Cant You Vacuum Distill SUPER PURE Hash Oil?!
- Thread starter Marzfisch
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murdergrow
Active Member
idm- you said you have all the lab equipment for this tek and have already done a few runs. would you mind sharing some pics of your process? or if not maybe just your setup? im interested in how you actually went about this. also got any pics of your resulting concentrate from this process? very intested thx.
ideletemyself
Member
That is a pretty huge bummer but that does lead me to the 2nd part or was my primary question, which was what if I just used distilled water instead? I was able to boil water at about 101F with my aspirator setup. But then you mention it condensing and clogging shit up so I dunno. I don't do large runs, typically I usually extract from 1/2 ounce of the most top shelf quality that I can find in my part of Arizona. This is all for my own use and I do have my med card here in Arizona as well, was thinking about doing a round of the cannabis alchemy at the Skunk Pharm labs (since reciprocity is part of Arizona's med laws, which I don't think matters in Oregon but still) but I don't really have the $$ or free time to take off from work so..... hence my trial & error approach...
As I said in my post, I really do love chemistry and so spending x $$$ doesn't matter one bit to me. I don't have much but am slowly amassing better and other various components(I have a 3 neck round bottom flask & squib style sep. funnel on order actually, lol). I'm always up for talkin' shop and I do other extracts which I won't mention here for topics sake. Here's some pics so ya'll know I'm not bullshittin' and I think someone wanted to see my setup and previous extracts.
So, I'm posting 2 of my chem setup and 2 of my last run of concentrate via QWET extraction, which was with some pretty choice blue dream...
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ideletemyself
Member
if the distilled water is a bust then I suppose I'll stick to my super chilled QWET extraction w/dry ice and then just vacuum distill the ethanol to reclaim and call it a day or night rather... will check my chemistry supply sites for D-Limonine tho. Why does that work? Does it travel together in gaseous form or would the clogging still pose an issue? I guess this all just advances me buying a proper fractioning column, probably a Vigreux column and try my hand at some vac assisted refluxing...
and to clarify, I've never extracted or distilled anything cannabis related with my organic chem. set as of yet because I wanted to test my organic chem. set as a whole, the heating mantle and most importantly to see how good my water aspirator is at pulling vacuum. Which is pretty goood, btw. Tonight is going to be my 1st attempt with anything cannabis related and if I don't get a clear answer on the water will most likely turn into a simple solvent reclaim. Which will still be fun tho!
and to clarify, I've never extracted or distilled anything cannabis related with my organic chem. set as of yet because I wanted to test my organic chem. set as a whole, the heating mantle and most importantly to see how good my water aspirator is at pulling vacuum. Which is pretty goood, btw. Tonight is going to be my 1st attempt with anything cannabis related and if I don't get a clear answer on the water will most likely turn into a simple solvent reclaim. Which will still be fun tho!
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ideletemyself
Member
never mind, now I see why you use d-limonine: "d-Limonene is a volatile oil steam-distilled from orange peel" ... one word comes to mind, DOOOOOOOOOPE! why have I not heard of this before! lol.
and secondarily, do any common shops in the USA sell this magical stuff?? Like, wally world(walmart/walgreens)? or perhaps a health food shop? I think there's one in my town but fuck they close so early, tough for a workin' man to make it there before they close.
and secondarily, do any common shops in the USA sell this magical stuff?? Like, wally world(walmart/walgreens)? or perhaps a health food shop? I think there's one in my town but fuck they close so early, tough for a workin' man to make it there before they close.
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ideletemyself
Member
so after some initial researching into d-limonene and how it's produced, I'm pretty confident I can just use distilled water and steam distill under reduced pressure... That's exactly how they make d-limonene in a lab is by grading up some orange peel and then steam distilling. The distillate will have odiferous properties that won't readily separate. An oily layer then forms at the top of the distilled water in the collection flask. Remove oily layer and extract with ethanol or use as is. I'll most certainly do the extract with ethanol, vacuum filter and distill off & reclaim the ethanol...
But that's pretty much the text book case on creating an absolute from distilled water or a "distilled-water absolute" which some guy was sourcing on the Skunk Pharm pages, I can link to it if you all would like to see that reference...
Does this seem valid to everyone?
