Nucleation

noprohibir · Jun 1, 2015

Nucleation is the first step in the formation of either a new thermodynamic phase or a new structure via self-assembly or self-organization. - Wikipedia

Nucleation, the initial process that occurs in the formation of a crystal from a solution, a liquid, or a vapor, in which a small number of ions, atoms, or molecules become arranged in a pattern characteristic of a crystalline solid, forming a site upon which additional particles are deposited as the crystal grows. - Brittanica

Let us now discuss & learn in order to prevent & improve!

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noprohibir · Jun 1, 2015

Shatter Nucleation

Shatter Nucleation

I have some shatter nucleation in a slab We just produced. I believe the cause may be residual butane. Shatter Doctor's? Do you Concur?

MrSpectre · Jun 2, 2015

Oh Boy,

justintime420 · Jun 2, 2015

In my experience it happens from residual solvent, moisture, thickness, even heat through out the slab, length of time in vacuum, heat level of vacuum, oxidation, poor growing methods and poor curing/storing methods. I would say the only way to prevent is to own your material from start to finish which cuts down on almost all variables as you will have full control. Not very easy to do so get into the details with your starting material and processes hows your relative humidity? besides all this there's a wealth of info scattered throughout ICmag about people and their experience with the auto budder effect.

MEMED · Jun 2, 2015

good answer justintime420.

HG23 · Jun 2, 2015

Gray Wolf said:
There are a couple things that affect an extractions propensity to autobudder, or wax before the rest of the patty, and those are points of nucleation and water content.

The budder is ostensibly a wax and oil hydrate, formed around a point of nucleation.

Points of nucleation can be plant wax particles or even a small spec of plant material.

The less plant wax present, and the better the filtration, the less prone to auto buddering.

By definition, hydrates need water. The less water, the less budder prone.

Here is a post by GW from earlier this year that I found very interesting. Maybe he can drop in and elaborate if at all possible. I have made some very nice oleoresins but been frustrated to go out to the oven and see them autobuddering. I have been heavily considering adding addition dewaxing capabilities to my setup to try and combat it. I run subzero so I haven't considered extra dewaxing measures necessary, but if it will reduce the instances of waxing I'll try.

I do a pretty good job keeping the tubes vacced and below freezing before extractions but have been wondering about what happens when I'm vapor assisting the liquid butane out of the column because it raises the temp above freezing. Same thing as when some people use their heat mats. Do these practices release too much water into the extracts?

Rickys bong · Jun 2, 2015

I think you are confusing nucleation with poor crystal formation or "buddering". Nucleation is just the initial stages of crystal formation.
It would be interesting to see the difference between the good and bad areas in the OP's pic under a high power microscope to see whether it's impurities or just poor crystal formation.

"seed crystals" are used extensively in production crystallization, I wonder if a bit of crushed shatter sprinkled on the slab might help to get a consistent output.

Humidity content seems to have a significant effect, and as the quote from GW above states, the less water the better. If you are in a location with high humidity flushing your oven with inert gas may help.

RB

Gray Wolf · Jun 2, 2015

HG23 said:
Here is a post by GW from earlier this year that I found very interesting. Maybe he can drop in and elaborate if at all possible. I have made some very nice oleoresins but been frustrated to go out to the oven and see them autobuddering. I have been heavily considering adding addition dewaxing capabilities to my setup to try and combat it. I run subzero so I haven't considered extra dewaxing measures necessary, but if it will reduce the instances of waxing I'll try.

I do a pretty good job keeping the tubes vacced and below freezing before extractions but have been wondering about what happens when I'm vapor assisting the liquid butane out of the column because it raises the temp above freezing. Same thing as when some people use their heat mats. Do these practices release too much water into the extracts?

Nucleation points are points that crystals grow from. As RB suggests, they act as seeds for the crystals.

It can be fines in your concentrate, or as simple as a minute positive sticking up from the surface the concentrate is on.

Fines from inadequate filtering and plant waxes are two major players.

Wax is a hydrate, so it needs water from somewhere. The more abundant the water is, the easier it is to form hydrates.

noprohibir · Jun 3, 2015

Thanks guys. (Yes this thread is title 'nucleation' not 'auto-buddering'.)

Initially I was curious if residual butane could create a nucleation point, but I learned more. I think in this case it was a humid day: Hydrate. It's not growing very fast, so hopefully the damage will be minimal.

I was looking at high powered microscopes last week. Expensive. Especially with the digital camera. Whoa......A microscopic time-lapsed video from nucleation point to full auto-budder... Sweet.

Thank you again for the knowledge, Senor's. Back to the books!

SkyHighLer · Jun 3, 2015

noprohibir said:
Thanks guys. (Yes this thread is title 'nucleation' not 'auto-buddering'.)

Initially I was curious if residual butane could create a nucleation point, but I learned more. I think in this case it was a humid day: Hydrate. It's not growing very fast, so hopefully the damage will be minimal.

I was looking at high powered microscopes last week. Expensive. Especially with the digital camera. Whoa......A microscopic time-lapsed video from nucleation point to full auto-budder... Sweet.

Thank you again for the knowledge, Senor's. Back to the books!

I miss FatherEarth... microscopic pictures of crystal formations,

https://www.icmag.com/ic/showpost.php?p=5976582&postcount=350

justintime420 · Jun 3, 2015

Also had the experience of heating and pressing the nucleation spot between a heated surface and parchment. Does not always work but I have cleaned up a few spots with heat and pressure

HG23 · Jun 4, 2015

What is Wolf Wurx currently doing to filter extractions? Right now I'm just using wadded up coffee filters in the tubes but have been contemplating the filter stacks I see several vendors using that have a lab filter and a pressure fitted ring. What are people's experiences with these stacks, worth it? I do get some visible debris in my scraped portions these days.

