Shatter??

[r543]

Ive been checking out on the net some interesting vac purge setups and wanted to see how tough it is to make Shatter. Anyone with experience? Any good shatter guides?? Found a youtube video that seems he just takes BHO and vacuum purges at a set temp for several hours....

http://www.youtube.com/watch?v=JtYnu_0y120

 

[Gray Wolf]

Ive been checking out on the net some interesting vac purge setups and wanted to see how tough it is to make Shatter. Anyone with experience? Any good shatter guides?? Found a youtube video that seems he just takes BHO and vacuum purges at a set temp for several hours....

http://www.youtube.com/watch?v=JtYnu_0y120

We like 115F at -29.5" Hg in a thin film, until the solvent bubbles cease.

 

[r543]

Hey Gray Wolf,

Thanks for the tips. Sadly my vac pump only goes to 28.5.

How do you measure the temp of the oil? Are you depresureizing mid purge to check temps?

Also anyone have experience using molds. I thought it would be interesting to make small discs or something of the like.

Ill post some pics later of my first attempt, still purging

 

[m314]

How do you measure the temp of the oil? Are you depresureizing mid purge to check temps?

Also anyone have experience using molds. I thought it would be interesting to make small discs or something of the like.

I use an infrared thermometer to check the temperature while it's still under vacuum. Someone with professional equipment can just set the temp with a vacuum oven.

With my last batch, I did the final purging step at 110 degrees in a little silicone concentrate jar. It came out as a perfect hard disc, like a coin only thicker. I have to heat up a little blade to cut pieces off for the vaporizer.

How it comes out depends partially on the strain and partially on how long the buds or trim have been curing. A different strain processed the same way a few weeks ago came out of the vacuum chamber as more of a wax.

 

[Gray Wolf]

Hey Gray Wolf,

Thanks for the tips. Sadly my vac pump only goes to 28.5.

How do you measure the temp of the oil? Are you depresureizing mid purge to check temps?

Also anyone have experience using molds. I thought it would be interesting to make small discs or something of the like.

Ill post some pics later of my first attempt, still purging

What altitude are you at?

We use a laser thermometer and watch the visual clues.

.

 

[vapeman24]

For the guys using a laser thermometer, how are you using it while the oil is still under vacuum? I thought you can't get a reading through glass/polycarbonate?

 

[Gray Wolf]

We can't, but after the set up stablizes, you can measure the heat source and open the unit up and measure a batch of oil, so as to know what the differential typically is.

Knowing the differential and watching what is actually happening, is enough for us to maintain our processes.

 

[r543]

Hey Graywolf, Im in Vancouver so basically sea level. I have been using a laser to test the bottom of the pot and know there is about a 15-25F differential to the oil.

First time using mostly bud I made a rock hard shatter then burnt it by accident. 2nd time I purged for over 48 hours and still couldn't get it rock hard. Is this a issue of over heating at somepoint? or strain? or both?

Im looking to make shatter like flint.

 

[r543]

l;

 

[r543]

The stuff I heated for 48 hrs was shatter like but soft for most of the purge until the end. it then became a honeycomb consistency, not sticky but not hard.

 

[Gray Wolf]

Hey Graywolf, Im in Vancouver so basically sea level. I have been using a laser to test the bottom of the pot and know there is about a 15-25F differential to the oil.

First time using mostly bud I made a rock hard shatter then burnt it by accident. 2nd time I purged for over 48 hours and still couldn't get it rock hard. Is this a issue of over heating at somepoint? or strain? or both?

Im looking to make shatter like flint.

The resin starts out as a carboxylic acid shatter, and softens with decarboxylation from heat.

We reliably produce room temperature shatter by purging in a thin film at 115F and -29.5" Hg until the solvent bubbles cease.

 

[r543]

THanks for the help Gray wolf! I tried a 3rd test this morning. Still ended up with a softer product but I think again this was due to over heating.

 

[r543]

are we talking under an hour time frames?

 

[StayHungry]

So I have a thermometer sitting underneath where my oil rests in the degassing chamber. It states it is running at 115 for bottom heat and that is when I put the oil in and purge. Now what I was wondering is this cooking the THC technically. Since the boiling points change with pressure etc.

I am currently trying two different things. One is heating at 115-120 in a separate chamber for 10 min then purging for 10 and repeat. The other is a constant heat of 110-120 over time while it degasses. My material is from this year, early depths. But it is coming out darker than I would like, whereas I have gotten better results with older stuff.

Before my methods were kinda a shot in the dark and I did everything off of feel. Now that I am trying to put numbers and time limits to things, my end products are not as shatter-y as they have been in the past and they are for sure darker. Been poking away at this now for a year and a half with consistent but not as nice colored product. I am striving to make the best medicine so I always figured time in a vacuum was my friend. I used to run 24-48 hours under no heat, while i pancake it onto itself and flip it every hour or two. So many variables, makes my head spin.

