Mk IVC Cotton Candy extraction video

[Gray Wolf]

Boiling point is where the internal vapor pressure exceeds atmospheric pressure suppressing it.

We've pretty much removed the atmospheric pressure, but lowered the temperature so that the molecular activity is less, hence so is the vapor pressure.

Awaiting a reply from my chemistry resource, so more if I learn the proper term, but in looking for the name for rapid evaporation, I ran across this interesting paper.

http://www.spscientific.com/DownloadGenevacFile.aspx?id=3891

http://www.news-medical.net/Sample-Genie-for-Drying-Large-Volumes-Directly-into-Vials

 

[frog357]

I would like to throw out some observations on the technique being discussed. I found that if you remove the heat source around -10"hg and continue the recovery until full vacuum you can achieve the muffin with just a recovery pump. That is not needed however because you can skip full recovery (stop any time after -10"hg) and just pull a muffin and let in air repeatedly until the muffin has stabilized (most of the solvent being removed). I have seen some muffins get stuck or not want to come out, just put the vacuum pump back on and pull longer and it fluffs right up. I also found if a muffin has fallen into a puddle after waiting too long, again with the vacuum and it will come right back. So to recap, don't worry too much about when you put the vacuum on, just finish the recovery stage until muffin and then apply vacuum while watching that your muffin doesn't get too big. If it does get too big, let in some air and then pull a vacuum, repeat until you can pull vacuum without the muffin moving. Smash, pour, and repeat if needed. I have not had any issues with nucleation except for one time when I failed to run the vacuum for over 24 hours while the slab was curing in the oven.

 

[Gray Wolf]

I would like to throw out some observations on the technique being discussed. I found that if you remove the heat source around -10"hg and continue the recovery until full vacuum you can achieve the muffin with just a recovery pump.

We don't use the recovery pump past about -22" Hg, because there isn't enough LPG left to keep the pump piston seals lubricated and that leads to rapid wear and early failure.

That is not needed however because you can skip full recovery (stop any time after -10"hg) and just pull a muffin and let in air repeatedly until the muffin has stabilized (most of the solvent being removed).

That may depend on your pump. A VaporHawg can pull a deeper vacuum than -10" with the pot half full of LPG.

I have seen some muffins get stuck or not want to come out, just put the vacuum pump back on and pull longer and it fluffs right up. I also found if a muffin has fallen into a puddle after waiting too long, again with the vacuum and it will come right back.

That works sometimes, but I haven't found it to be true once most of the butane is gone but the cotton candy hasn't solidified yet. Not enough LPG left to fluff it back up.

So to recap, don't worry too much about when you put the vacuum on, just finish the recovery stage until muffin and then apply vacuum while watching that your muffin doesn't get too big. If it does get too big, let in some air and then pull a vacuum, repeat until you can pull vacuum without the muffin moving.

I prefer to close the vacuum valve before the muffin gets too big, and when I backfill, I use N2 so that when the pot is opened, it is below 10% of LEL, and the N2 doesn't oxidize the concentrate.

Smash, pour, and repeat if needed. I have not had any issues with nucleation except for one time when I failed to run the vacuum for over 24 hours while the slab was curing in the oven.

We typically get below 10% of FDA residual standards in about 4 hours starting with cotton candy. Nucleation is also typically not an issue, unless we induce it on purpose to grow crystals.

 

[Funkyfranklin]

Man, I wish I had some of that in a slick right now!

 

[HG23]

I just read that Colorado raised the allowable residual levels of butane/propane in Cannabis extracts from 800 to 5,000 PPM. I believe Oregon just did the same the other day, didn't they??

With that type of limit, I wonder if you would even need to pull a vacuum on the oil while it's in the oven, just melt the cotton candy powder down into a slab. GW didn't you get the powdered cotton candy oil tested at one point a while ago?

I have been running through some live resin recently and it definitely loses significant terpenes to the cold trap on the oven after multiple flips. It would be nice to hold on to as many of those terps as possible in the original extract.

What do you all think about those new limits? For reference, 5,000 PPM is the same as .5%. People I talk to seem unsure about the "big" PPM numbers that are in the hundreds and thousands, so i usually say it as "99.5% solvent free".

