winterizing BHO

[MMAjay420]

im hoping this isnt a stupid question BUT can I winterize with 100 proof smirnoff?

 

[Gray Wolf]

So to be clear here, once we have filtered out the waxes and we are left with our oil ethanol solution you guys are just vacuum purging at ambient temperatures? Would it not be advantageous to hold it around 100f with a hot plate or something? Or will I really end up with fully purged shatter if I just vac at room temp?

I vacuum at 115F and -29.5" Hg.

 

[Gray Wolf]

And I've seen people saying you need 15-65ml/g of oil before winterization. Is that really necessary? I have my oil completely dissolved in some amount less, is it possible I could be messing something up by not adding enough ethanol even if it appears to be dissolved?

I do it by eyeball at about 10:1. When frozen to 0F, it still needs to flow like alcohol, not oil.

 

[Gray Wolf]

im hoping this isnt a stupid question BUT can I winterize with 100 proof smirnoff?

Never tried it because of having to get rid of that much water later.

 

[Young Bull]

I vacuum at 115F and -29.5" Hg.

I'm not sure where to post this, I'm just not having any luck getting shatter.

I'm extracting with an MKIIIa, I pack my columns to the right density, chill them before if I have time. I keep my butane tank just sitting inside of a deep freezer, no bath or dry ice, maybe that is part of my problem?

I keep the collection chamber in a water bath of 115f, in the winter I was having problems with the process coming to a stop from cold weather, and my machine frozen to the ground from trying to check the frost line with water and then that water freezing to the ground. Now that the weather is nicer I could get rid of it, maybe that is part of my problem?

When extracting I do one fill and overflow, pump it down to -10, then overflow and pump down to -10 2 or 3 more times and then following with a dump/shower. I've experimented with less butane washes and only ended up with less oil, not better oil so I don't really think that is the problem but I'm trying to provide as many details about my process as I can.

My starting material is not the freshest but not that old. I don't grow it so I don't have as much control over that timing but its never more than a month old. I don't crush or grind the trim, just pack it in.

after my dump and the recovery pump has pulled down to -22ish I switch to the high vacuum pump and just let that go for a while. Then I crack it open and pour in my Ethanol, Everclear 190 proof. I swish the container around using my water bath to help melt the oil into the ethanol. Then I pour it into a glass flask and into the deep freeze for 48 hours.

Then I use my vacuum assisted büchner funnel with whatman #1 lab filters. So far the wax I've pulled out has been a different color and consistency every time, ranging from creamy white, to nasty brown.

I then pour the filtered solution into a Pyrex for evaporating. Now I have tried this a few different ways with pretty much the same results every time.

I've cold boiled at 100f through 115f under the full vacuum force of the CPS 6.2 CFM. I've built a cold trap and it always pulls yellow ethanol so I know I'm pulling some cannabinoids and have been thinking about adding a bleeder to my vac chamber for when cold boiling.

But I've also tried ambient evaporating and evaporating at 100f through 115f.

Once it has been reduced to a thick viscous oil I pour/scrape/squeegee the oil onto parchment paper.

Then its into the vacuum chamber for purging. But no matter how long or at what temperature I try to purge it at I always end up with sappy sticky oil. This last batch is the worst yet seeming almost completely decabolated somehow. It also leaves an astonishing amount of nasty black stuff in the bottom of my nail. Not just a coating but a big nasty chunk of black shit. What is all that? I thought by winterizing I would have a pretty clean product.

My vacuum chamber consists of a stainless steel stock pot that has a thick 3 layer designed base to distribute heat evenly, I've insulated the whole thing with a shit ton of duct wrap insulation. It has an almost 2 inch thick poly lid that I imagine acts as a pretty good insulator. my heating element is a nu-wave induction pro cook top. It has 5 degree variations and a 99 hour timer. I've had a lot of people tell me the only thing they can think could be wrong could be my heat source (including Joe from SP). But it is always so very close to what I set it almost immediately after I set it. Without any fluctuation to speak of. It really does produce a steady even heat it just seems hard for me to believe this is the source of my problem. Regardless I've talked to a counter store and they are making me a custom 6 cm granite slab to sit in the bottom of the chamber and I plan to upgrade to an oven when I can afford it.