But that's pretty much the text book case on creating an absolute from distilled water or a "distilled-water absolute" which some guy was sourcing on the Skunk Pharm pages, I can link to it if you all would like to see that reference...
Does this seem valid to everyone?
SaybianTv
Active Member
LOL Congrats! you figured out my trade secret all on your own.
You are! the kind of folk I knew where out there.
You can get it from new direction aromatics....
You are back in time where I was on July 8th 2013 Grrr why can't i upload images anymore.....
Look the limonene route isn't easy, it is very difficult to get consistent results with a magnetic stir bar.
Everything is dandy till 80% of the limonene is gone and your oil starts to get thick. "your oil never leaves the boiling flask your solvent does"
Your stirbar is going to come to a grinding halt and the water is going to start BUMPING. its going to be scary, oil is going to start splattering all over your flask.
You gotta tidy up that aspirator setup you will need -28.5 hg. If your only boiling water at 101f Wait Im so dumb you mean farenheight Im in Celcius it sounds like your fine.
You sound like you don't have allot of bud to loose, so I dunno about venturing outside of the qwet your use to, my first 15 batches I wouldn't even dab these days.
The great news is I'm telling you all this, cuzz purging is hard, its going to take you at least 2 days n you can't leave the stirbar unless BUMPING is what ur into.
Warning number 3. GET the largest largest largest long football shaped stirbar you can find, all of those pill shaped things can't spin oil........Don't be like me and wait 2 weeks only to have to wait another 2 weeks after getting to use it for 40 mins.
I can't write the history of how to get from where you are to where Im at, plus you dont have the money to go comercial gear until you can make at least 1 batch of shatter using the steam distil tek. I slept on the floor for weeks while it ran, so you have to earn your lumps....
\
You are! the kind of folk I knew where out there.
You can get it from new direction aromatics....
You are back in time where I was on July 8th 2013 Grrr why can't i upload images anymore.....
Look the limonene route isn't easy, it is very difficult to get consistent results with a magnetic stir bar.
Everything is dandy till 80% of the limonene is gone and your oil starts to get thick. "your oil never leaves the boiling flask your solvent does"
Your stirbar is going to come to a grinding halt and the water is going to start BUMPING. its going to be scary, oil is going to start splattering all over your flask.
You gotta tidy up that aspirator setup you will need -28.5 hg. If your only boiling water at 101f Wait Im so dumb you mean farenheight Im in Celcius it sounds like your fine.
You sound like you don't have allot of bud to loose, so I dunno about venturing outside of the qwet your use to, my first 15 batches I wouldn't even dab these days.
The great news is I'm telling you all this, cuzz purging is hard, its going to take you at least 2 days n you can't leave the stirbar unless BUMPING is what ur into.
Warning number 3. GET the largest largest largest long football shaped stirbar you can find, all of those pill shaped things can't spin oil........Don't be like me and wait 2 weeks only to have to wait another 2 weeks after getting to use it for 40 mins.
I can't write the history of how to get from where you are to where Im at, plus you dont have the money to go comercial gear until you can make at least 1 batch of shatter using the steam distil tek. I slept on the floor for weeks while it ran, so you have to earn your lumps....
\
ideletemyself
Member
Sweet thx, yeah I was able to find a couple of sources on food grade and even what one place referred to as "Ultra Pure" at 98% d-limonene. Will prolly end up buying from them. You're dead right on me not being able to waste material. Ideally, I'd like to be doing runs of 1 ounce, I do 1/2 ounce a week and usually run out of concentrate usually the day of my next extract. If I were doing the whole ounce I could more closely follow the gram a day regiment needed for results, again I'm doing this to help my crohn's disease...
After finishing reading a research tek paper on using steam distillation using only distilled water and it ended by saying that THC doesn't readily get absorbed by water and so had I gone through with using just distilled water on my top shelf buds I would've ended up with an awesomely smelling but totally useless concentrate as it would have very little THC... Another bummer but oh well...
The plan is to now just do my super-chilled QWET and then just reclaim my ethanol with my chem. set. Order up some d-limonene and then proceed with lump taking. I think I might just get an 1/8th of some mid-grades to do my initial testing with, that way I'm not out my medicine for the week.