 

[narniachronic]

It depends what you mean by cooking the THC. If you are talking about whether you are boiling off the THC under your vacuum, it depends on what pressure your vacuum is at. Look at this chart on Grey Wolf's website:

http://skunkpharmresearch.com/vacuum-purging-and-processing-tips/

It shows how THC's boiling point changes with pressure. If you stay under THC's boiling point then the only thing you should be worrying about is the temperatures that cause decarboxylation, which is also explained here on the SkunkPharmResearch website:

http://skunkpharmresearch.com/decarboxylation/
(especially check the graph that has been posted here on IC before)

As far as I know, the temperatures you are working with (I see you were aiming at under 120 about) are pretty low for decarboxylation; I would think it would take a long time at those temperatures. But I am still learning too so please anyone correct me if I am wrong. Hope this helps at all. Check out the rest of that site if you haven't been on it before; Grey Wolf and the rest of the folks that put up that site are BOSSES. Thanks again for the knowledge Grey Wolf!

 

[jump117]

, the temperatures you are working with (I see you were aiming at under 120 about) are pretty low for decarboxylation; I would think it would take a long time at those temperatures. But I am still learning too so please anyone correct me if I am wrong.

Theoretically decarboxylation under vacuum should occur at lower temperatures than those on the chart, although specific values ​​of temperature and time depending on the vacuum has not yet been proposed.

 

[narniachronic]

jump117 for the clarification, after doing some re-thinking and more reading I think I understand it better. This was posted by Grey Wolf in a previous post and is helpful:

"We like thin film purging under vacuum and use 115F at -29.9" Hg for our oil. We use a laser pyrometer to keep track.

We picked that temperature by pulling a vacuum and slowly raising the temperature, until the bubbles break free. If your's aren't breaking free at 120F, you have some really thick oil, or perhaps the puddle isn't at the same temperature as what you're measuring.

I would start out by measuring the temperature of the puddle carefully with a laser thermometer, if you haven't already, and using it and the bubbles as your guide.

You can also just start slowly raising the temperature until the bubbles break free, by assuming that regardless of what the temperature might be, it isn't enough. That should work as well, but does expose you to some unknowns.

The more heat you use, the more decarboxylation will also occur and conversion of THC to CBN. If you wish to retain it in carboxylic acid form, you need to minimize heat input.

If you are making an oral med and need it decarboxylated anyway, I would cut to the chase and just drop a container with the oil in it, in a 250F hot oil bath to both purge and decarboxylate, and forget about the vacuum."

I also read on his website (the link with the chart I posted previously) that, "Note that at sea level, Delta 9 THC boils around 157C/315F.
Now look at what happens at -29.9196″ Hg, where Delta 9 THC is boiling at only minus -5C or 23F."

So I guess I am confused; does that mean no matter what we do in a vacuum, in order get to the point where we purge the butane, we are going to be boiling at least some THC off(because at a vac of -29.9, THC is boiling at 23F)? Does that mean there is a time limit at that vacuum level we should leave the oil in? (Sorry if I am re-asking the same question I tried to answer, I am slow at times )

 

[SkyHighLer]

115F down to -29.5" Hg... Here's why,
https://www.icmag.com/ic/showthread.php?p=5869346#post5869346

Imo, decarboxylation doesn't seem to be speeded up by lowering the pressure. The BHO lab results the MMJ dispensaries put online show both THC and THC-A percentages, and I only see about the same relative proportion of THC-A to THC, never anything close to all THC. These oils are vacuum purged, some of the waxes probably for days... Another thing, I recently purged some BHO for several hours trying to get rid of mercaptans, no little bubbles from CO2. I then decarbed it at ~250F, watching the bubbles, and it stopped bubbling only a few minutes short of the expected twenty-seven.

Here's a chart of the boiling points of THC under vacuum, calculated with the heat of evaporation for delta-9 THC equal to 66.49 kj/mol using this BP under vacuum calculator, http://www.trimen.pl/witek/calculators/wrzenie.html

 

[G.O. Joe]

So I guess I am confused; does that mean no matter what we do in a vacuum, in order get to the point where we purge the butane, we are going to be boiling at least some THC off(because at a vac of -29.9, THC is boiling at 23F)

The boiling point taken from the untrustworthy Russo and McPartland chart is wrong. I've gone over that before.

Only with rare equipment no lab has can such a boiling point (157C) theoretically be obtained, with pressure a handful of microns. I don't know who has claimed it, it's below any figure quoted by anyone else anywhere, at any pressure.

THC obviously has some vapor pressure when heated, and the lost THC in decarboxylation charts (at the highest temperature) not explained by increase in CBN content is mostly volatilization. The terpenes will go first, and the lightest ones will boil pretty low in that kind of vacuum.

Purging without vacuum by heating in air inevitably causes some oxidation and presumably terpene volatilization again; no free lunch. The vacuum at least prevents access to oxygen. Maybe a vacuum less hardcore and expensive and just less - like from a little Nalgene aspirator - eventually works as well for purging butane from slightly warmed BHO, but doesn't have such volatilization concerns.

 

[narniachronic]

Thank you SkyHighLer and G.O. Joe!