Water Extraction Drying Techniques

[jayjayfrank]

If I am correct RiverRock said they use fresh plants flash frozen to make the water hash, then they used sublimation to remove all moisture from the frozen extracted resin, but anyone can do this I suggested it years ago. The real secret is real low heat to preserve the terpenes, sublimation as well as the fresh plant extracts.
-SamS

I have not seen them but Bubbleman did take a few photos he will post them. The 3rd place was pressed really great piece it will shatter if dropped on a table or floor. The first was rock hard glue, the second was dry sift unpressed, but all squashed up not so free flowing, so the pictures are not like last years winner.
-SamS

Try sublimation to remove all moisture from the extracted resin when frozen. Less heat.

-SamS

Hey Sam!

Sorry to dredge this up after so long has passed, but your suggestion intrigued me and I can't find any information on it, so I figured I'd go to the source...

I am a Prop 215 patient and do ice water extractions as frequently as I have time. I was working with some fresh frozen material a couple weeks ago and, while the results were absolutely amazing in every respect (taste, melt, effect, etc.) a lot of the product came out in such a sticky, putty-like state that all my normal methods for increasing the surface-to-air ratio to ensure even and effective air-drying proved ineffective. Once air dried, the product still turns to insanely sticky goo after a few seconds of body heat contact. As a result, my sturdiest efforts to pass it through a sieve, a micro plane, even to cut it into small pieces with a knife were unsuccessful. I even went so far as to freeze it, freeze my microplane, and then try to plane it in the freezer. But even the heat from my gloved hand in a cold environment was too much to maintain a workable composition.

So I'm sitting with my patty on ice trying to figure out how the hell to process it without it molding up on me. Then I find your post at the end of this informative thread and go on to look up information on the process of sublimation, which, as I have come to understand it, is the active process in freeze-drying where bringing the material's temperature way down and then decreasing pressure using a vacuum pump causes the frozen water particles to instantly vaporize and be removed from the material.

This seems like a brilliant idea for drying ice water extractions! Compared to air-drying, even in a humidity-controlled environment, it seems like you get a much more complete, consistent drying effect while also maintaining extreme cold to preserve all the volatile terpenes. Surprisingly enough though, I can't really find any information outside of your post that would suggest anyone has actually tried such a method. Do you have experience doing this? If so, how have you found the process and what equipment did you use? Any extra information would be very helpful, as I'm finding basically nothing!

Sublimation :
Definition: Sublimation is the term for when matter undergoes a phase transition directly from a solid to gaseous form, or vapor, without passing through the more common liquid phase between the two. It is a specific case of vaporization. The most well known example of a material that undergoes sublimation is dry ice, or frozen carbon dioxide.

has anybody done this? care to share tools and technique?

in hash making we seem to use a lot of tools from the cooking and chemistry world. one of the only machines i found specifically for sublimating is a Rotary Vacuum Evaporator

http://www.youtube.com/watch?v=f6IJDyho-m8

am i too far out on a limb here?

do i have the wrong end of the stick?

could you just throw a frozen patty of bubble hash into one of these things and get it dry? at 70F?

any way to do this without spending 10 grand?

 

[DTFuqua]

it's been awhile but long ago, in a place far, far away, there was a method using dry ice and container in a freezer Don't remember much this many years later but might be a path to re-discovery.

 

[Jhhnn]

has anybody done this? care to share tools and technique?

in hash making we seem to use a lot of tools from the cooking and chemistry world. one of the only machines i found specifically for sublimating is a Rotary Vacuum Evaporator

http://www.youtube.com/watch?v=f6IJDyho-m8

am i too far out on a limb here?

do i have the wrong end of the stick?

could you just throw a frozen patty of bubble hash into one of these things and get it dry? at 70F?

any way to do this without spending 10 grand?

Sublimation occurs only below the triple point of a volatile substance- it has to be in a solid state. The apparatus you link is intended to extract substances with a relatively high triple point, condense them on the "cold finger". You want to do the opposite- extract that substance, water, & discard it, save the rest.

What you need is a vacuum pump & a vacuum chamber that can be kept below 0C, The deeper the vacuum, the faster the process will occur, so long as the temp is below 0C. A friend uses a pressure cooker in the freezer w/ a small diameter tube running behind the door gasket to a vacuum pump that isn't really very strong. He lets it run overnight, thaws it out to see what he's got, tries again as necessary. Having the extract in a thin layer apparently speeds the process because of greater surface area for sublimation.

http://en.wikipedia.org/wiki/Sublimation_(phase_transition)

Extracts aren't my thing, so that's just from what I've observed in passing & what I've read.

 

[Pangea]

Been doing some googling this morning as I had also taken note of skunkmans post about river rocks use sublimation to dry the bubble.

I have similar issues as snacks_latrine does with fresh material being very difficult to handle do to the sticky state and hope that sublimating will help preserve the terps while removing the water.

I'm just starting to look into it and hope there is a more ghetto tek solution as opposed to using a freeze drying machine, much like johnn posted.

Does anyone else have input or experience on flash freezing fresh material or drying bubble with dry ice or a sublimation process?

