcohol from the top layer of the solution, careful not to disturb the sediment on the bottom. The removed alcohol was put into the 3rd wash tray.








This is the 3rd tray with the excess alcohol. Notice the greener hue and little sediment.

I don't have a background in science, though I am scientifically minded. My hypothesis is that the cold temperature is freezing the oil (or at least condensing it), which falls out of solution to the bottom, while other solubles like chlorophyll and wax stay suspended and are removed by decanting.

I'm looking for solid information on this topic if anyone's got references.

So both trays are back in the freezer while I take care of some other things. Will decant the last little bit then purge tonight.

First tray, purging. I removed the line of green from the top and returned it to 3rd tray.


Second tray purging.


Third tray, a combination of the decanted liquid and the third wash of the buds. Very little sediment, even after chilling.


so...I mixed the original bud material back into it to see if I could get a max yield from the buds, even if the second batch here will be much lower quality.





After the first tray was evaporated, it was frozen again, and then collected while cold. It took about 10 seconds to scrape it all together.

Total weight for the first quick wash = 0.5g

I'm disappointed with the weight, but the quality seems excellent.


I also got a little bit of blond from the fourth tray, which was used as a transfer bowl.

This is a photo of the first collection from the 3rd tray, it's currently chilling along side the rest of the 3rd tray. I've noticed sediment in the rest of the 3rd tray so I'll decant/filter it again.

It seems like the waxes float to the surface while purging. With this small a run, it'd be tough to skim it off, but with a larger batch or, ideally, a separatory funnel, I bet you could get most of the waxes separated too.

It seems the waxes precipitate as the solution warms and the alcohol evaporates. It forms small islands on the surface which can be gently moved around by blowing.


And here's the 2nd tray purged. Beautiful blond. Couldn't be happier with the quality of this!

Look at that color and texture. Mmmhmm. Again you can see the green ring around the "beach" on the back of the tray. I'll be sending this to the 3rd tray as well.

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This makes me think my first wash wasn't fully purged, so I'll be chopping it up and letting it air out today, see if I can get the same quality from it.

Edited by GrapeStreet, 26 June 2010 - 09:54 PM.

For the 3rd tray, I'll be trying to purify the muddled mix using freeze distillation. This is the first time I've tried this, so wish me luck.

Freeze distillation is a term for a process of enriching a solution by partially freezing it and removing frozen material that is poorer in the dissolved material than is the liquid portion left behind. Such enrichment parallels enrichment by true distillation, where the evaporated and recondensed portion is richer than the liquid portion left behind.

Except in reverse. The enriched material is what I'm trying to get rid of.

I'm going to split the 3rd tray in two, one of which I'll run through the same process I've been doing, the other, I'm going to dilute with water, then freeze.

My hope is that the resin will sink, the water on top of it will freeze and the alcohol and waxes will float, creating a barrier for me to extract the alcohol containing pigments and waxes that remain in the alcohol. I'll then double-boil the water off.

Gotta go pull some weeds and burn some rubbage. Be back later.

For the 3rd tray, I'll be trying to purify the muddled mix using freeze distillation. This is the first time I've tried this, so wish me luck.


Except in reverse. The enriched material is what I'm trying to get rid of.

I'm going to split the 3rd tray in two, one of which I'll run through the same process I've been doing, the other, I'm going to dilute with water, then freeze.

My hope is that the resin will sink, the water on top of it will freeze and the alcohol and waxes will float, creating a barrier for me to extract the alcohol containing pigments and waxes that remain in the alcohol. I'll then double-boil the water off.

Gotta go pull some weeds and burn some rubbage. Be back later.

That last batch looks great bro. I'm interested to see the results to see if dilution helps. Good luck post some more pics for us

Grapestreet,

I'm reading the first post thinking WTF until you make mention of alcohol not freezing, like a mental hand grenade. All made sense after that. Reminds me of how the settlers made applejack out of hard cider in the winter.

Gonna give this a shot. Happy hashsmoking.

Yea, this thread started after I posted a question here about cold + decanting.