But I just can't seem to figure out what I'm doing wrong. And its too expensive to just keep experimenting. As far as I can tell the main differences between me and most other close loopers is the lack of an alcohol/dry ice bath, and a nice vacuum oven to finish in. I've still got over 3K sunk into this so far and haven't made any oil I'm proud of. I cant begin to explain how frustrating this is. Any help at all you guys could offer I would appreciate so much. I can answer any questions and try to provide pics if they will help.

 

[Gray Wolf]

I'm not sure where to post this, I'm just not having any luck getting shatter.

I'm extracting with an MKIIIa, I pack my columns to the right density, chill them before if I have time. I keep my butane tank just sitting inside of a deep freezer, no bath or dry ice, maybe that is part of my problem?

I keep the collection chamber in a water bath of 115f, in the winter I was having problems with the process coming to a stop from cold weather, and my machine frozen to the ground from trying to check the frost line with water and then that water freezing to the ground. Now that the weather is nicer I could get rid of it, maybe that is part of my problem?

When extracting I do one fill and overflow, pump it down to -10, then overflow and pump down to -10 2 or 3 more times and then following with a dump/shower. I've experimented with less butane washes and only ended up with less oil, not better oil so I don't really think that is the problem but I'm trying to provide as many details about my process as I can.

My starting material is not the freshest but not that old. I don't grow it so I don't have as much control over that timing but its never more than a month old. I don't crush or grind the trim, just pack it in.

after my dump and the recovery pump has pulled down to -22ish I switch to the high vacuum pump and just let that go for a while. Then I crack it open and pour in my Ethanol, Everclear 190 proof. I swish the container around using my water bath to help melt the oil into the ethanol. Then I pour it into a glass flask and into the deep freeze for 48 hours.

Then I use my vacuum assisted büchner funnel with whatman #1 lab filters. So far the wax I've pulled out has been a different color and consistency every time, ranging from creamy white, to nasty brown.

I then pour the filtered solution into a Pyrex for evaporating. Now I have tried this a few different ways with pretty much the same results every time.

I've cold boiled at 100f through 115f under the full vacuum force of the CPS 6.2 CFM. I've built a cold trap and it always pulls yellow ethanol so I know I'm pulling some cannabinoids and have been thinking about adding a bleeder to my vac chamber for when cold boiling.

But I've also tried ambient evaporating and evaporating at 100f through 115f.

Once it has been reduced to a thick viscous oil I pour/scrape/squeegee the oil onto parchment paper.

Then its into the vacuum chamber for purging. But no matter how long or at what temperature I try to purge it at I always end up with sappy sticky oil. This last batch is the worst yet seeming almost completely decabolated somehow. It also leaves an astonishing amount of nasty black stuff in the bottom of my nail. Not just a coating but a big nasty chunk of black shit. What is all that? I thought by winterizing I would have a pretty clean product.

My vacuum chamber consists of a stainless steel stock pot that has a thick 3 layer designed base to distribute heat evenly, I've insulated the whole thing with a shit ton of duct wrap insulation. It has an almost 2 inch thick poly lid that I imagine acts as a pretty good insulator. my heating element is a nu-wave induction pro cook top. It has 5 degree variations and a 99 hour timer. I've had a lot of people tell me the only thing they can think could be wrong could be my heat source (including Joe from SP). But it is always so very close to what I set it almost immediately after I set it. Without any fluctuation to speak of. It really does produce a steady even heat it just seems hard for me to believe this is the source of my problem. Regardless I've talked to a counter store and they are making me a custom 6 cm granite slab to sit in the bottom of the chamber and I plan to upgrade to an oven when I can afford it.

But I just can't seem to figure out what I'm doing wrong. And its too expensive to just keep experimenting. As far as I can tell the main differences between me and most other close loopers is the lack of an alcohol/dry ice bath, and a nice vacuum oven to finish in. I've still got over 3K sunk into this so far and haven't made any oil I'm proud of. I cant begin to explain how frustrating this is. Any help at all you guys could offer I would appreciate so much. I can answer any questions and try to provide pics if they will help.

