45 hour long low purge(B Mav) vs. 45 min fast purge method(GW). Also 30inHg too much?

M

MinnesotaHomegrown303

Active Member
Been experimenting with my BVV passive closed loop and HFS .9 CF vac oven for the past few weeks and am wondering what peoples opinions on purge methods for shatter are.

The brett mav type method is the long 90-100 purge for days, I know he leaves his vac pulling for 2 hour periods with no bleed valve(30inHg) then closes the valve and leaves the vac for 12 hour periods(mine always seems to stop reacting shortly after the pump is cut off so this seems pointless to me).

The Grey Wolf method claims to pull most of the butane within 45 minutes by pulling 29.5inHg @ 115 until most solvent bubbles stop(bleeding nitrogen or atmosphere in so that the vaccum is not too deep, I would really love to know how this is accomplished).

Obviously these methods are vastly different and neither is seeming to work very well for me. I have no bleed valve and have been experimenting with running my vacuum for hours at 95(30inHg) only to find that my patty stays inflated and pops extremely slowly if at all,(should I increase temps and wait for reaction to stop rather than deflate with solvent bubbles unpopped or are these bubbles due to the extremely deep vac?) and at a certain point the beautiful clear amber will begin to nucleate before it becomes hard(thinking this particular problem is just one strain I have but unsure). On the other side of the spectrum the issue I run into is apparent decarb happening when I approach 110 under hard vac(intense fast paced bubbling makes this obvious) which makes the GW method impossible to me to test. 110 is much too hot 90 is much too low and 100 does not seem to change much. Am I pulling too deep of a vac to achieve the desired results of either method? I have turned one strain into a nasty brown wax and never went over 110, no amount of purging can dry/stabilize it, and from the same strain I made some beautiful glass. Currently I have a muffin at 96 F that has been flipped once and is now stuck muffined up after 3 hours of vac with pump running on each side, should I deflate and flip or raise temps until reaction stops and muffin deflates before removing from the oven? I would leave it longer but it seems the large bubbles are endless and extremely slow to pop(after 3 hours with pump running it is still a muffin or large bubbles)

I am at 5000ft above sea level, the temp is oil temp, not oven and I am running the solvent(n butane) through sub zero, freezing my dehydrated trim before the run, and recovering at 80f. I am not asking for anyone to hand me information please keep your opinion to yourself if you are going to tell me to do my research, I have 132 book marks relating to this and have been practicing for months. I am seeking specific answers. Also whenever I pull my initial muffin even with no heat it will not stay inflated longer than it takes to get to full vac which makes me wonder why I can hold a slight muffin with full vac @ 95. My gut feeling is that @ that deep of a vac (30inHg) and my current temps that the bubbles whether solvent, c02, terps, ect will continue to create a muffin as long as the pump is on(two stage 3 cfm harbor freight pump 20 micron). I'm going to flip then kick it up to 100 before I pass out but if anyone has any input or advice I would greatly appreciate some second opinions. 45 minutes and 45 hours could not be further apart I don't see how they claim to have similar results as neither currently works for me.
 
M

MinnesotaHomegrown303

Active Member
Inconsistent results with consistent methods are driving me nuts not to mention every strain acts different so by the time I hone in on the correct method for one I'm already on to the next. Any words of wisdom or fingers pointed in a helpful direction are welcome.
 
Fadedawg

Fadedawg

Well-Known Member
MinnesotaHomegrown303 said:
Been experimenting with my BVV passive closed loop and HFS .9 CF vac oven for the past few weeks and am wondering what peoples opinions on purge methods for shatter are.

The brett mav type method is the long 90-100 purge for days, I know he leaves his vac pulling for 2 hour periods with no bleed valve(30inHg) then closes the valve and leaves the vac for 12 hour periods(mine always seems to stop reacting shortly after the pump is cut off so this seems pointless to me).

The Grey Wolf method claims to pull most of the butane within 45 minutes by pulling 29.5inHg @ 115 until most solvent bubbles stop(bleeding nitrogen or atmosphere in so that the vaccum is not too deep, I would really love to know how this is accomplished).