It's at the heart of bubble hash method, which has become more popular around here than the iso due to perceived quality. Resin is heavier than water, and when cooled, separation of solutes by density is inevitable. The resins fall through the bag screens, collecting when they cant go down any more through the filter. And so...the magic of bubble hash, a relatively simple method, and a crude execution thereof.

This is in truth the testing/learing stage of a larger project. I'm looking into getting some graded silk screens and building what I've called a cascade distiller. It's like a bubble bag system, but improves on the design, adding surface area and tension to the screens, and in stead of a soak+stir method for the cold and agitation, it's a cycling system. Perpetual distillation instead of batch distillation.

The idea behind it is to use chemical, thermal and mechanical distillation in a looping system that separates each grade out. A tower is constructed with shelves for drawers, the drawers are 4 sided with a particular mesh of silk screen stretched over the bottom that gets finer towards the bottom of the tower.

Collection of solvent from the bottom of the tower is pumped up and cooled (or heated?), then sent back through the plant material at the top of the tower, repeating the cycle. The drawers allow lots of surface area and ventilation, making purging very quick and collection easy.

This is still in the research stage. And I'm experimenting with results from both vaporized and chilled alcohol to see if it makes a difference and if I can implement the research.


Some of this batch may be mixed in with an oil extraction from a Chocolate Mint plant for flavor/volume. We'll see how that goes.

Edited by GrapeStreet, 27 June 2010 - 03:32 AM.

Third tray purging. I got all the green out! I am amazed at how much was in this tray. When I first chilled it and looked, I could barely see sediment, but after decanting, it's clear there was more in there that I thought. This is what was recovered from the big green jar of goo. I think I'm going to go all out and soak the buds in the alcohol overnight with occasional agitation. I want it all man...leave no trich behind!


Left:Tray 2, Right:Tray 1, Center: Tray 4 (transfer tray)

I don't know why Tray 2 looks better. My guess it it was left overnight to air dry, while Tray 1 was frozen after I detected no more vapors. And why Tray 2 has more is beyond me too. I thought the first tray would be the best yield and quality. Turns out it was the second, and the finest quality seems to be what was left in the transfer tray, further supporting my theory that removing as much alcohol before purging will give the best results. This tray only held liquid being transfered, meaning it had a very small amount of alcohol in it when it dried., the resulting hash is very light in color and very fine texture.

Edited by GrapeStreet, 27 June 2010 - 04:26 AM.

Here's the first recovery from the green jar.



The second recovery is purging.



These last two extracts came out of this! It's almost completely opaque now after soaking for 24 hours. There's still trichs on the buds....


And I've mixed 75ml C3H8O + 50ml H2O which is freezing now. Who knows...I sure don't.

Enjoy the day GC.

Looks good. I'd gladly smoke some of that!

Freezing in this scenario would begin at a temperature significantly below 0. The first material to freeze would not be water, but a dilute solution of alcohol in water. The liquid left behind would be richer in alcohol, and as a consequence, further freezing would take place at progressively lower temperatures, and the frozen material, while always poorer in alcohol than the (increasingly rich) liquid, would become progressively richer in alcohol. Further stages of removing frozen material and waiting for more freezing will come to naught once the liquid uniformly cools to the temperature of whatever is cooling it. If progressively colder temperatures are available, the frozen material will contain progressively larger concentrations of alcohol, and the fraction of the original alcohol removed with the solid material will increase. In practice, unless the removal of solid material carries away liquid, the degree of concentration will depend on the final temperature rather than on the number of cycles of removing solid material and chilling. Thermodynamics gives fair assurance, even without more information about alcohol and water than that they freely dissolve in each other, that even if temperatures somewhat below the freezing point of ethyl alcohol are achieved, there will still be alcohol and water mixed as a liquid, and at some still lower temperature, the remaining alcohol-and-water solution will freeze without an alcohol-poor solid being separable. In practice, while not able to produce an alcohol concentration comparable to distillation, this technique can achieve some concentration with far less effort than any practical distillation apparatus would require.

I thought this might be the case. The alcohol+water will not freeze until lowered far below 0C, and will never fully separate.



However I've noticed greater separation of the pigments towards the top 1cm of the flask and the sediment is collected on the bottom, so I did succeed in increasing separation and concentration of some of the waste. This will be decanted again and the remaining sediment purged.