It's a bitch trying to do all of this already living paycheck to paycheck but I've gone through a decade of doing very little and getting absolutely nowhere with the professional medical community. Basically going gluten-free and cannabis concentrate are the only things that have ever helped my crohn's disease in any regard and so I'll continue my chemistry skills to someday reach the ability to do isomerization or THC acetate. Something more potent that can help me not have to rely on opiod meds ever again... That's my hope and what I work towards as much as I can...
Thanks for all your feedback and I'll be posting some pics from my run tonight regardless. Then I'm going to be purifying ethyl rubbing alcohol into pure ethanol for future extractions! My kind of friday night
ideletemyself
Member
oh and yeah with my aspirator I was boiling water at about 39 - 41 deg. C. I didn't go through with the calculations as you would in a standard chemistry class I'm sure, to figure out my specific rate of pull but I'm pretty sure it's the at or above -29hg... The bigger, football shaped stir bar recommend is a great one and makes sense...
My question is this... Why not just never go below half volume on your d-limonene in your boiling flask? The research paper I was reading actually pointed this out, they were extracting d-limonene from orange peels but they said if you went below half the amount your started with that you'd get some "jamming" up and it would become pretty tough to get out at that point. So, why not just distill the d-limonene to about half it's starting volume and then add more and repeat until you're satisfied?
That seems like a pretty good solution to me, thoughts?
My question is this... Why not just never go below half volume on your d-limonene in your boiling flask? The research paper I was reading actually pointed this out, they were extracting d-limonene from orange peels but they said if you went below half the amount your started with that you'd get some "jamming" up and it would become pretty tough to get out at that point. So, why not just distill the d-limonene to about half it's starting volume and then add more and repeat until you're satisfied?
That seems like a pretty good solution to me, thoughts?
SaybianTv
Active Member
Do not stop your Qwet for chron's PLEASE, don't even fiddle faddle with the limonene thing if your at all resource stricken. You've got a great setup for recycling your solvent in a qwet setup. The first time you try to make anything with limonene have the intended goal be oral instead of dabs please, the hole dab's business is for me to subsidize my pheonix tears. The reason why im saying that is because your not going to be able to get all the water out of your oil without allllllllllllllllot of patience and you will have to hand twirl your flask when the stirbar dies from oil. If you do it for orals and you end up tainting your product "reasonable taint" i don't want you ingesting limonene to any degree that might irritate your condition. But yes compared to butane, naptha, even ethanol if you ask a former alcoholic swalowing limonene wont hurt you.
If your going to order it from the florida organge company which you should because your in the US. Don't bother buying the high purity, buy the food grade and "pre distill it" basically you need to run just water n limonene and then only extract with the limonene that went into your receiving flask. Throw out All that wont boil in the boiling flask n wash it like hell then put it in the oven for an hour at 500f. Presto high purity limonene, thats why they have to send it to you in glass, or it will go back down to food grade limonene from interacting with something... Its the same as Mystery oil for canned butane. I don't care what it says on a site im going to predistill All of it, in fact i like to only pre distill 2 weeks worth at a time n keep recycling it on runs till i hit 300 ml then i can't extract so i brew up some more high purity. Store your limonene in glass in the freezer in the dark. It can oxidize if you leave it out, i've never seen it do it but so they say without giving a time n environmental condition so blah blah be careful n don't play games with you or anyone elses health n just keep it locked up.
You know enough from working with alcohol to do this man!
If your going to order it from the florida organge company which you should because your in the US. Don't bother buying the high purity, buy the food grade and "pre distill it" basically you need to run just water n limonene and then only extract with the limonene that went into your receiving flask. Throw out All that wont boil in the boiling flask n wash it like hell then put it in the oven for an hour at 500f. Presto high purity limonene, thats why they have to send it to you in glass, or it will go back down to food grade limonene from interacting with something... Its the same as Mystery oil for canned butane. I don't care what it says on a site im going to predistill All of it, in fact i like to only pre distill 2 weeks worth at a time n keep recycling it on runs till i hit 300 ml then i can't extract so i brew up some more high purity. Store your limonene in glass in the freezer in the dark. It can oxidize if you leave it out, i've never seen it do it but so they say without giving a time n environmental condition so blah blah be careful n don't play games with you or anyone elses health n just keep it locked up.
You know enough from working with alcohol to do this man!
ideletemyself
Member
excellent tips, you rock!
