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Old 04-23-2015, 12:35 AM #21
CLSn00b
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Originally Posted by live resin View Post
I think buds should not be frozen in contact with ambient atmosphere. GW recommended packing the tube before freezing so less air contacts the buds, but I think no air is better.

I've had success doing cyro temp live resin soak extractions in a homemade glove box thats been purged and filled with co2 before freezing the buds with dry ice/IPA. No air contacts the buds and forms ice, the water in the buds remains ice, and no ice builds up on the outside of the extraction container. You could also use a Schlenk line for the same purpose.

Distill and dry your butane, use thermometers to make sure temps at -40C. I never use any heat so the fresh frozen is always wax instead shatter due to all the terps. Its not light yellow like PHO, but definitely not dark either
Packing prior to freezing isn't an option unless you mean packing and refreezing. The bags are coming from their freezer to mine. I am, and have been distilling the pure tane N-tane I have been using. It's amazing how much stuff is still in a can of 99.99999% "pure" n-tane. I'm thinking maybe it's not cold enough, I am using an mt69 in a bucket of ice water between the recovery pump and the recovery tank/manifold, same with my recovery tank
Should I be packing the tube with material straight from the freezer and putting it back in the freezer with caps on for a time? Or straight connect it to the system and fill the cryo sleeve with di/ipa and letting it chill before filling it with solvent? I've always been able to make vibrant yellow tinted extracts from fresh frozen material via thermos soaks and letting them chill in a cooler full of dry ice, so this learning curve is definitely disappointing, but not surprising.
Really appreciate all the input thus far.
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Old 04-23-2015, 08:55 AM #22
live resin
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Quote:
Originally Posted by CLSn00b View Post
Should I be packing the tube with material straight from the freezer and putting it back in the freezer with caps on for a time? Or straight connect it to the system and fill the cryo sleeve with di/ipa and letting it chill before filling it with solvent?
Really appreciate all the input thus far.
Ideally you would pack the tube with buds at room temp then put it straight into the cryo sleeve. Freezer not really necessary. I like to have the butane tank in di/ipa too.

I think its really important to not have any atmospheric water vapor condense into ice crystals and cover the bud surface. Lowering the surface area for extraction will lower yields.

Maybe you could drive out the remaining air in the tube by putting a small chunk of dry ice in the bottom of the tube and seal the bottom, then add the buds, then straight to cryo sleeve. As it sublimes the heavier co2 should push the air out the top of the tube
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Old 04-23-2015, 10:50 AM #23
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Quote:
Originally Posted by live resin View Post
I think buds should not be frozen in contact with ambient atmosphere. GW recommended packing the tube before freezing so less air contacts the buds, but I think no air is better.

I've had success doing cyro temp live resin soak extractions in a homemade glove box thats been purged and filled with co2 before freezing the buds with dry ice/IPA. No air contacts the buds and forms ice, the water in the buds remains ice, and no ice builds up on the outside of the extraction container. You could also use a Schlenk line for the same purpose.

Distill and dry your butane, use thermometers to make sure temps at -40C. I never use any heat so the fresh frozen is always wax instead shatter due to all the terps. Its not light yellow like PHO, but definitely not dark either

what was yeld like in your cryo soak extraction?

and generally speaking
whats yeld like in a CLS using fresh frozen material and subzero extraction?
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Old 04-23-2015, 04:30 PM #24
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CLSn00b,

To reword what live resin is saying, when you freeze the bud and then transfer it to the columns later (like you're doing), moisture from the air will condense on the outside of the cold buds when it is exposed to atmosphere. To prevent this, pack the column with room temp buds, seal it, and then freeze it. This will help with your moisture problem and probably help with you color. Also make sure your tane is nice and cold when injecting as well.

RulaTone,

Yields are generally pretty low on these type of runs. In my experience, 10-11% is pretty typical. Could be more or less, but there are so many variable in that equation (number of trichome heads present, temp of tane, temp bud, soak time, etc.)

GH
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Old 04-23-2015, 09:51 PM #25
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GH is this 10-11% off trim or nugs? It might take 2-3 soaks depending on the length but I think 15-20% yield is pretty attainable.

Given equal quality buds yield should be comparable to winterized room temp runs.

If you're only getting 10-11% do you repurpose the leftover material somehow or extract it again with another solvent?
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Old 04-23-2015, 10:54 PM #26
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Quote:
Originally Posted by live resin View Post
GH is this 10-11% off trim or nugs? It might take 2-3 soaks depending on the length but I think 15-20% yield is pretty attainable.

Given equal quality buds yield should be comparable to winterized room temp runs.

If you're only getting 10-11% do you repurpose the leftover material somehow or extract it again with another solvent?
Live resin,

Yes. In that scenario there would be a good deal of goodies left to extract. That yield is low, but when looking for only the most premium product, that isn't too far off. If desired, that bud could be dried and run again. We would either use butane or ethanol to extract a second grade run for edible oil.

GH
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Old 04-23-2015, 11:13 PM #27
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Originally Posted by gholladay View Post
CLSn00b,

To reword what live resin is saying, when you freeze the bud and then transfer it to the columns later (like you're doing), moisture from the air will condense on the outside of the cold buds when it is exposed to atmosphere. To prevent this, pack the column with room temp buds, seal it, and then freeze it. This will help with your moisture problem and probably help with you color. Also make sure your tane is nice and cold when injecting as well.