However now that the hash is mixed with water, I'll need a heat source to purge quickly, and I doubt the yield will be decent enough to justify the extra steps. I just can't stand the thought of throwing away good trichs!

This will be the 5th extract from the same pulp material.

I'm considering purging the bud pulp and kiefing it...yeh...i'm might be crazy.


Here's the second recovery of the green goo. Quality is slowly decreasing and it's a much smaller yield.

Edited by GrapeStreet, 28 June 2010 - 03:24 AM.

Does all the extra work make any of it worth while? that's what Im wondering...


Maybe a control batch with the same quality trim/bud , One way doing a normal quick wash and air cure , and then your way, and smoke up to see the quality changes , but then factor in your time spent doing all the freezing to see if Its worth it..

good concept, Ill keep watching.

Does all the extra work make any of it worth while? that's what Im wondering...


Maybe a control batch with the same quality trim/bud , One way doing a normal quick wash and air cure , and then your way, and smoke up to see the quality changes , but then factor in your time spent doing all the freezing to see if Its worth it..

good concept, Ill keep watching.

I've been doing regular 2 tray quiso for awhile and I've never gotten quality like this. Even the first tray ends up with at least a little bit of 'tar.' I've actually been thinking maybe this method produces too pure of hash...I haven't heated or pressed it, but it cant be molded or rolled up. I cant even touch it, it's just powdery and sticky.

I will see if I can do a photo log with a control batch to show the difference. I've got some nasty underbrush nuglings that are drying out now.

I've also never been able to get multiple extractions without coming up with foul black gunk on the later runs. I've only smoked out of the first wash tray, the second always seemed to be to gross.

The method definitely works. This run took a while because I've only got 1 tray that can fit in the freezer and did 5 extractions. It's more work, but I mean damn, blond hash out of that black-green garbage jar...it works!

Just takes patience and 3 minutes decanting. Without the photos, the process would have taken less than 5 minutes a day after the initial batch. Most of it's just waiting time.

I was thinking you could maybe use a gravy dish to pour the trichs off the bottom, might be quicker than decanting. Or just use a spouted jar to freeze in, then pour off the top. Wouldn't be quite as pure as this stuff, but it'd work just the same.


I think the key here is removing as much alcohol as possible before purging. However you do it, that seems like it's the reason it's so pure.

I know I certainly wouldn't have gotten as much had I just washed the buds once. I've gotten about as much from the 3rd-5th runs as I did in each of the first two, which is where I would have stopped on a normal qwiso tray. The rest would have ended up in tray two, with all the black goo.

Edited by GrapeStreet, 28 June 2010 - 08:41 AM.

After drying and kiefing what was left of the bud, I ended up with roughly the same amount of kief as I got hash. I'm sure it's a lower quality, but I'm not complaining. It still looked damn good through the scope. I think I got all the trichs, I can't find any more.

Goes to show though, qwiso leaves a lot behind.

I put 3 test piles on the small pyrex in the toaster at 220F; some tar-hash mixed with the blond, some blond, and some kief to decarboxylate.

Anyone know the melting point of THC? Not the boiling or vape point, the melting point.

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I also decanted the separated green layer from the flask.

The top green layer was thin, like the alcohol, but the middle layer was almost gelatinous, and I noted floating pockets of what I can only imagine is the chlorophyll and wax, hovering in the middle layer. Coagulated is the best term I got for it.

After decanting, there was still debris in the middle layer, so I added enough water to fill it up. this caused an instant reaction in the still freezing cold flask. A thin green layer instantly appeared at the top of the flask, and the middle layer turned milky white.

No joke man, it's some mad science shit. Even has condensation vapors dripping from the outside. I'll get a photo tonight.

My theory is adding the water diluted the mix and raised the freezing temperature of some of the water, which partially froze making the opaque white but remained a liquid because of the alcohol.

It's jello water!

But, it totally separated the waxy green layer from the bottom of the flask, and the white layer is much more viscous and thick, like oil in water.

Edited by GrapeStreet, 30 June 2010 - 05:35 AM.