A few thoughts starting from the top.

Heat transfer from your tank to the air in your freezer is far less than transfer to a liquid. You might put your tank into an antifreeze bath, regardless of how its cooled.

When using a freezer, if you have any leaks, the vapors can find its way to the electrical section, where it can find ignition.

The colder the butane during extraction, the less wax and other non-targeted elements are extracted and the lighter the color.

If you are going for shatter, leave the collection chamber out of the water bath, except for an occasional rinse to wash the ice off, so you can at what level it reforms. Heat at this stage at least partially decarboxylates the material.

When the ice is gone from the column and it doesn’t reform on the lower pot, plus the vacuum gauge reads ~22, you are done with recovery and can move to final high vacuum purge.

Soak and flood works well for extracting oil in the shortest time possible, but for best control making shatter and waxes, try timing your first flood until it over flows, and then dumping it out the bottom and flushing it with the top flood. You can experiment with soak times between the over flow, dump and rinse.

Leave the dump valve open during recovery to -10, which will freeze the material, and then close the dump valve and run the second flood/dump/rinse cycle.

The plant waxes are typically light beige, so the nasty dark brown suggest other polar elements present, or residual oil. What happens when you rinse the nasty brown stuff with fresh alcohol and re-filtering?

Nasty black stuff at the bottom of your nail, can either be a nail that isn’t hot enough, isn’t regularly burned out, or that the oil has longer chained, higher boiling point content, such as residual waxes, chlorophyll, water solubles, etc.

Whats left after an extended bright orange nail burnout?

How low is your freezer and are you also freezing your funnel, filters, etc? 0F is where I would recommend running both for 48 hours.

I would add a bleed valve on your chamber, so that you can control your vacuum levels to around 29.5” Hg.

Austenitic 18-8 Stainless is non magnetic, so I infer that the sandwich on the bottom of your pot addresses that issue, but without knowing how it is constructed, am just guessing what it might be.

It is hard to correlate the outside chamber temperature with the oil temperature without some experimentation to determine the delta-Temperature between them. You can do that with thermocouples or by measuring the outside of the chamber and then opening it and quickly measuring the oil temperature.

If you are using a chamber, you should have good contact between the product and the bottom, but without knowing how even the temperature measures along the bottom, there is no way of knowing how stable it is. I agree it would be good to add some thermal mass to even out the temperature.

 

[SkyHighLer]

"It is hard to correlate the outside chamber temperature with the oil temperature without some experimentation to determine the delta-Temperature between them. You can do that with thermocouples or by measuring the outside of the chamber and then opening it and quickly measuring the oil temperature."

"Reversible Temperature Labels, Multi Temp Liquid Crystal Strips

RLC-60-90/120-10 In Stock $13.00 16 Temperature Levels Label, 90 to 120°F/32 to 49°C (2°F increments) in package of 10"

http://www.omega.com/pptst/RLC-60.html

I stick one to my parchment paper in the vacuum chamber, it's removed and used over and over.

 

[Young Bull]

A few thoughts starting from the top.

Heat transfer from your tank to the air in your freezer is far less than transfer to a liquid. You might put your tank into an antifreeze bath, regardless of how its cooled.

When using a freezer, if you have any leaks, the vapors can find its way to the electrical section, where it can find ignition.

The colder the butane during extraction, the less wax and other non-targeted elements are extracted and the lighter the color.

I'm going to switch to an alcohol and dry ice bath this next run and see how things turn out. I only have standard hoses though, If I don't chill it all the way to the very top of the tank will it be okay?

If you are going for shatter, leave the collection chamber out of the water bath, except for an occasional rinse to wash the ice off, so you can at what level it reforms. Heat at this stage at least partially decarboxylates the material.

I'm also going to try again without water now that the weather is better and see how it goes.