Obviously these methods are vastly different and neither is seeming to work very well for me. I have no bleed valve and have been experimenting with running my vacuum for hours at 95(30inHg) only to find that my patty stays inflated and pops extremely slowly if at all,(should I increase temps and wait for reaction to stop rather than deflate with solvent bubbles unpopped or are these bubbles due to the extremely deep vac?) and at a certain point the beautiful clear amber will begin to nucleate before it becomes hard(thinking this particular problem is just one strain I have but unsure). On the other side of the spectrum the issue I run into is apparent decarb happening when I approach 110 under hard vac(intense fast paced bubbling makes this obvious) which makes the GW method impossible to me to test. 110 is much too hot 90 is much too low and 100 does not seem to change much. Am I pulling too deep of a vac to achieve the desired results of either method? I have turned one strain into a nasty brown wax and never went over 110, no amount of purging can dry/stabilize it, and from the same strain I made some beautiful glass. Currently I have a muffin at 96 F that has been flipped once and is now stuck muffined up after 3 hours of vac with pump running on each side, should I deflate and flip or raise temps until reaction stops and muffin deflates before removing from the oven? I would leave it longer but it seems the large bubbles are endless and extremely slow to pop(after 3 hours with pump running it is still a muffin or large bubbles)

I am at 5000ft above sea level, the temp is oil temp, not oven and I am running the solvent(n butane) through sub zero, freezing my dehydrated trim before the run, and recovering at 80f. I am not asking for anyone to hand me information please keep your opinion to yourself if you are going to tell me to do my research, I have 132 book marks relating to this and have been practicing for months. I am seeking specific answers. Also whenever I pull my initial muffin even with no heat it will not stay inflated longer than it takes to get to full vac which makes me wonder why I can hold a slight muffin with full vac @ 95. My gut feeling is that @ that deep of a vac (30inHg) and my current temps that the bubbles whether solvent, c02, terps, ect will continue to create a muffin as long as the pump is on(two stage 3 cfm harbor freight pump 20 micron). I'm going to flip then kick it up to 100 before I pass out but if anyone has any input or advice I would greatly appreciate some second opinions. 45 minutes and 45 hours could not be further apart I don't see how they claim to have similar results as neither currently works for me.
Click to expand...
45 minutes is for a thin film in a 6" Petri dish. Larger, deeper films take longer. A full sheet typically takes all day.

I stick a thin film of the material into an oven preheated to what ever temperature it takes to maintain 115F at the puddle.

When the material liquefies, I start pulling a vacuum and when I see a flurry of bubbles, I hold the vacuum at that level until the flurries subside, and then continue pumping until I reach about -29.5" and it no longer flurries.

I then take it out of the oven, cool it in the freezer until I can flip it, and stick it back in the oven and repeat, until it no longer flurries and then continue to vacuum until the solvent bubbles stop.

115F the average temperature, but if you watch the puddle, you can tell when the surface tension is too high for the bubbles to burst, and raise it some.
With ethanol, I sometimes bump the vacuum level enough to deflate the humongous bubbles it blows, rather than cranking the temperature up higher than about 130F. I just bleed in enough nitrogen for them to collapse, and then close the bleed and pull it back down.

Once you reach -29.5" with no flurries, and the pump starts to pump lower, you can keep the vacuum levels at -29.5" by bleeding a small amount nitrogen into the oven while the pump continues to run.

An oven typically has a vent to allow you to equalize it enough to open the door, and if you pull the sheet metal off, you should be able to reach the valves and plumbing involved, so as to be able to tap in to it.
 
M

MinnesotaHomegrown303

Active Member
Fadedawg said:
45 minutes is for a thin film in a 6" Petri dish. Larger, deeper films take longer. A full sheet typically takes all day.

I stick a thin film of the material into an oven preheated to what ever temperature it takes to maintain 115F at the puddle.

When the material liquefies, I start pulling a vacuum and when I see a flurry of bubbles, I hold the vacuum at that level until the flurries subside, and then continue pumping until I reach about -29.5" and it no longer flurries.

I then take it out of the oven, cool it in the freezer until I can flip it, and stick it back in the oven and repeat, until it no longer flurries and then continue to vacuum until the solvent bubbles stop.

115F the average temperature, but if you watch the puddle, you can tell when the surface tension is too high for the bubbles to burst, and raise it some.
With ethanol, I sometimes bump the vacuum level enough to deflate the humongous bubbles it blows, rather than cranking the temperature up higher than about 130F. I just bleed in enough nitrogen for them to collapse, and then close the bleed and pull it back down.

