Closed loop everything comes out as crumble

[younger_dryas]

Hi everybody,
I use to come to these grow forums years ago under another account for my home gig. Now I'm working for a medicinal company, and need some help with concentrates.

A run down of our gear:
We have a Mk II Terpenator closed loop extractor. Our trim is dried and then stored in totes in the dry room for no longer than 4 days after drying. Before a run I hand mulch it to small-medium pebble size to stay away from the fine dust plant matter our grinder use to produce. The sugar leaf is then lightly tamped, and I hand the column off to our blaster. The tubes are not pre-cooled. [He does not seem willing to go down that road after some live resin runs he did before I started.] The butane tank is chilled in IPA with dry ice, and the catch pot is in warm water to help with recovery times. We do NOT run a dry ice jacketed column.

We have three vacuum ovens. One is across international the other two I can not remember the brand of, but I will update on Monday. Each oven has its own 8 cfm CPS vacuum pump. [I will get the specific model on Monday.]

For our medicinal products we will not sell above 40ppm Butane.

My issue:
After the blaster finishes a run I receive the product on parchment. It is not soupy I'd say its more like a warm Abazaba bar. Very high viscosity. I then place it in the vacuum oven to warm for 30 minutes. I then use an IR thermometer to ensure it has reached the set temp across the whole product. (As far as temps go I thought this was part of my issue so I have one oven at 95 degrees Fahrenheit one at 100 degrees Fahrenheit and one at 105 degrees Fahrenheit. Previously all slabs were purged at 115 degrees Fahrenheit because the former lab tech thought that would help pass testing. I have no trouble passing testing at any of the three temps listed.) Once up to temp I apply a vacuum. Allowing it to muffin as much as the slab needs to, or until it reaches the limit of the shelf to the top the next part of the oven. Most slabs collapse before I reach the full vacuum available from the pumps. After collapse when the slab forms a uniform layer it appears to be shatter. Obviously warm and sappy, but uniform and translucent. As purging continues I sometimes see the beginning of crumble and try to remove it, or the whole slab will crumble overnight. This happens with EVERY stable slab. I'm at a loss at this point, and could use some help.

I've back checked all I can think to at work. We had a period of constantly dark wax from fresh not old trim, but it appears that was due to improper flushing by our former grower. All the trim since our new grower took over has produced wax between goldenrod and light brown sugar. I have inspected the trim before it is dried and noticed more fan leaves than I would expect to see, but I'm not sure that is a possible issue or if I am just grasping.
I pass all 3rd party testing with either zero residual[within their testing limits] or 16-24ppm butane.

Any help or direction would be greatly appreciated!

 

[Mr.Goodtimes]

What do you pull your vacume to?

 

[younger_dryas]

Correct me if I'm wrong, but I believe it is relative to local air pressure. Locally we are average at 30.02 in Hg. My across shows it pulling to below 27 in Hg approx 27.5 from memory. I'll get a photo of the gauge when I'm back to work. The other two I don't really trust. They have digital readouts and one reads 14.7 psi the other can get to 15.2 psi on the readout. Since they all have the same vacuum pump and approximately the same volume I trust my across gauge most. It is the most consistent. Once I get the model I can tell you what the pump is rated to as well.

 

[Mr.Goodtimes]

From my knowledge yeah local air pressure will prevent you from getting to a full vac. What I was thinking is if pulling ~27.5 hg at your altitude is it the same as pulling 30 hg at sea level? The higher the vac the lower the boiling point of thc, and I've noticed I get wax/crumble from higher temperatures, so maybe the vac pressure would have something to do with it?

Did you run at 27.5 hg at all four temps (95-100-105-115) and came out the same consistancy?

If that makes sense... I'm a lil high and brainstorming lol

 

[Mr.Goodtimes]

I'm 100ft above sea level and I pull to 29.5 hg in my AI oven temps from 90-110 and it doesn't wax up til I get aroun 140

 

[cannabineer]

Here is my take; I have observed and pursued the same phenomenon in my putterings with hydrocarbon extractions on our favorite botanical.