When the ice is gone from the column and it doesn’t reform on the lower pot, plus the vacuum gauge reads ~22, you are done with recovery and can move to final high vacuum purge.

Soak and flood works well for extracting oil in the shortest time possible, but for best control making shatter and waxes, try timing your first flood until it over flows, and then dumping it out the bottom and flushing it with the top flood. You can experiment with soak times between the over flow, dump and rinse.

Leave the dump valve open during recovery to -10, which will freeze the material, and then close the dump valve and run the second flood/dump/rinse cycle.

The plant waxes are typically light beige, so the nasty dark brown suggest other polar elements present, or residual oil. What happens when you rinse the nasty brown stuff with fresh alcohol and re-filtering?

I don't know I've not tried that, I still have the nasty ball I could try and clean it up just to see.

Nasty black stuff at the bottom of your nail, can either be a nail that isn’t hot enough, isn’t regularly burned out, or that the oil has longer chained, higher boiling point content, such as residual waxes, chlorophyll, water solubles, etc.

Whats left after an extended bright orange nail burnout?

I get my nail red hot and let it cool down a bit before every dab, If I take the time to really blast it out with the torch and get it all at the right angle I can get it looking pretty clean but this last batch left more than any oil I've ever had. The only thing I can think of is my butane was too hot when extracting and I pulled a lot of shit I don't want.

How low is your freezer and are you also freezing your funnel, filters, etc? 0F is where I would recommend running both for 48 hours.

My deep freeze is kept around -20f and I chill the whole flask/funnel apparatus with the filter already in place for at least an hour before I filter the solution. The solution itself is always chilled for at least 48 hours. Sometimes upwards of a week before I can get to it.

I would add a bleed valve on your chamber, so that you can control your vacuum levels to around 29.5” Hg.

Have you done this before? Did you just use the standard chemistry equipment somehow mounted to your lid? The gauge I have is analog and not at all very accurate to read, I can't really tell the difference between 26 and 29, do you have a budget digital manometer you could recommend? Or at least a very accurate analog gauge?

Austenitic 18-8 Stainless is non magnetic, so I infer that the sandwich on the bottom of your pot addresses that issue, but without knowing how it is constructed, am just guessing what it might be.

I can't find my pot online so I can't link to it, but the base has an aluminum plate as the middle heat distribution layer, to be honest I don't recall the type of stainless it is but the entire pot is magnetic.

It is hard to correlate the outside chamber temperature with the oil temperature without some experimentation to determine the delta-Temperature between them. You can do that with thermocouples or by measuring the outside of the chamber and then opening it and quickly measuring the oil temperature.

If you are using a chamber, you should have good contact between the product and the bottom, but without knowing how even the temperature measures along the bottom, there is no way of knowing how stable it is. I agree it would be good to add some thermal mass to even out the temperature.

I have a digital meat thermometer that I place inside my chamber with the probe under the parchment, but placed so as not to keep any oil from creating contact with the bottom of the pot. I have already talked to a counter company and they are making me a real thick slab of granite that can sit right down in the bottom of my chamber and I'm saving up for an AI oven.

"It is hard to correlate the outside chamber temperature with the oil temperature without some experimentation to determine the delta-Temperature between them. You can do that with thermocouples or by measuring the outside of the chamber and then opening it and quickly measuring the oil temperature."

"Reversible Temperature Labels, Multi Temp Liquid Crystal Strips

RLC-60-90/120-10 In Stock $13.00 16 Temperature Levels Label, 90 to 120°F/32 to 49°C (2°F increments) in package of 10"

http://www.omega.com/pptst/RLC-60.html

I stick one to my parchment paper in the vacuum chamber, it's removed and used over and over.

This is a really good idea though, I have some of these from when I was growing mushrooms, they will be put in use when my wife demands her meat thermometer back for food lol


Who knows though guys, it could just be that radioactive oil is sappy, what with my chambers sight glass being from a closed down nuclear facility and all

 

[Young Bull]

When the ice is gone from the column and it doesn’t reform on the lower pot, plus the vacuum gauge reads ~22, you are done with recovery and can move to final high vacuum purge.