 

[jayjayfrank]

thanks for the bump


maybe some kind of contraption could be set up with dry ice and a styrofoam cooler?

 

[Pangea]

Yeah something like that, google up food freeze drying with dry ice, seems simple.

 

[Former Guest]

I would think the water would freeze before it would be evaporated because flash freezing is instant. It's the best way to freeze homegrown veggies and fruit/berries.

I just bought my first set of bubble bags and drying is the one part I feel unsure about. What about a fan to dry? Light breeze to evaporate?

 

[jayjayfrank]

no, not at all

freeze-dry

if sam says so

 

[ThirdEyeVision]

Now that industrial freeze dry machines don't cost a few hundred grand more people are using them. Throw your freshly wicked puck in there and boom...you have a totally dried patty that will sizzle like drysift when smoked.

Others will put freshly seived bubble into a vac oven at low temps and get a fully dried product in a quarter of the time it would normally take.

 

[jayjayfrank]

^
thanks for sharing

 

[RulaTone]

Sublimation occurs only below the triple point of a volatile substance- it has to be in a solid state. The apparatus you link is intended to extract substances with a relatively high triple point, condense them on the "cold finger". You want to do the opposite- extract that substance, water, & discard it, save the rest.

What you need is a vacuum pump & a vacuum chamber that can be kept below 0C, The deeper the vacuum, the faster the process will occur, so long as the temp is below 0C. A friend uses a pressure cooker in the freezer w/ a small diameter tube running behind the door gasket to a vacuum pump that isn't really very strong. He lets it run overnight, thaws it out to see what he's got, tries again as necessary. Having the extract in a thin layer apparently speeds the process because of greater surface area for sublimation.

http://en.wikipedia.org/wiki/Sublimation_(phase_transition)

Extracts aren't my thing, so that's just from what I've observed in passing & what I've read.

the method you suggest requires negative pressure, seems a proper way to fast dry bubblehash.

If i get it correctly if you work with the tupperware and dry ice tek instead a positive pressure is required to let the gas+water escape from container. is it true?

 

[Buddyy]

Hi
I did 2 runs of bubble hash the last week or so and after seeing a video of Frenchy Cannoli and a post on another forum by brown bear I tried to process my bubble hash into a dry homogenous storable hash using the hot glass bottle technique.
My first run looked like it went fine until the next day the hash went waxy and crumbly.
My second run I left the bubble hash to dry for longer, 48hrs at 22deg. and cca 50% RH and repeated the process with the hot bottle. Because the plastic ziplock baggie I was using couldn't take the heat I only did the flattening process once but plied it in my hands after for a while. I had only a small batch 5g and it looked like it worked fine but the next day the hash was also waxy and crumbly.
Did the hash go waxy because the material wasn't properly dry or because I didn't repeat the hot bottle flattening process enough times?
How hot should the water in the bottle be? I poured in boiling and used bottle straight away so it was quite hot, so hot the plastic warped.
I broke up the hash into crumbs and have left it to dry again. If I repeat the hot bottle flattening process with this hash will it be ok or am I losing something in this process?
What are the advantages of processing bubble hash into this homogenous piece?

If anyone understands me I'd be really happy if they could try to answer my questions

 

[jayjayfrank]

it needs to be very dry to be stable when pressed.

see bubble mans videos on youtube

when you take the wet hash patties out of the bubble bag you should dab it a little against paper towels and then use the back side of a spoon to run into thru a screen/sieve. spread the sieved bubble hash over a piece of parchment paper on top of card board and let dry for up to two weeks at no higher than 65f.


and no, frenchy is all about that old world technique thats been around since the days of buddha. this thread is about using equipment that has only been invented recently(100yrs) to further advanced the extraction process.

 

[Buddyy]

thx jay jay, yea I should've done more research before making, bubble man is great.

no higher than 65f is not possible, my ambient house temps of 70f and 45RH will have to do.

do you press bubble hash or just smoke as is once dry?

 

[jayjayfrank]

i keep it unpressed then smoosh it on to a little dabber for smoking

 

[jayjayfrank]

what you will notice is that the lower temp when drying the better long term stability and higher smoking quality's and in fact, if we were able to extract a very large (90%+) portion of the water out as fast as possible(using new drying technique) we might achieve a constantly higher quality hash than if an other wise normal method were followed.

and in fact, most of the equipment to do this was only invented over the last 100 years, about the same time frame this plant has been illegal.

 

[BlazinAzn]

I wouldn't pay a few Gs for a freeze dryer and I'm sure most of you wouldn't want to either. I am very blessed to have close ties with a my dads friends family. They have a freeze dryer they bought for around 4 grand and it hasn't been used yet. Still needs to be put together but you bet your ass I get to be the one who gets to try it out first! -30 to -50 degrees vacuume sealed for 24 hours. I'm gonna be washing all my outdoor material and I'll let you guys know how it goes!

 

[BlazinAzn]

45 micron fullmelt bubblehash sublimated using a harvest right freeze dryer. Cheers!

 

[BlazinAzn]

73 micron ice water extracted full melt close up resin heads.

 

[transplanted]

beautiful work my friend