 

[Old Gold]

That's surprisingly high. I'm with it. Let's just make sure the suppliers are highly adept in all things distillation, and ensure they go to reputable/proven sources for solvents.
As long as the patient or customer knows what is in it, I see nothing wrong with it.

With that type of limit, I wonder if you would even need to pull a vacuum on the oil while it's in the oven, just melt the cotton candy powder down into a slab
. . .
It would be nice to hold on to as many of those terps as possible in the original extract.
".

I dot that all the time with my head stash.

 

[Gray Wolf]

I just read that Colorado raised the allowable residual levels of butane/propane in Cannabis extracts from 800 to 5,000 PPM. I believe Oregon just did the same the other day, didn't they??

With that type of limit, I wonder if you would even need to pull a vacuum on the oil while it's in the oven, just melt the cotton candy powder down into a slab. GW didn't you get the powdered cotton candy oil tested at one point a while ago?

I have been running through some live resin recently and it definitely loses significant terpenes to the cold trap on the oven after multiple flips. It would be nice to hold on to as many of those terps as possible in the original extract.

What do you all think about those new limits? For reference, 5,000 PPM is the same as .5%. People I talk to seem unsure about the "big" PPM numbers that are in the hundreds and thousands, so i usually say it as "99.5% solvent free".

5000 ppm is the FDA standard for Class III solvents. Butane is classified as GRAS, or generally regarded as safe. It is even used as a propellent.

The issue that I see, is that the human sensory threshold for hydrocarbons is in the low ppm range, and I can taste n-Butane at 5000 ppm.

I personally prefer it under 500 ppm.

 

[SkyHighLer]

I made the argument for raising the limits due to the GRAS recognition in another thread,

https://www.icmag.com/ic/showpost.php?p=7704587&postcount=16

In the post previous to the linked above, I provided a response to those trying to equate the ppm of residual butane in BHO to the concentration of butane in the mixture of air and oil vapor actually inhaled.

"^ You're saying the state cannabis concentrate residual solvent standards are based on inhaling an undiluted dab? Pure vapor, no air? Chokes me up..."

https://www.icmag.com/ic/showpost.php?p=7703651&postcount=15

You can't detect with your senses the little bit of residual butane once it's been diluted with air, not to mention the impossibility of discerning it among the overwhelming smell of the oil's vapors.

The 5,000 ppm isn't even necessary, but it does ensure a basic purge was done, if for no other reason than appearance.


If the limits were actually raised, my deepest thanks to whoever expedited it.

 

[Old Gold]

Gray Wolf: Do you taste 5000 ppm in a controlled environment or just taking a dab of something that tests at 5000 ppm?
It might make for a harsher smoke, as can be the case with the terpenes it might carry. Safe? That much is relatively agreed upon, but there is still plenty of room for 0 ppm extracts on shelves.

 

[Gray Wolf]

Gray Wolf: Do you taste 5000 ppm in a controlled environment or just taking a dab of something that tests at 5000 ppm?
It might make for a harsher smoke, as can be the case with the terpenes it might carry. Safe? That much is relatively agreed upon, but there is still plenty of room for 0 ppm extracts on shelves.

I just take dabs that I can taste it in and have run them through the GC to see where they were.

My taste buds are shot through age and abuse, so both partners Carla and Joe can taste things I can't as well.

 

[SkyHighLer]

Dude, calculate the mass of the butane in a dab at .5% (5,000 ppm,) and place that tiny amount of liquid butane in a liter bag of air, and you're going to tell me you can detect the butane in the bag with your unaided senses?

https://en.wikipedia.org/wiki/Lung_volumes


Another thing to think about is the butane comes off first when a dab hits the nail, over in an instant, so, when are you detecting the butane? At that first instant, or at full dilution?


I'll even present data to support your conjecture, lol,

Although butane is considered odorless by some, it has been reported that the odor of butane can be detected at concentrations of 1.2-6.2 ppm (2.85-14.63 mg/m3) (Ruth 1986).

Ruth J.H. Am. Ind. Hyg. Assoc. J. 3. Vol. 47. 1986. Odor thresholds and irritation levels of several chemical substances: A review; pp. A142–A151.

But that's diluted with only pure air, not mixed with the heavy vapors of a dab.