Interestingly, I've looked into d-limonene in the treatment of Crohn's Disease and there are quite a few studies and research papers available on the benefits of using d-limonene. One of the possible reasons d-limonene is beneficial to crohn's patients is it's ability to destroy bad bacteria. It's now well known that crohn's is amplified and perhaps even caused by the bad bacteria accumulating in the gut. This is the reason I also adhere to a very strict 'select carbohydrate diet' because bad bacteria love to leech onto the sugars those carbs produce. It's also why I eat probiotic-anything that I can find to promote good bacteria in the gut.
So your fears about d-limonene affecting my crohn's in a bad way might just be careful thinking. Someone tried getting me into drinking aloe juice and that shit WOULD fuck my shit up from all the chlorophyll and fiber. So, I understand the caution in the area. The only way to know is to test this out myself. Will definitely just get the regular ole d-limonene and purify it myself as you've suggested, it's more fun that way right and was a bit cheaper to boot... Heh.
Interestingly, I've looked into d-limonene in the treatment of Crohn's Disease and there are quite a few studies and research papers available on the benefits of using d-limonene. One of the possible reasons d-limonene is beneficial to crohn's patients is it's ability to destroy bad bacteria. It's now well known that crohn's is amplified and perhaps even caused by the bad bacteria accumulating in the gut. This is the reason I also adhere to a very strict 'select carbohydrate diet' because bad bacteria love to leech onto the sugars those carbs produce. It's also why I eat probiotic-anything that I can find to promote good bacteria in the gut.
So your fears about d-limonene affecting my crohn's in a bad way might just be careful thinking. Someone tried getting me into drinking aloe juice and that shit WOULD fuck my shit up from all the chlorophyll and fiber. So, I understand the caution in the area. The only way to know is to test this out myself. Will definitely just get the regular ole d-limonene and purify it myself as you've suggested, it's more fun that way right and was a bit cheaper to boot... Heh.
SaybianTv
Active Member
Thats fantastic to hear, thats so confidence building to hear. I can't wait to get this batch of catatonic pheonix tears into service now, i was worried of that 1 out of 10 person and i figured it would be chron's related because i'd herd of the chlorophyll sensitivity that drew some into making extracts. I wish i could send you something so you had a basic to know what the potential can be both dab and orally.
Please do winterize because your now working with a non polar which will strip fats just like the rest, but you got plenty of alcohol recycled for the job now dont you!
Please do winterize because your now working with a non polar which will strip fats just like the rest, but you got plenty of alcohol recycled for the job now dont you!
ideletemyself
Member
haha, yeah after tonight I'll be good w/ethanol for some time to come... which is always a good thing!
I primarily dab but will occasionally ingest orally, it's just because of the need to decarb that I don't do more that way. And admittedly being a near life-long pot smoker I do enjoy my vap setup and the taste & aroma of my qwet extracts with it.
Well, it's about that time. I'll snap some pics of my vac assist filter & such for those that haven't seen whatever before... PEACE!
I primarily dab but will occasionally ingest orally, it's just because of the need to decarb that I don't do more that way. And admittedly being a near life-long pot smoker I do enjoy my vap setup and the taste & aroma of my qwet extracts with it.
Well, it's about that time. I'll snap some pics of my vac assist filter & such for those that haven't seen whatever before... PEACE!
Blunter the kid
Well-Known Member
See the problem you have here is thc, like the other cannabinoids is a diterpene and this class of terpenes possesses a molecular weight much higher than that of the aromatic terpenes that make up the smell, and what that means is regardless of the boiling point, these compounds are generally tough to distill because the vapor will want condense on anything room temperature, for this reason your extract would have to be distilled in an extremely small apparstus where the boiling flask and condenser are relatively close together , a sublimation apparatus would be the piece of glassware i would choose for this application.
I imagine it would be more economical to make a cold ethanol extract to begin with and then after you have removed the alcohol from the extract, place your purged extract into the bottom piece of the apparatus and affix the top piece with your cold water circulation hoses attached to it.
As long as the temperature is held closely around 314 F degrees the thc would really have no choice but to sublimate this would actually save your the headache of trying to steam distill with your simple distillation setup.
