vac purge after extensive heat purge + sitting overnight?

[vbsponger]

It feels good to finally be able to post after all of the hours of reading. I hope i can get some good feedback as the google searches and forum threads are often subjective to the conditions of the entire process.

I dont know where to start (wish i had taken more pictures throughout my extraction and purging ), but i chopped up some flowers that had been already dried and cured. I then dehydrated this material in the oven at 100 - 105 degrees for 4-5 hours long. Packed the tubes tight and extracted onto a hot water bath outside. Sprayed until the liquid was no-longer yellow and was clear. Once there was no more liquid butane, i brought inside and put in the oven where it purged at a temp of 115 degrees for 5-7 hours roughly. I let the heat do it's thing naturally and did not whip oil to pop butane bubbles nor did i use a heat gun.

After the ~7hr purge, i took it off heat and scraped onto parchment paper. It was not even at this point on the parchment paper so i put the parchment paper with the pools of oil onto a presto griddle and heated it to about 110 degrees and let the oil become more viscous so i could make an even spread of it by tilting the paper different ways until the oil was spread evenly throughout the paper.

I would have put it into my vac chamber at this point, but the oil for my pump had not arrived so i could not use the vacuum to purge it further.

Instead of vacuum purging at this point, i took it off the heat and set the paper into a clean pyrex dish and put a lid on it so that it was 4/5 covered (left a little opening so it could breathe).

It sat for 10 hours in a dark area in my garage. It was a stable and crisp shatter consistancy. not too sticky. I will try to get a couple pics that i do have up momentarily as this is my first post and need to look further into how to do it. I have a picture taken after the heat purge before it sat for 10 hours and then the final product after it sat for 10 hours.

There is no sizzle, its a beautiful crystal clear amber/dark yellowish color and tastes amazing.

I suppose here comes my question,
since i let it sit out for 10 hours like that (no heat, just at room/garage temp ), what is the best way to finalize this and vacuum it to purge the rest of the butane out. it is full of tiny little bubbles and i was hoping to get it to crystal clear although the taste and effect of it now are very pleasant.

Will i ruin anything by vac'ing it now? Should i heat it a little before i vac it? Should i do my first pull, as-is, with no heat, as a lot of these forum posts suggest to?

When i do my first pull, I should not pull it to full vacuum, correct?(To avoid implosion) Pull to -20 or so, release it (muffin should shrink), then heat to 110 and do another pull but at full vacuum?

The pump should be above the chamber to avoid the unwant Vb ed mixture of substances/oil/gasses , correct?

Sorry, I know this may start to be sounding like vac purging 101 but it is hard to find good accurate information on my particular situation as i do not want to ruin anything.

Any help and guidance will be very much appreciated and am so greatful for such an informative forum. I will upload the pics shortly, but because of you guys i was able to make this without any help, purely from reading. This is my first time reaching out, please help! Thank you!!!!!

~

 

[vbsponger]

Okay, definitely wasnt as hard as i thought it would be to upload pictures hahah. Here are two pictures, these are actually both before it sat in the dark for ~10 hours.

After the 10 hours, it was crisp and it seemed like a lot more of the really tiny bubbles started to appear... taste is very good and so is the effect.

Thanks again!

 

[midnitetoak]

The key phrase I got from your post was- there was no sizzle. After 10 hrs & it is silent on the nail oughta be purged. Enjoy

 

[vbsponger]

I had a feeling this was hard to understand , sorry!!

I would like to purge out the remaining butane. I let it sit on full vac for an hour. Not much happened , it did muffin up in areas and those areas are where I believe there is the most tane present. Going to try again today, but with minimal heat , 100-110ish.

Will be my second time vacuuming anything, ever

a lot of trial and error.... Will post pics when finished

 

[midnitetoak]

That is cuz there is no butane left... When you start to vac under lo heat- I like to call it pulling a muffin- there will be a violent reaction in the chamber... The glob of oil will expand like a sponge many times it's size- that is the butane releasing. Then after awhile you will need to allow the tane to escape by releasing the pressure & returning to full vac (-25 to -30hg) and then repeat this process until the oil is "mellow" -which means there is no more reaction under vac & lo heat- it's done have fun trial and error is part of learning process but not much to it really. Every run gets better than the last as you gain exp

 

[BCOGYODA]

Right on VB you are on your way. Looks great for your first run man. A key to watch for also during your purge is the color of the bubbles. If they look rainbow like or like bubbles that you blow when your a kid with soap through a ring then you have solvent releasing through the bubbles. If the bubbles are clear and see through with no blues/pinks/orange/green colors in them then your oil is free of solvent. Something else you can do to quicken the vac purge time is to fold the oil over itself once and awhile. This makes other areas of the oil more exposed and will purge the trapped tane quicker.