Check my homework,

Average dab .05 gram

5,000 ppm = .5%

.05 x .005 = .00025g of butane in a normal sized dab with 5,000 ppm of butane residuals

Dry air at sea level is about 1.2 grams per liter

.00025/1.2 = .000208 concentration level = 208 ppm of butane hits your lungs for a few seconds while you hold in a dab

Remember your body isn't taking it all in, it's being exhaled along with the cannabinoids in those huge vapor clouds we all take such pride in...

 

[SkyHighLer]

I just read that Colorado raised the allowable residual levels of butane/propane in Cannabis extracts from 800 to 5,000 PPM. I believe Oregon just did the same the other day, didn't they??

With that type of limit, I wonder if you would even need to pull a vacuum on the oil while it's in the oven, just melt the cotton candy powder down into a slab. GW didn't you get the powdered cotton candy oil tested at one point a while ago?

I have been running through some live resin recently and it definitely loses significant terpenes to the cold trap on the oven after multiple flips. It would be nice to hold on to as many of those terps as possible in the original extract.

What do you all think about those new limits? For reference, 5,000 PPM is the same as .5%. People I talk to seem unsure about the "big" PPM numbers that are in the hundreds and thousands, so i usually say it as "99.5% solvent free".

Came back channel, here's the basis:


Farrer DG. Technical report: Oregon Health Authority’s process to decide which types of contaminants to test for in cannabis. Oregon Health Authority. 2015 December.

https://public.health.oregon.gov/Pr...ical-report-marijuana-contaminant-testing.pdf



Colorado Medical Marijuana Rules

https://www.colorado.gov/pacific/si...lgamated Medical Rules Effective 01012017.pdf



The attached chart is from the latter, page 127.

The other scans are from the Oregon Health Authority report.

 

[TerpChild]

I think the taste GW might be referring to is a mild sweetness upon exhale, something that tastes almost artificial versus the natural flavor of cannabanoids and terpenes. It was something I noticed with some real terpy sugar trim run that I didn't spread as thin as i usually do for the low-temp vac purge, and it did not purge as fast or as thoroughly as other slabs I thinned out more. Never got it tested though so I cannot say anything for sure, but i did another trim run and replicated everything as close i could, except spread the slab thinner for purge, and i did not notice the strange mild sweet flavor in back of my mouth. I used whip-it premium butane straight from the can for all of those extractions, if that matters.

On another topic... The cotton candy thing is hard for me to manipulate as it shatters off in dust size pieces. Is there some trick to not losing these bits? Is the main purpose of the cotton candy method to improve safety versus pouring off? Thanks guys!

 

[Old Gold]

I agree that it is a taste that can be learned given enough ---err -- practice?

 

[Gray Wolf]

I think the taste GW might be referring to is a mild sweetness upon exhale, something that tastes almost artificial versus the natural flavor of cannabanoids and terpenes. It was something I noticed with some real terpy sugar trim run that I didn't spread as thin as i usually do for the low-temp vac purge, and it did not purge as fast or as thoroughly as other slabs I thinned out more. Never got it tested though so I cannot say anything for sure, but i did another trim run and replicated everything as close i could, except spread the slab thinner for purge, and i did not notice the strange mild sweet flavor in back of my mouth. I used whip-it premium butane straight from the can for all of those extractions, if that matters.

On another topic... The cotton candy thing is hard for me to manipulate as it shatters off in dust size pieces. Is there some trick to not losing these bits? Is the main purpose of the cotton candy method to improve safety versus pouring off? Thanks guys!

It is slightly sweet, with a butyl flavor. I can taste it in an extract, but not smell it.

A slightly different topic, because of lack of competing background flavors, but check the taste standards for hydrocarbons in drinking water.

We freeze cotton candy and stir it to powder while it is still in the pot. We then carefully pour that out as a powder.

Cotton candy technique combined with N2 backfill keeps the pot below LEL when opened.

It also reduces residual solvents in the concentrate, because there is no thinner film to purge from that the wall of a bubble.