I am also not doing any winterizing at this time. Has anyone ever had a winterized slab budder up? Does that happen? It seems winterization definitely removes the most waxes so that would be an interesting piece of information as to what is the biggest contributing factor to wax/crystal formation.

It's tough to iron out the propensity to auto budder. I just did a run of 4 separate strains, trim and nuggets with the same solvent under the same environmental conditions. The nicest trim run buddered quickly and is about 60% buddered, the next trim run looks great with no budder, and the nug runs are pretty good with slight buddering starting just now on one of them.

I'm thinking about adding increased particulate filtering and SSD capabilities along with a WolfWorx water filter to my setup but that will all take time and money.

Gray Wolf · Jun 5, 2015

HG23 said:
What is Wolf Wurx currently doing to filter extractions? Right now I'm just using wadded up coffee filters in the tubes but have been contemplating the filter stacks I see several vendors using that have a lab filter and a pressure fitted ring. What are people's experiences with these stacks, worth it? I do get some visible debris in my scraped portions these days.

I am also not doing any winterizing at this time. Has anyone ever had a winterized slab budder up? Does that happen? It seems winterization definitely removes the most waxes so that would be an interesting piece of information as to what is the biggest contributing factor to wax/crystal formation.

It's tough to iron out the propensity to auto budder. I just did a run of 4 separate strains, trim and nuggets with the same solvent under the same environmental conditions. The nicest trim run buddered quickly and is about 60% buddered, the next trim run looks great with no budder, and the nug runs are pretty good with slight buddering starting just now on one of them.

I'm thinking about adding increased particulate filtering and SSD capabilities along with a WolfWorx water filter to my setup but that will all take time and money.

We use wads of coffee filters. Never had any winterized oil budder.

noprohibir · Jun 7, 2015

Gray Wolf said:
We use wads of coffee filters. Never had any winterized oil budder.

Coffee filters are the way to go. But I do have to ask, GW, whats your opinion on a buchner funnel? Does the benefit out way the cost?

I guess it would be another preference situation. I ask only because I have used one in community college gen chemistry one, but not in 'this' particular case. I have been thinking of investing in one but don't know if its worth the expense.

What's the general opinion?

Gray Wolf · Jun 7, 2015

noprohibir said:
Coffee filters are the way to go. But I do have to ask, GW, whats your opinion on a buchner funnel? Does the benefit out way the cost?

I guess it would be another preference situation. I ask only because I have used one in community college gen chemistry one, but not in 'this' particular case. I have been thinking of investing in one but don't know if its worth the expense.

What's the general opinion?

I love our Buchner funnels and use them during winterizing.

For inline dewaxing, the Mk III I'm building uses a 1 micron sock filter from the biodiesel trades.

ThaDocta · Jun 7, 2015

If I take trim bin kif of a really terpy strain and rosin it, it will budder within 3 days.

HG23 · Jun 21, 2015

Gray Wolf said:
We use wads of coffee filters. Never had any winterized oil budder.

Thanks for that. So it would make sense that the lipids removed during winterization are, as you already said, a strong factor in the tendancy to budder.

I'm really trying to minimize buddering without resorting to a full scale winterization to retain the max amount volatiles and flavor in my end product. I already run subzero solvent and get the columns down to about -35C on the outside when running. I'm planning to add the WolfWurx designed water trap and add some form of dewaxing while the oil is still in hydrocarbon solution. I know that winterizing is the most complete way to destearinate, but if I can still get a product that's clear and brittle and stays that way a higher percentage of the time, but still has that extra nose on it, I'll be happy. If buddering is a wax/oil hydrate, hopefully this plan of attack will work. What do you all think?

Foxfur · Jul 12, 2015

Once I tried winterizing I was hooked. That and post-filtration with .4 & .2 32/33mm syringe filters from eBay.
I've had no buddering since.
Glad I found this thread, there's a stash of kif that might soon meet its doom.

HG23 · Jul 13, 2015

Can you elaborate a little more on your reasoning?

Gray Wolf · Jul 14, 2015

HG23 said:
Thanks for that. So it would make sense that the lipids removed during winterization are, as you already said, a strong factor in the tendancy to budder.

I'm really trying to minimize buddering without resorting to a full scale winterization to retain the max amount volatiles and flavor in my end product. I already run subzero solvent and get the columns down to about -35C on the outside when running. I'm planning to add the WolfWurx designed water trap and add some form of dewaxing while the oil is still in hydrocarbon solution. I know that winterizing is the most complete way to destearinate, but if I can still get a product that's clear and brittle and stays that way a higher percentage of the time, but still has that extra nose on it, I'll be happy. If buddering is a wax/oil hydrate, hopefully this plan of attack will work. What do you all think?

If you are already extracting at subzero temperatures, your water pickup will be minimal, so I would hold off on the trap and just use a dryer.

WolfWurx is still in fore line trap prototype stage, but after beta testing I'll pass on how well Plan C works.

As far as in-line dewaxing, Graywolf Creations, Inc and Sweetleaf have agreed to corroborate on a Mk VIII dewaxing column build and I'll pass on the results.

In a nut shell, we plan to chill the butane/oil mix and pull it through a 4" X 8" 1 micron sock filter full of glass/other beads.

We're building our own stainless filter case for the sock filter, as well as the rest of the stainless ancillaries, but the design is simple.

Soak and chill tank, conical bottom, valve, sock filter case, recovery tank. Here is an original conceptual design.

Nucleation

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