Once you reach -29.5" with no flurries, and the pump starts to pump lower, you can keep the vacuum levels at -29.5" by bleeding a small amount nitrogen into the oven while the pump continues to run.

An oven typically has a vent to allow you to equalize it enough to open the door, and if you pull the sheet metal off, you should be able to reach the valves and plumbing involved, so as to be able to tap in to it.
Click to expand...
Thank you! One more question, At 100F and 30Hg do I run the risk of decarbing my oil? I noticed that it was harder earlier before this last flip and has gotten quite sticky since sitting in the oven for a few hours with my pump going. It is clear and smells great but is just as sticky as when I first scraped it now and has been purging a 100 with the pump on for at least 6 hours. I was under the impression it would take a while to harden but it seems maybe I have been over purging it and causing it to become unstable with too high of a vac and too long. Maybe next time I should half my time between each flip and check consistency before returning to the oven?
 
M

MinnesotaHomegrown303

Active Member
The slab is around 20g and appears to still slowly be releasing large rainbow solvent bubbles even after 7-8 hours 95 increased to 100 and 3 flips. When the vac was released last time(bubbles would not pop @ full vac with pump running and 100F, decided to flip and raise temp)it left rainbow like trails on top of the oil which I believe is solvent. I plan on getting my bleed system set up before next run but I wonder why there is little to no mention of 29.5 vs 30Hg and what the same temps at respective vac does to each. I would be Extremely interested to see as it would seem half of the people who use vac pumps just leave them running with no regard to the exact level achieved.
 
M

MinnesotaHomegrown303

Active Member
Fadedawg said:
45 minutes is for a thin film in a 6" Petri dish. Larger, deeper films take longer. A full sheet typically takes all day.

I stick a thin film of the material into an oven preheated to what ever temperature it takes to maintain 115F at the puddle.

When the material liquefies, I start pulling a vacuum and when I see a flurry of bubbles, I hold the vacuum at that level until the flurries subside, and then continue pumping until I reach about -29.5" and it no longer flurries.

I then take it out of the oven, cool it in the freezer until I can flip it, and stick it back in the oven and repeat, until it no longer flurries and then continue to vacuum until the solvent bubbles stop.

115F the average temperature, but if you watch the puddle, you can tell when the surface tension is too high for the bubbles to burst, and raise it some.
With ethanol, I sometimes bump the vacuum level enough to deflate the humongous bubbles it blows, rather than cranking the temperature up higher than about 130F. I just bleed in enough nitrogen for them to collapse, and then close the bleed and pull it back down.

Once you reach -29.5" with no flurries, and the pump starts to pump lower, you can keep the vacuum levels at -29.5" by bleeding a small amount nitrogen into the oven while the pump continues to run.

An oven typically has a vent to allow you to equalize it enough to open the door, and if you pull the sheet metal off, you should be able to reach the valves and plumbing involved, so as to be able to tap in to it.
Click to expand...
Would I accomplish this by adding a valve to
Fadedawg said:
45 minutes is for a thin film in a 6" Petri dish. Larger, deeper films take longer. A full sheet typically takes all day.

I stick a thin film of the material into an oven preheated to what ever temperature it takes to maintain 115F at the puddle.

When the material liquefies, I start pulling a vacuum and when I see a flurry of bubbles, I hold the vacuum at that level until the flurries subside, and then continue pumping until I reach about -29.5" and it no longer flurries.

I then take it out of the oven, cool it in the freezer until I can flip it, and stick it back in the oven and repeat, until it no longer flurries and then continue to vacuum until the solvent bubbles stop.

115F the average temperature, but if you watch the puddle, you can tell when the surface tension is too high for the bubbles to burst, and raise it some.
With ethanol, I sometimes bump the vacuum level enough to deflate the humongous bubbles it blows, rather than cranking the temperature up higher than about 130F. I just bleed in enough nitrogen for them to collapse, and then close the bleed and pull it back down.

Once you reach -29.5" with no flurries, and the pump starts to pump lower, you can keep the vacuum levels at -29.5" by bleeding a small amount nitrogen into the oven while the pump continues to run.

An oven typically has a vent to allow you to equalize it enough to open the door, and if you pull the sheet metal off, you should be able to reach the valves and plumbing involved, so as to be able to tap in to it.
Click to expand...
In the internals of my oven under the metal door I find a wishbone shaped hose leading from the metal hose attached to the vacuum and the oven. The two tubes that go from this metal hose are rubber and lead to the bleed valve and the gauge. Is this where I would install my bleed valve? And if so where do I find such a device that will bleed nitrogen in and maintain the levels I am seeking?
 