Soak and flood works well for extracting oil in the shortest time possible, but for best control making shatter and waxes, try timing your first flood until it over flows, and then dumping it out the bottom and flushing it with the top flood. You can experiment with soak times between the over flow, dump and rinse.

Leave the dump valve open during recovery to -10, which will freeze the material, and then close the dump valve and run the second flood/dump/rinse cycle.

I've been reading this part over again and I think I may have been misunderstanding you. When you are doing your initial flood and overflow are you pumping it down to -10 before you switch to dump and shower or are you waiting until after you finish your shower before you even pump -10 at all? If so I've been wasting a lot of time pumping down to -10 before my next overflow or dump/shower.

And then you would pump it all the way down to -22 before you put on the next tube? Or if you were putting on another tube would -10 be sufficient? I usually run a few tubes before I clean out but I've been pumping down to -22 in-between all tubes. If -10 is okay it would save me a lot of time.

Also what would you think the maximum amount of oil that would fit into the bottom of a 6" wide x 12" tall collection vessel? It has the standard mkiiia lid, just with a double tall spool. When you are pumping it down at the end with the high vacuum pump it muffins up pretty good. Has anyone figured out what the max that will fit is? The more tubes I can run before I have to clean out the bottom the better. But I don't want it all over the inside of the lid.

Thanks again!

 

[cwigg878]

Final Purging

Final Purging

I vacuum at 115F and -29.5" Hg.

I have an AI 1.9 cu ft oven with a 10 cfm robinair. I also am using a closed loop tamisium. I also have a freezer that runs to -30F. When I was using a smaller pot to vac purge my oil, I seemed to be getting a better end product (was shooting thru tubes at the time tho). Assuming its not my technique with the closed loop extraction (which i am not 100% sure on).

Whether winterizing with alcohol or butane only, I set the vac oven to 115F and bring the level to -29.5?

Do i shut off the pump when it reaches -29.5? Or Leave it running with the regulator set to -29.5? (also could you recommend a blead regulator and inline solvent filter for alcohol and butane vapor)

How long does it stay under vac for? Does it matter one continuous purge vs 5 at 20 min increments? Is it best to drop the heat or add heat for final purges?

Then when you pull it out the oven are you best to let it slowly cool or throw it in the freezer?

My pump should vac to 20 microns. Does a lower temp deeper purge remove more or damage the oil? Or even purging with little to no heat at higher neg pressures?

Also is the oven vacuum gauge accurate enough or is an inline one needed? if so could you recommend one?

I have been trying to keep up on all the threads. Sorry in advance if I repeated something. Thanks for the help

 

[Drosepro]

Can you winterize the oil is suspended in butane? For example sealing the jar before the butane evaporates and then freezing. Will the fats and lipids still congeal?

 

[SkyHighLer]

Can you winterize the oil is suspended in butane? For example sealing the jar before the butane evaporates and then freezing. Will the fats and lipids still congeal?

If you're referring to a glass jar like a Mason jar, they shouldn't be sealed up, you're at the burst strength of the glass, and the sealing ring also isn't up to it.

Never put an open container of butane in your refrigerator/freezer!

It was recently reported dry ice in an ice chest outside will work with a Mason jar containing your butane/oil solution, you could easily break the jar with these massive temperature shifts, so I'd recommend a stainless steel container of some sort.

Haven't tried it, though other's have...

 

[DRF]

You would need a reflux or fractionating still to produce >95% volume. Do a search online for the bokakob 2 mini-still column, to see a guide on how to construct your own mini-still. If you were going to use ethanol to do the primary extraction then I'd say that it is worth making your own ethanol but if it's just to redissolve BHO then you need so little that it's not really worth constructing a reflux still. In such a case, it would be alot simpler to buy a liter of 95% ethanol and recapture it during the purge, with a condenser.

How much water does the liquor pick up when condensed during the purge?

 

[Gray Wolf]

I'm going to switch to an alcohol and dry ice bath this next run and see how things turn out. I only have standard hoses though, If I don't chill it all the way to the very top of the tank will it be okay?