 

[MiG pilot]

If they look rainbow like or like bubbles that you blow when your a kid with soap through a ring then you have solvent releasing through the bubbles.

Observed thin-film interference speaks only about the thickness of the resin film and is not associated with the presence of a solvent.

 

[Fadedawg]

Observed thin-film interference speaks only about the thickness of the resin film and is not associated with the presence of a solvent.

Good point! All of the terpenes, including the diterpene cannabinoids are aromatic hydrocarbons, and produce rainbows in bubbles.

 

[Fadedawg]

I had a feeling this was hard to understand , sorry!!

I would like to purge out the remaining butane. I let it sit on full vac for an hour. Not much happened , it did muffin up in areas and those areas are where I believe there is the most tane present. Going to try again today, but with minimal heat , 100-110ish.

Will be my second time vacuuming anything, ever

a lot of trial and error.... Will post pics when finished

The bubbles have a problem exiting the puddle unless the surface is molten, which happens between 110 and 115F. We purge at -29.5" Hg and 115F until the larger irregularly sized bubbles cease and only fizzy equally sized C02 bubbles remain to get shatter. Usually takes only around 30 to 45 minutes.

 

[BCOGYODA]

Observed thin-film interference speaks only about the thickness of the resin film and is not associated with the presence of a solvent.

Hey MP please explain this further if you could please.
As I understand it "thin film interference" has to do with light waves refracting and reflecting kind of like a mirror image from layers of the material.
Can you explain how then you can physically watch a butane extracted oil vac purging away and progressively watch those "oil rainbow colored" bubbles decreasing in appearance as the oil continues purging?
I have pulled oil out during the purge where I though it should be void of tane while making a shatter product at several different intervals of the purge to test your theory against the presence of tane in those rainbow bubbles.

My observation and conclusion was that the oil was not purged until the bubbles became clear for several reasons. Those being the oil did not become shatter quality until the rainbows disappeared, the oil didn't burn cleanly, smoothly, non spark/crackly until those rainbow bubbles disappeared, and the physical look, behavior, smell, and taste of the oil is significantly different to me after the bubbles go from rainbow color to clear color.

I'm no chemist in any way so I just have to do my research from reading and doing my own physical experiments to come to my own conclusions. I may be off here so please expand on your theory some more if you can?

Further, please explain if the rainbow colors of the bubbles are just "thin film interference", what is the explanation for the rainbow colors disappearing? The light sources, or conditions of the room the oil purge is happening in aren't changing so why would the "thin film interference" action change it's effect on the bubble coloring.

Good point! All of the terpenes, including the diterpene cannabinoids are aromatic hydrocarbons, and produce rainbows in bubbles.

Hey Fade so I was doing some reading on hydrocarbons and thinking about these theories. Something I noted during my readings is that there are different kinds of hydrocarbons; the two relevant ones we are talking about here are the aromatic, and the alkane hydrocarbons. (just from a quick read up from the net) I noticed that diterpene, an aromatic hydrocarbon is an arene. When reading up on it I didn't note any talk about it being petroleum based. But when I read up on butane (an alkane) it does talk about it being a saturated hydrocarbon and what I read mentioned that alkanes are the basis of petroleum fuels.
Would it not be a the petroleum based saturated hydrocarbon that would be giving off the rainbow colored bubbles? All the petroleum based products I can think of off hand all give off that rainbow colored effect when mixed with water, or other liquid products.

I also couldn't find any studies (just googling) that showed results which talked about aromatic hydrocarbons giving off those rainbow colors. I did read a lot about them giving off sweet smells though.

So I'm not sure if I'm interpreting your theory as you intend it to be? Are you saying that if I am purging out my oil until all the rainbow colors are gone, would that not then produce a product that is odorless or very close to odorless if those are in fact the aromatic hydrocarbons that are the cause of the rainbow colors?