There is a range of THCA, the original plant product, to its thermal degradation product, the active THC, that is dependent on cultivar (strain) as well as harvest time. I think you have a lucky strain that produces a very high percentage of THCA. It is a solid but very very soluble in organic solvents. This means introduced solvents like butane or hexanes ... or intrinsic solvents, terpenes from the plant.
Your vacuum protocol seems ideal for achieving the optimum between being warm enough to drive off the "varnishy" terpenes under pump vacuum - and cool enough to spare the THCA from the sort of partial degradation the hot-plate cowboys regularly encounter. Frankly, I;m envious. A crumbly extract is its own hallmark of purity, and is mechanically easier to handle than tarry goopy high-THC preps that I currently like to make.

 

[gtir]

How often are you flipping the slab?

 

[younger_dryas]

Here is my take; I have observed and pursued the same phenomenon in my putterings with hydrocarbon extractions on our favorite botanical.

There is a range of THCA, the original plant product, to its thermal degradation product, the active THC, that is dependent on cultivar (strain) as well as harvest time. I think you have a lucky strain that produces a very high percentage of THCA. It is a solid but very very soluble in organic solvents. This means introduced solvents like butane or hexanes ... or intrinsic solvents, terpenes from the plant.
Your vacuum protocol seems ideal for achieving the optimum between being warm enough to drive off the "varnishy" terpenes under pump vacuum - and cool enough to spare the THCA from the sort of partial degradation the hot-plate cowboys regularly encounter. Frankly, I;m envious. A crumbly extract is its own hallmark of purity, and is mechanically easier to handle than tarry goopy high-THC preps that I currently like to make.

Thank you! Hearing that makes me feel a lot better. I also prefer the crumble consistency. We have had a running request from our wholesale person to produce shatter to suppl some other medicinal facilities. If not for that I would gladly produce crumble all day long.

 

[younger_dryas]

How often are you flipping the slab?

I usually flip my slabs twice.

 

[younger_dryas]

I'm 100ft above sea level and I pull to 29.5 hg in my AI oven temps from 90-110 and it doesn't wax up til I get aroun 140

Interesting. Thank you!

 

[younger_dryas]

To satisfy orders and not completely change our methods I made some winterized shatter. So I'll keep plugging away at getting shatter straight from blast, but for now this will satisfy our wholesaler.
Thank you guys for the input!

 

[cannabineer]

Thank you! Hearing that makes me feel a lot better. I also prefer the crumble consistency. We have had a running request from our wholesale person to produce shatter to suppl some other medicinal facilities. If not for that I would gladly produce crumble all day long.

You can probably convert the crumble into shatter by partially decarbing, say 90 degrees C for a few minutes ... or decarb 1/3 and mix with the crumble; it should melt together and stay glassy.

I have had good crumble go gooey and finally not throw any solid at all (if I dewaxed!) because of brief overheat. I can't tell you exact proportions but you might want to play with some small test batches.

 

[doniawon]

Here is my take; I have observed and pursued the same phenomenon in my putterings with hydrocarbon extractions on our favorite botanical.

There is a range of THCA, the original plant product, to its thermal degradation product, the active THC, that is dependent on cultivar (strain) as well as harvest time. I think you have a lucky strain that produces a very high percentage of THCA. It is a solid but very very soluble in organic solvents. This means introduced solvents like butane or hexanes ... or intrinsic solvents, terpenes from the plant.
Your vacuum protocol seems ideal for achieving the optimum between being warm enough to drive off the "varnishy" terpenes under pump vacuum - and cool enough to spare the THCA from the sort of partial degradation the hot-plate cowboys regularly encounter. Frankly, I;m envious. A crumbly extract is its own hallmark of purity, and is mechanically easier to handle than tarry goopy high-THC preps that I currently like to make.

Is there still a rep button? I love this post!