For optimum results, you will want the butane around -30C, which is too low for continuous exposure for most polymers.

If you are going to run at -30C, the -30C butane will be passing through the hose and seals, whether they are submerged in it, or not. I recommend stainless overbraided PTFE hoses with JIC connectors.

I'm also going to try again without water now that the weather is better and see how it goes.



I don't know I've not tried that, I still have the nasty ball I could try and clean it up just to see.



I get my nail red hot and let it cool down a bit before every dab, If I take the time to really blast it out with the torch and get it all at the right angle I can get it looking pretty clean but this last batch left more than any oil I've ever had. The only thing I can think of is my butane was too hot when extracting and I pulled a lot of shit I don't want.

Even if your oil only has a small amount, it will accumulate. Mechanically scraping the bulk off and turning the nail bright orange will remove all organics.

My deep freeze is kept around -20f and I chill the whole flask/funnel apparatus with the filter already in place for at least an hour before I filter the solution. The solution itself is always chilled for at least 48 hours. Sometimes upwards of a week before I can get to it.

Should be adequate.

Have you done this before? Did you just use the standard chemistry equipment somehow mounted to your lid? The gauge I have is analog and not at all very accurate to read, I can't really tell the difference between 26 and 29, do you have a budget digital manometer you could recommend? Or at least a very accurate analog gauge?

http://www.cpsproducts.com/pdf/FLY_VG2001.pdf

I can't find my pot online so I can't link to it, but the base has an aluminum plate as the middle heat distribution layer, to be honest I don't recall the type of stainless it is but the entire pot is magnetic.

If it is magnetic, it should work.

I have a digital meat thermometer that I place inside my chamber with the probe under the parchment, but placed so as not to keep any oil from creating contact with the bottom of the pot. I have already talked to a counter company and they are making me a real thick slab of granite that can sit right down in the bottom of my chamber and I'm saving up for an AI oven.



This is a really good idea though, I have some of these from when I was growing mushrooms, they will be put in use when my wife demands her meat thermometer back for food lol


Who knows though guys, it could just be that radioactive oil is sappy, what with my chambers sight glass being from a closed down nuclear facility and all

In blue.

 

[Gray Wolf]

I've been reading this part over again and I think I may have been misunderstanding you. When you are doing your initial flood and overflow are you pumping it down to -10 before you switch to dump and shower or are you waiting until after you finish your shower before you even pump -10 at all? If so I've been wasting a lot of time pumping down to -10 before my next overflow or dump/shower.

And then you would pump it all the way down to -22 before you put on the next tube? Or if you were putting on another tube would -10 be sufficient? I usually run a few tubes before I clean out but I've been pumping down to -22 in-between all tubes. If -10 is okay it would save me a lot of time.

Also what would you think the maximum amount of oil that would fit into the bottom of a 6" wide x 12" tall collection vessel? It has the standard mkiiia lid, just with a double tall spool. When you are pumping it down at the end with the high vacuum pump it muffins up pretty good. Has anyone figured out what the max that will fit is? The more tubes I can run before I have to clean out the bottom the better. But I don't want it all over the inside of the lid.

Thanks again!

We flood from the bottom, until it overflows, to establish how long it takes to push/pull one volume of butane through the system, at the different column packing rates and butane temperature.

We then use that flood rate to compute how many column volumes of butane we wish to put through the column from the bottom.

After flooding from the bottom for the desired amount of time, we open the column dump valve and rinse the column from the top, usually one column volume worth.

If we are running multiple floods on one column, or a Mk V with dual columns, we pull down to around -10" between floods if we are running blind, or with a lighted sight glass, when there is room in the lower tank for another flood.

The 10" is just a general indicator that the butane puddle is gone, when running blind. It no longer works well when using an unheated recovery pot.

We only recover to -22 at the end of the extraction, or between columns if we are extracting a series of columns without cleaning the pot.

At -22", 75% of the butane vapor is also gone, which is how far we pull down for column changes. Prior to changing the column, the Mk V floods the column with nitrogen and pumps it down to -29" using the high vacuum pump.