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Bublonichronic

Bublonichronic

Well-Known Member
I feel like I get a better end product by using slightly more heat and less time under vac, and if it's sticky after the solvent is gone that's a good thing, a lot of teerrps with do that I really don't understand why people think shatter is better a obvious way of looking at it is take some shatter then add some extra terps to it, what do you get a stinky sticky sap
 
M

MinnesotaHomegrown303

Active Member
Bublonichronic said:
I feel like I get a better end product by using slightly more heat and less time under vac, and if it's sticky after the solvent is gone that's a good thing, a lot of teerrps with do that I really don't understand why people think shatter is better a obvious way of looking at it is take some shatter then add some extra terps to it, what do you get a stinky sticky sap
Click to expand...
It depends on the material I run but it is usually bend and snap or yes a very nice smelling amber sap. Sometimes it will nucleate and become brown but will never seem to wax up. If that happens I winterize and purge the everclear out leaving me with a semi sticky/very sticky sap that is a beautiful color. Seems odd to me that I get anything brown as a run sub zero N tane through my closed loop a majority of the time to avoid pulling waxes and fats in the first place. I agree with you I like the sap but my associates prefer a more stable and easy to handle product. Higher temps and less vac? Do you have a rough temp/time you would suggest I test? Thanks!
 
Fadedawg

Fadedawg

Well-Known Member
MinnesotaHomegrown303 said:
Thank you! One more question, At 100F and 30Hg do I run the risk of decarbing my oil? I noticed that it was harder earlier before this last flip and has gotten quite sticky since sitting in the oven for a few hours with my pump going. It is clear and smells great but is just as sticky as when I first scraped it now and has been purging a 100 with the pump on for at least 6 hours. I was under the impression it would take a while to harden but it seems maybe I have been over purging it and causing it to become unstable with too high of a vac and too long. Maybe next time I should half my time between each flip and check consistency before returning to the oven?
Click to expand...
There is decarboxylation going on at room temperature, but not a lot until you get above 140F, but the solvent can't typically readily escape at 100F. I use 115F to liquify the puddle, and shorten the purge time.
 
Fadedawg

Fadedawg

Well-Known Member
MinnesotaHomegrown303 said:
Would I accomplish this by adding a valve to


In the internals of my oven under the metal door I find a wishbone shaped hose leading from the metal hose attached to the vacuum and the oven. The two tubes that go from this metal hose are rubber and lead to the bleed valve and the gauge. Is this where I would install my bleed valve? And if so where do I find such a device that will bleed nitrogen in and maintain the levels I am seeking?
Click to expand...
The beige hose is ostensibly your oven back fill line. You can tee in there.

We use a nitrogen bottle regulated down to about 10 psi and a needle valve. A plug valve will also work, but not as well, and a ball valve doesn't meter well at all. Mostly off, cracked slightly, and on.
 
Fadedawg

Fadedawg

Well-Known Member
Bublonichronic said:
no point me givng advice FD is here, id listen to him if i were me...
Click to expand...
If Fadedawg/Graywolf are the voice from the mountain, we are in deep doo.

He/they/moi, is a student himself (themselves?), and regularly trolls forums like this one for clues guiding experimentation. Trust me when I say I/he/they, don't have all the answers and learn a lot from the experience of others, so please do share freely.
 
M

MinnesotaHomegrown303

Active Member
Fadedawg said:
If Fadedawg/Graywolf are the voice from the mountain, we are in deep doo.

He/they/moi, is a student himself (themselves?), and regularly trolls forums like this one for clues guiding experimentation. Trust me when I say I/he/they, don't have all the answers and learn a lot from the experience of others, so please do share freely.
Click to expand...
Great advice. I sincerely appreciate all the help and hope to contribute to something of the sort in the future!
 
Bublonichronic

Bublonichronic

Well-Known Member
Fadedawg said:
If Fadedawg/Graywolf are the voice from the mountain, we are in deep doo.

He/they/moi, is a student himself (themselves?), and regularly trolls forums like this one for clues guiding experimentation. Trust me when I say I/he/they, don't have all the answers and learn a lot from the experience of others, so please do share freely.
Click to expand...
Modesty is a good quality to have
 
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