 

[Mr.Goodtimes]

Interesting. Thank you!

I have to check my comment there, my last run (last week) was at 29.5 hg and 115f and it all waxed up for some reason. still delicious but not quite what I was going for.

I had a friend tell me that dewaxing column was key to getting shatter, by removing the plant waxes would allow for a stable end product... So I will try that my next run and see if that helps. Id like to figure everything out and get the process down perfect eventually lol.

 

[Fadedawg]

Material and process. You can't make chicken salad out of chicken manure, so you need to start with material still in the (C-22) carboxylic acid state. The COOH carboxyl group raises the boiling point and its stiffness at room temperature. C-21 phenolic cannabinoid material is more of an oil than a resin.

Wax is a hydrate, so you need water and the grains form around points of nucleation, which plant waxes and fine dust are.

We extract subzero, so water is tied up as ice and longer chain molecules like C-30 plant waxes are not as readily dissolved. Our cotton candy is shatter coming out of the Terpenator, and typically stays that way during subsequent final purge in the vac oven.

A butane/propane mix also extracts less longer chain molecules, and we use up to 50/50 when we use ultra low injection temperatures, to both improve select-ability, and to keep it thin enough to flow at those temperatures.

I suggest you try freezing your material and using subzero butane/propane.

 

[younger_dryas]

You can probably convert the crumble into shatter by partially decarbing, say 90 degrees C for a few minutes ... or decarb 1/3 and mix with the crumble; it should melt together and stay glassy.

I have had good crumble go gooey and finally not throw any solid at all (if I dewaxed!) because of brief overheat. I can't tell you exact proportions but you might want to play with some small test batches.

I have never thought of partially decarbing some at low temp. I will definitely give that a go!

I have a rotary evaporator at work so I pull vacuum until I can recover EtOH at 86 degrees. A little slower, but I noticed the product comes out very nice. Now I just wish there was some declared safe value for residual ethanol in concentrate. I have the U.S. Department of Health and Human Services pharmaceuticals data for residual solvents, and it lists ethanol as a class 3 solvent with 10g of 5,000 PPM a day as safe. I don't know of any big pharma products that are combusted for use so I'm not sure that is a value that works in this market. I would never want to be that high on residual either, but I also don't want to spend half a week purging down to get 5 PPM at low enough temps to protect my product.

 

[younger_dryas]

I have to check my comment there, my last run (last week) was at 29.5 hg and 115f and it all waxed up for some reason. still delicious but not quite what I was going for.

I had a friend tell me that dewaxing column was key to getting shatter, by removing the plant waxes would allow for a stable end product... So I will try that my next run and see if that helps. Id like to figure everything out and get the process down perfect eventually lol.

Me too! Hopefully we can both get there!

 

[younger_dryas]

Material and process. You can't make chicken salad out of chicken manure, so you need to start with material still in the (C-22) carboxylic acid state. The COOH carboxyl group raises the boiling point and its stiffness at room temperature. C-21 phenolic cannabinoid material is more of an oil than a resin.

Wax is a hydrate, so you need water and the grains form around points of nucleation, which plant waxes and fine dust are.

We extract subzero, so water is tied up as ice and longer chain molecules like C-30 plant waxes are not as readily dissolved. Our cotton candy is shatter coming out of the Terpenator, and typically stays that way during subsequent final purge in the vac oven.

A butane/propane mix also extracts less longer chain molecules, and we use up to 50/50 when we use ultra low injection temperatures, to both improve select-ability, and to keep it thin enough to flow at those temperatures.

I suggest you try freezing your material and using subzero butane/propane.

I understand. I previous trim would definitely fall into the chicken manure category. The current trim is far superior which is why I think we should be able to pull this off.

I will try freezing the trim before we blast it on the next run and see what results we get. I have looked into using a butane/propane mix, but with the increased pressures I have hesitated to try it. Once I have exhausted all avenues I will bring it up to our blaster, and see where he stands on attempting it. Thank you for the suggestions!