It would actually make more sense to try to distill off the terpenes and save them so they can be added back into the Sublimate. The liquid aromatic terpenes may cause the thc to drip off the condenser (Im assuming the terpenes stay somewhat liquid even when they condense on the cold finger) so it would be of benefit to remove the terpenes somehow by simple distillation.
I imagine it would be more economical to make a cold ethanol extract to begin with and then after you have removed the alcohol from the extract, place your purged extract into the bottom piece of the apparatus and affix the top piece with your cold water circulation hoses attached to it.
As long as the temperature is held closely around 314 F degrees the thc would really have no choice but to sublimate this would actually save your the headache of trying to steam distill with your simple distillation setup.
It would actually make more sense to try to distill off the terpenes and save them so they can be added back into the Sublimate. The liquid aromatic terpenes may cause the thc to drip off the condenser (Im assuming the terpenes stay somewhat liquid even when they condense on the cold finger) so it would be of benefit to remove the terpenes somehow by simple distillation.
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Hydrotech364
Well-Known Member
I blast it to make it more potent,in 2 hour's tonight I cut, trimmed and blasted pure amber that crumbles like peanut brittle..
Hydrotech364
Well-Known Member
Most of these can be improvised.....Vacuum chamber's are so simple.I am currently reclaiming my butane and using a Nitrogen preload Accumulator....I have to add a small amount from time to time but it's Sweet.
ideletemyself
Member
hmm, interesting. I think I've come across sublimation before but skipped over it to look into other processes. When you say, "extremely small apparatus" do you mean like a short path setup? Or is a sublimation apparatus completely different?
ideletemyself
Member
Yeah, I'm aware that pretty much all of this stuff can be jimmy-rigged together if the right McGuyver-type guy is around like yourself, seemingly... I'm not that improvisational in handyman-hardware skills. I'm sure if I just took the time & effort I could hack it but I'd rather spend a lil bit of $$$ and be sure it's not my equipment that's fucking whatever up at the moment. As I become more confident in my chem abilities overall, then I'll start trying my hand and making my own equipment. Gotz'ta crawl before ya walk!
Blunter the kid
Well-Known Member
Yea, i should have mentioned that a short path distillation setup would still cause the vapor to travel farther than it needs to before It has to condense, so really a sublimation apparatus would be the bees knees.
Is a little but different from regular distillation, but all you really need to is buy a cold finger that fits your boiling flask and you can make yourself a nice little apparatus it's the same concept as distillation but in a much smaller environment, here's a little picture of a sublimation apparatus, simple little piece of equipment
EDIT: The main difference between distillation and sublimation is that a sublimator will vaporize and condense all inside a small enclosed apparatus, whereas in distillation the vapor is required to vaporize in the boilin flask and travel through the condenser coil into the chilled flask.
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ideletemyself
Member
so here are some pics from last nights fun... As you'll see at the end I let my heating mantle got a lil too hot since it seems to really jump in heat around the halfway mark of the knob. Overall I'm really happy with how it went, reclaimed my ethanol (though it does seem I lost a bit in the process which is kinda confusing since I was at about -29hg.) and now I know that if I wanted to fully decarb I could easily do so in the boiling flask just by watching it...
The picture of the thermometer shows when I started to get rapid boiling though it really started to get going at around 40deg. C... didn't have time to do my second wash or purify the ethyl rubbing alcohol but that leaves it for today
Lastly, the reason for the dark color of my extract is because of my caretaker/courier service running out of most of their really top shelf flavors. This was done with mostly Grape Ape which was apparently starved of nitrogen to look more purple. It was still really great bud (I only actually smoke to test my material before extracting, otherwise I only vap.) but it was lacking in visible crystals. Also letting my rig get too hot prolly didn't help either but I never even came close to 160 F staying at around 101 F or 40 C.
The picture of the thermometer shows when I started to get rapid boiling though it really started to get going at around 40deg. C... didn't have time to do my second wash or purify the ethyl rubbing alcohol but that leaves it for today
Lastly, the reason for the dark color of my extract is because of my caretaker/courier service running out of most of their really top shelf flavors. This was done with mostly Grape Ape which was apparently starved of nitrogen to look more purple. It was still really great bud (I only actually smoke to test my material before extracting, otherwise I only vap.) but it was lacking in visible crystals. Also letting my rig get too hot prolly didn't help either but I never even came close to 160 F staying at around 101 F or 40 C.