RulaTone,

Yields are generally pretty low on these type of runs. In my experience, 10-11% is pretty typical. Could be more or less, but there are so many variable in that equation (number of trichome heads present, temp of tane, temp bud, soak time, etc.)

GH
Thanks for the reply, I'm not prefreezing dried cured material, I'm keeping fresh material frozen not dried cured material. I have always had success with fresh frozen material by keeping it vac sealed and frozen in the chest freezer then transferring it to a SS thermos for soaking. I assumed this was the same concept. It's coming out a greenish brown vs a deep amber so I'm pretty sure I'm pulling chlorophyll. Is there a way to run this and get good results without cryo Temps? I only have viton gaskets atm and am cautious as hell. Am I to take what you said as packing the columns straight away then freeze? That's going to be a challenge seeing as the farm and I are 40 minutes apart. I can't see that being the answer.
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Old 04-24-2015, 03:45 AM #28
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Quote:
Originally Posted by CLSn00b View Post
Thanks for the reply, I'm not prefreezing dried cured material, I'm keeping fresh material frozen not dried cured material. I have always had success with fresh frozen material by keeping it vac sealed and frozen in the chest freezer then transferring it to a SS thermos for soaking. I assumed this was the same concept. It's coming out a greenish brown vs a deep amber so I'm pretty sure I'm pulling chlorophyll. Is there a way to run this and get good results without cryo Temps? I only have viton gaskets atm and am cautious as hell. Am I to take what you said as packing the columns straight away then freeze? That's going to be a challenge seeing as the farm and I are 40 minutes apart. I can't see that being the answer.
CLSN,

Packing the buds straight from the plant into the columns and then freezing them would be ideal, but everyone has to make the best of their own situation. The amount of moisture that will condense on the buds also really depends on your relative humidity, air temp, and the exposure time of the bud. This might not be your issue, but I'd be willing to bet your issue is related to water content. Water in the tane will pick up more undesirables (aka chlorophyll and other polar molecules that darken the color). The ways to prevent this are by keeping the extra water from condensing on the bud during transfer, making sure your tane doesn't have water in it (if it's coming from a tank instead of a can), making sure the tane is cold and the bud is frozen, limiting soak time, and limiting the heat exposure to the oil/tane mixture during finishing processes.

If you do all those things correctly you should get blonde oil. It's already been mentioned, but tri-chome color plays a big factor into the color of your finished product as well. I would inspect the buds with a hand microscope to see the color of the trichomes. If they are already a dark amber color, the oil will keep that color (this will vary with strain type, process, crop time, etc). There are so many variables in this equation that it is hard to answer these types of questions without seeing every step of the process specifically.

Hope this helps!

GH
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Old 04-24-2015, 05:39 AM #29
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Originally Posted by gholladay View Post
CLSN,

Packing the buds straight from the plant into the columns and then freezing them would be ideal, but everyone has to make the best of their own situation. The amount of moisture that will condense on the buds also really depends on your relative humidity, air temp, and the exposure time of the bud. This might not be your issue, but I'd be willing to bet your issue is related to water content. Water in the tane will pick up more undesirables (aka chlorophyll and other polar molecules that darken the color).The ways to prevent this are by keeping the extra water from condensing on the bud during transfer, making sure your tane doesn't have water in it (if it's coming from a tank instead of a can), making sure the tane is cold and the bud is frozen, limiting soak time, and limiting the heat exposure to the oil/tane mixture during finishing processes.

If you do all those things correctly you should get blonde oil. It's already been mentioned, but tri-chome color plays a big factor into the color of your finished product as well. I would inspect the buds with a hand microscope to see the color of the trichomes. If they are already a dark amber color, the oil will keep that color (this will vary with strain type, process, crop time, etc). There are so many variables in this equation that it is hard to answer these types of questions without seeing every step of the process specifically.

Hope this helps!

GH
I definitely feel like I'm pulling water and not so much that the product itself should be dark like this. I've gotten nice coloured stuff from their garden with cured material and thru thermos soaking. I have a feeling butane temp is something I have overlooked, I have generally been running it at or just below ambient temp. and using an ice water bath for recovery as I know butane will chase the cold. I will have to try freezing the butane, ice bath won't get it cold enough I assume, and the thought of putting a 30LB. tank in a chest freezer is a scary thought. I suppose a DI/IPA slurry is the best to achieve the desired temps? I've seen discussions about using 50' coils submersed in a slurry to drop the tane temp without needing to keep the tank itself in a bath, I guess that works as well? How would I make sure my tane has no water in it besides a filter drier? I'm can tapping 99.9999% N-tane by purtane and distilling it to get out the heavier properties. so I'm fairly confident in the cleanliness of the tane. again thanks for all the input and help
Thanks again for all your input, I really appreciate it.
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Old 04-24-2015, 11:11 AM #30
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I will have to try freezing the butane, ice bath won't get it cold enough I assume, and the thought of putting a 30LB. tank in a chest freezer is a scary thought. I suppose a DI/IPA slurry is the best to achieve the desired temps? I've seen discussions about using 50' coils submersed in a slurry to drop the tane temp without needing to keep the tank itself in a bath, I guess that works as well? How would I make sure my tane has no water in it besides a filter drier?
Thanks again for all your input, I really appreciate it.
https://en.wikipedia.org/wiki/Cooling_bath

Ice and salt will get you to -20C, still I'd go with di/ipa.

Drying butane, your options are molecular sieve or chemical drying agent (calcium chloride, sulfuric acid, the list goes on...)

If bubbling thru sulfuric acid makes sure you've removed any iso-butane as it will react
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