To note my wax is super dank and intense smelling. When you open a jar the smell is crazy powerful and smoke is very, very smooth. I purge my oil until ALL the rainbow color is gone from all of the bubbles coming out of my oil.
How is this explained if the rainbow color is aromatic hydrocarbon, and NOT an alkane hydrocarbon?

I hope you guys take this as an intellectual conversation and not as me trying to discount your guys' theories. I'm trying to learn as much as I can about all this stuff. Please explain further thank you!

 

[SaybianTv]

BC i'll throw a statement out there to back Fade's statement.
We all know I use limonene, a non polar aromatic hydrocarbon to extract.
It definetly gives rainbow color's just shaking it around in a round bottom flask.
I don't know where it stands in regards to an Alkane because the brand name limonene is like kleenex. I only know it's also called cyclohexane so maybe in fact it's an alkane and not an aromatic.

But this does pose a headache, plenty of strains have a tonne of limonene in them. In a butane extraction they should theorectically still be present during the vac and should produce rainbow bubble's. My statement falls apart here because limonene doesn't boil till 176c so if your getting limonene rainbow bubbles, your vac pump is getting pretty high off thc.

Fade off the top of your head, could it be said that if your coming across aromatic rainbow bubbles in the vac after solvent removal your temps are too high and approaching thc's boiling point in the vac hence a new "stratosphere" of aromatic compounds with higher boiling points is starting to move?

 

[BCOGYODA]

Ya I dunno Saybian. My wax tests at 60-70% thc on the average and absolutely reeks with potent dank deep smell so I don't think there is any loss of aromatic smells there. And I don't ever go over 110F when purging so something doesn't quite add up. Somethings missing in these equations somewhere..

Analytical testing for residual solvents in relation to the presence of the rainbow bubbles would certainly be eye opening I imagine. Sure wish there was a full service lab close by with solvent testing. I would like to test some theories.

 

[BluJayz]

The pump should be above the chamber to avoid the unwant Vb ed mixture of substances/oil/gasses , correct?

I'm curious to hear more about this?

 

[blackforest]

I always purge until there is no more rainbow colors and then some.

There's always a pot of gold at the end of a Rainbow purge!
(don't mind the flakes those were on purpose

 

[vbsponger]

The bubbles have a problem exiting the puddle unless the surface is molten, which happens between 110 and 115F. We purge at -29.5" Hg and 115F until the larger irregularly sized bubbles cease and only fizzy equally sized C02 bubbles remain to get shatter. Usually takes only around 30 to 45 minutes.

Great! I am going to do my best to keep it at 110. I noticed those little rainbow bubbles but they werent in the 'larger' bubbles just the smaller 'fizzy' like bubbles. So, if i am reading this correctly, small rainbow fizzy-like bubbles = terps, and are essential for a nice aromatic finish ?

Going to do another run today, will take a lot more pictures along the way too.

Side note: I think i got lucky in ordering tane, i ordered 2 cases of 5x vector tane and they sent 2 cases of the 14X TANE!!! How will this change my extraction/end product? I know it is cleaner butane and a hell of a lot more expensive, but will i notice any difference along the way ?

Thanks again guys, great discussions to be had in the future . this is so much fun and feels nice to have a million coaches with me right along the way!

 

[vbsponger]

I'm curious to hear more about this?

sorry for the typo there, i am very new to this. This was in reference to where i put the chamber and the pump to avoid oil being sucked into the chamber and ruining your bho. If i understand correctly, as long as the vacuum pump is sitting lower than the chamber, you will be fine. I have my vacum pump on the floor, and the chamber sitting a couple feet above the pump. I will add pictures later today or tomorrow to be more clear. I believe it is also important to have valve opened when turning the pump on and closed before turning the pump off.

 

[Fadedawg]

Hey Fade so I was doing some reading on hydrocarbons and thinking about these theories. Something I noted during my readings is that there are different kinds of hydrocarbons; the two relevant ones we are talking about here are the aromatic, and the alkane hydrocarbons. (just from a quick read up from the net) I noticed that diterpene, an aromatic hydrocarbon is an arene. When reading up on it I didn't note any talk about it being petroleum based. But when I read up on butane (an alkane) it does talk about it being a saturated hydrocarbon and what I read mentioned that alkanes are the basis of petroleum fuels.
Would it not be a the petroleum based saturated hydrocarbon that would be giving off the rainbow colored bubbles? All the petroleum based products I can think of off hand all give off that rainbow colored effect when mixed with water, or other liquid products.