We also pump the new column down to -29" before venting it to the lower system sitting at -22" and subsequently flooding it.

How many columns you can run, is highly dependent on what you're running. I would run two and check, then adjust accordingly.

With prime material, I've filled a 6" X 6" pot with with two 24" column, so I suspect four might be a push on a 12" with some material.

Don't forget to extend your down tubes, using the taller spool, as dropping the liquid in mid tank, promotes pump liquid aspiration.

 

[Gray Wolf]

I have an AI 1.9 cu ft oven with a 10 cfm robinair. I also am using a closed loop tamisium. I also have a freezer that runs to -30F. When I was using a smaller pot to vac purge my oil, I seemed to be getting a better end product (was shooting thru tubes at the time tho). Assuming its not my technique with the closed loop extraction (which i am not 100% sure on).

Whether winterizing with alcohol or butane only, I set the vac oven to 115F and bring the level to -29.5?

Not sure what you mean about winterizing with butane, but for removing the alcohol, I usually rotovape or open evaporate the bulk of it away before sticking it in the vacuum oven in a thin film and finishing it off.

Alcohol is harder to remove than butane, so I use 120F as a good starting place and pull as full a vacuum as the pump is capable of, until vacuum levels reach the -29.5.-29.8" range, at which time it depends on which TVO-2 oven I'm using.

On our test oven, I bleed in N2 through the back fill valve, to keep the vacuum levels in check. Eloquentsolution just bleeds in atmosphere on her production oven, or uses the vacuum control with the bleed closed.

Do i shut off the pump when it reaches -29.5? Or Leave it running with the regulator set to -29.5? (also could you recommend a blead regulator and inline solvent filter for alcohol and butane vapor)

Google vacuum pump fore traps for a selection, but fore traps all reduce available performance at the oven or chamber itself. If you pull too low on the trap, it will boil off there as well, so you are at a compromise.

I recommend using a chemical duty vacuum pump on the oven, so it doesn't matter what you are putting through it. If you want what is in the stream, you can more easily trap it after the pump.

How long does it stay under vac for? Does it matter one continuous purge vs 5 at 20 min increments? Is it best to drop the heat or add heat for final purges?

Techniques abound, so I encourage you to read the threads on the subject.

The techniques for getting rid of alcohol are also different than for getting rid of butane.

When purging butane, I use 115F and -29.5", flipping every time the surge of bubbling ceases.

Then when you pull it out the oven are you best to let it slowly cool or throw it in the freezer?

When I'm flipping, I use the freezer to speed things up.

My pump should vac to 20 microns. Does a lower temp deeper purge remove more or damage the oil? Or even purging with little to no heat at higher neg pressures?

20 microns is ostensibly low enough to boil away the diterpenes at ambient temperatures, but we have yet to establish the temperature and pressure loss curves.

The residual gas analyzer on our test oven show that the terpenes start sublimating off below their calculated boiling points under vacuum, so there is concern with loss of diterpene cannabinoids.

I picked -29.5" Hg to give some margin to -29.8" Hg, based on a boiling point chart that was subsequently determined to be flawed, and opened the larger picture of vapor points, vis a vis boiling points.

We are hoping to have the loaner RSA MS back on the oven for further testing soon, and will endeveour to answer some of those questions.

Also is the oven vacuum gauge accurate enough or is an inline one needed? if so could you recommend one?

We get by with the ones on our Cascade TEK. CPS makes a digital that is not too spendy.

[FONT=&quot]http://www.cpsproducts.com/pdf/FLY_VG2001.pdf
[/FONT]


I have been trying to keep up on all the threads. Sorry in advance if I repeated something. Thanks for the help

More, shorter threads are less overwhelming and will get greater participation. I save long threads for last and often forget to get back to them.

 

[Gray Wolf]

Can you winterize the oil is suspended in butane? For example sealing the jar before the butane evaporates and then freezing. Will the fats and lipids still congeal?

If you dramatically drop the temperature of the butane, the heavier plant waxes will become less soluble and precipitate out.