 

[errl-is-a-myth]

It is really hard to say when something is truly tasteless and odorless. It may be lacking the specific phenols, eseters, etc, but it is possible we still sense the presence of the residual solvent--it just doesn't fit into a typical category of sensation? Our taste and olfactory (chemosensational) systems mainly function for dietary reasons, things taste good, things taste bad. We did not evolve tasting and smelling for hydrocarbons. It is possible we perceive it, but lack a discernible sensation for it. Unless perhaps you've dabbed yourself into oblivion so many times you named your couch "oblivion." As far as being able to detect it at levels around 200ppm... well I don't know about that. Then add the heavy vapor cocktail that is a dab and I'm even more skeptical. The only thing I can think of that's remotely analogous is something like scotch and water. Water is (baring additives and minerals) tasteless and odorless. Scotch is a strong complex whiskey, no two are the same. Add a couple ice cubes to a glass and the flavor profile is altered. If you use ice, this partially because the colder temperature numbs your taste buds. Well I forgot what I was talking about, but you get the point right?

 

[TerpChild]

Maybe ice cubes introduce additional oxygen to the scotch in addition to whatever trace minerals are in the ice cube water?
I dunno about you guys, but to me good butane smells pleasant. Maybe thats cuz my brain knows it will make yummy errl though, lols...
Good point GW about the wall of a bubble being the thinnest possible membrane to purge. When i do cotton candy i have basically no purge action in the oven.

 

[Gray Wolf]

It is really hard to say when something is truly tasteless and odorless. It may be lacking the specific phenols, eseters, etc, but it is possible we still sense the presence of the residual solvent--it just doesn't fit into a typical category of sensation? Our taste and olfactory (chemosensational) systems mainly function for dietary reasons, things taste good, things taste bad. We did not evolve tasting and smelling for hydrocarbons. It is possible we perceive it, but lack a discernible sensation for it. Unless perhaps you've dabbed yourself into oblivion so many times you named your couch "oblivion." As far as being able to detect it at levels around 200ppm... well I don't know about that. Then add the heavy vapor cocktail that is a dab and I'm even more skeptical. The only thing I can think of that's remotely analogous is something like scotch and water. Water is (baring additives and minerals) tasteless and odorless. Scotch is a strong complex whiskey, no two are the same. Add a couple ice cubes to a glass and the flavor profile is altered. If you use ice, this partially because the colder temperature numbs your taste buds. Well I forgot what I was talking about, but you get the point right?

I don't know what my limits are, but I do know that at age 73, both of my younger partners can taste and smell things I can't (but I can eat way spicier shit).

The one closest my age is a female and besides being an EE, is a world class cook, and probably started with more acute sense of taste and smell.

I can taste the butane at 5000 ppm, but not at 375 ppm, which is about where our cotton candy is after 4 hours in a vacuum oven.

In NV the standard that we had to meet was 10% of FDA residual Class III solvent standards, or 500 ppm, plus be free (ND) of evil spirits in the form of mystery oil, mold, and pesticides, etc.

At 500 ppm, the concentrate is typically still rife with monoterpenes, so a good place to stop for best aroma and flavor, and those monoterpenes no doubt make the alkane aftertaste less noticeable, even if it is detectable at those levels.

The studies on human sensory thresholds for hydrocarbons, often show a second number called adapted, which is about an order of magnitude lower than unadapted. IE: ~22 ppm vis a vis 200 ppm, but as noted, in addition to those residual alkanes, you have all of the terpenes and terpenoids, which are pungent alkene hydrocarbons because some have oxygen atoms in their structure.

The C-4 H-10 alkane flavor is pretty much lost in the pungent mix of C-10 H16 alkenes on inhale and smacking of the lips ceremony, but detectable on exhale as an aftertaste.

 

[SkyHighLer]

My suggestion for the shoot out test:

Take some hight quality THC distillate, dissolve in n-butane, divide the liquid butane/oil in half, vacuum purge one half to 5,000 ppm and the other half to 500 ppm, blindfold A/B dab test for sense of residual butane.

I'm so sure you can't actually sense the butane, I didn't bother to include adding terpenes in post purge to cover butane recognition.

 

[TerpChild]

What do people in this thread think about the 5000ppm limit in OR - too high or is that ok?
GW says in NV its 500ppm, and that sounds like a better number to me to have for health standards. Even if butane is now GRAS.
I am curious to see what it will end up being for recreational bho in CA once everything is all said and done...