I also couldn't find any studies (just googling) that showed results which talked about aromatic hydrocarbons giving off those rainbow colors. I did read a lot about them giving off sweet smells though.

So I'm not sure if I'm interpreting your theory as you intend it to be? Are you saying that if I am purging out my oil until all the rainbow colors are gone, would that not then produce a product that is odorless or very close to odorless if those are in fact the aromatic hydrocarbons that are the cause of the rainbow colors?

To note my wax is super dank and intense smelling. When you open a jar the smell is crazy powerful and smoke is very, very smooth. I purge my oil until ALL the rainbow color is gone from all of the bubbles coming out of my oil.
How is this explained if the rainbow color is aromatic hydrocarbon, and NOT an alkane hydrocarbon?

I hope you guys take this as an intellectual conversation and not as me trying to discount your guys' theories. I'm trying to learn as much as I can about all this stuff. Please explain further thank you!

Good point! I should slow down and not make broad statements, because the hetero-arenes have carbon atoms replaced with oxygen, sulfur, or nitrogen, so are polar and more miscible with water.

A better statement would be that there are enough terpenes that also refract light when stretched into a thin film, that judging purging by watching the colors is not a pure science.

Neither is my method of watching the bubble type and formation, so both are just tools in the tool box, so we use a GC, as well as our sense of taste and smell as final judge of when purging is complete.

I do note that it is way easier to see colors in the larger solvent bubbles than the small fizzy C02 bubbles, so that is another variable to consider.

 

[Fadedawg]

BC i'll throw a statement out there to back Fade's statement.
We all know I use limonene, a non polar aromatic hydrocarbon to extract.
It definetly gives rainbow color's just shaking it around in a round bottom flask.
I don't know where it stands in regards to an Alkane because the brand name limonene is like kleenex. I only know it's also called cyclohexane so maybe in fact it's an alkane and not an aromatic.

But this does pose a headache, plenty of strains have a tonne of limonene in them. In a butane extraction they should theorectically still be present during the vac and should produce rainbow bubble's. My statement falls apart here because limonene doesn't boil till 176c so if your getting limonene rainbow bubbles, your vac pump is getting pretty high off thc.

Fade off the top of your head, could it be said that if your coming across aromatic rainbow bubbles in the vac after solvent removal your temps are too high and approaching thc's boiling point in the vac hence a new "stratosphere" of aromatic compounds with higher boiling points is starting to move?

d-Limonene is a mono cyclic aromatic Alkene. Please notice that it has no oxygen, nitrogen, or sulfur atoms.

 

[SaybianTv]

Ok so it is an alkene, i'm not Hot like you so I have to preface things with room to get slapped. So i guess all i can ask is Is d-limonene a terpene oddity for mmj being an alkene or are there other terps that are like this which throws the rainbow bubbles aregument to pieces? I guess im now looking at the tool in my tool chest and it looks like a hand cranked screwdriver now..... Ughhhh why can't every mmj state/province having a testing scene like analytical360 in washingston. It would help allot to have a theory on how you got it all out then test you did get it all then breathe easy. Just when i felt like you know im not sure if this can get cleaner now I'm like hey you solvent bubble where the f do you think your going with my flavor.

 

[Fadedawg]

Ok so it is an alkene, i'm not Hot like you so I have to preface things with room to get slapped. So i guess all i can ask is Is d-limonene a terpene oddity for mmj being an alkene or are there other terps that are like this which throws the rainbow bubbles aregument to pieces? I guess im now looking at the tool in my tool chest and it looks like a hand cranked screwdriver now..... Ughhhh why can't every mmj state/province having a testing scene like analytical360 in washingston. It would help allot to have a theory on how you got it all out then test you did get it all then breathe easy. Just when i felt like you know im not sure if this can get cleaner now I'm like hey you solvent bubble where the f do you think your going with my flavor.

Sorry if that felt like a slap. I score in the 99th percentile in mechanical and abstract reasoning, but alas, have always been sadly challenged inter personally. Please just consider my input as additional information pertinent to arriving at common grounds, with no slap or personal attack intended.

d-Limonene as a monterpene isn't an oddity, as there are a litany of monocyclic monoterpenes, as well as bicyclic monoterpenes. So many that they haven't even all been identified.