How to perfect the process of extraction at home

[RootsRuler]

Lucky you, I've never gotten anything topical to work.

Try Medterras topical. Its worked for a few friends of mine.

 

[Moe.Red]

I used a paper shopping bag of leaf and trim, ground it all, ending up with 2000ml of plant matter, QWISO, distilled and decarbed it, added it to 237ml coco oil and 40g Bees wax, added Eucalyptus and Spearmint for smell.

I've never used a Topical cream like this before and I didn't know what to expect? I walk like a Pirate because of an Ankle injury long ago, The pain is constant and never ending. The first time I used it, It helped very little, 2nd time I had no pain. It lasts for about 4 hours, and sometimes I feel a little dizzy? I've never heard that you can feel effects through the skin? I'll have to be careful.

Using DMSO you can push cannabinoids thru the skin into the bloodstream. Not sure about without it tho.

 

[Eskander]

Using DMSO you can push cannabinoids thru the skin into the bloodstream. Not sure about without it tho.

I would have agreed had I not been high off my ass with no other intake. Try a bit of decarbed oil in MCT on your forearm. 20mg total dose seems about right for me but onset is after well over an hour. No dose data for anyone else.

-Eskander

 

[Moe.Red]

I would have agreed had I not been high off my ass with no other intake. Try a bit of decarbed oil in MCT on your forearm. 20mg total dose seems about right for me but onset is after well over an hour. No dose data for anyone else.

-Eskander

Sublingually dosing works (tinctures) so there is no reason to think externally it can't. I've never gotten high personally touching concentrates or anything like that. Maybe the exposure site is important. Thin skin with tons of capillaries like under your tongue. If you have to go thru thicker skin, a transportation agent such as DMSO brings more predictability to the dosage would be my gut.

My wife has made cremes for her hand arthritis and nothing has worked or even been felt. Maybe we are doing it wrong. Or more likely topical application of cannabinoids on your hands to treat arthritis is not effective. And in general if you are attempting to push cannabinoids into your bloodstream via the skin, application location is important. I could see that.

The interesting effect here is the lack of liver involvement in the body accessing the blood stream directly. The 1 hour onset is surely the time it takes to penetrate the epidermis, since the action in the body is the same as smoking. This could be useful to me for sure, I'm going to look into this deeper. A slow release patch that takes all day to push in for constant low levels of meds, probably on the shoulder.

 

[Eskander]

I'm going to look into this deeper. A slow release patch that takes all day to push in for constant low levels of meds, probably on the shoulder.

Sub lingual and rectal are mucous membranes so absorption is pretty different there. Lipid solubles will cross skin anywhere but delicate skin like the nipples would be be faster than the bottoms of your feet. I agree that DMSO would give you more predictable results and if you want a easy base then this would be a good base:

Amazon.com

Perhaps homogenized with some extract and soaked into a bandaid pad would give you metered designing with faster absorption. I'm not sure I really see the point vs an edible though unless nausea and vomiting are an issue but as far as investigations go, I'm sure someone will find a niche.

-Eskander

 

[Moe.Red]

Sub lingual and rectal are mucous membranes so absorption is pretty different there. Lipid solubles will cross skin anywhere but delicate skin like the nipples would be be faster than the bottoms of your feet. I agree that DMSO would give you more predictable results and if you want a easy base then this would be a good base:

Amazon.com

Perhaps homogenized with some extract and soaked into a bandaid pad would give you metered designing with faster absorption. I'm not sure I really see the point vs an edible though unless nausea and vomiting are an issue but as far as investigations go, I'm sure someone will find a niche.

-Eskander

2 reasons some people do not process thc when eaten due to a genetic difference, and for people like myself that do not want liver interaction.

 

[cronicoldguy]

So I finally got a rotovap in my hands! All I can say is just "Wow!"

This is the shit. It was worth the trials and tribulations. With that said, this unit didnt come without a hitch. What I ordered was not what I received. I ordered it from LeDAB. What they sent me was used. Not just a little bit used. WELL USED! They hadnt even taken the time to clean the flasks. White shit all over the power cords. Unit dented and marred. Water bath housing has big crack in it and signs all over saying "I was rode hard and put away wet".

Contacted LeDAB and asked WTF?! Literally. "I ordered a brand new unit. Not some beat up piece of shit". I was told it was shipped by 'accident' by warehouse. I was also told they would have to source a new to send to me to replace the used one. So, back to the 'accident'. Was it really? There were only 3 resolutions I was interested in:
1) Replacement with brand new machine and return used unit at LeDAB expense.
2) Return unit at LeDAB expense and receive full refund of cost of unit.
3) Keep used unit and receive partial refund. (I was thinking half the cost given the condition.)

After putting the unit thru it's paces, it appeared to function as it should. So I went with option #3. I didnt want wait any longer. Was tired of getting the run-around trying to get one. Needless to say I was very disappointed with LeDAB at the time. This was the second order I had placed with them. The first order was a painless process. Only about $200 worth of stuff. They even threw in a bunch of graft which I thought was too cool. This order totaled $3583. Not only did I receive a used unit, not one stitch of graft. LOL! As a matter of fact, the 2.5kg bag of Celite that I ordered with it had a huge hole in the bag. About 1/3 emtied into box and all over rotovap.

Now, after talking with Zach at LeDAB, he offered me the same three resolutions I proposed. He wanted to do what he could to make things good. Except I would only get $1153 back as a refund. That was less than what half the cost was, but I was satisfied. He aslo said LeDAB would send me a 1kg bag of Celite to replace the loss. I accepted Option 3. This has restored some faith in LeDAB. Really disappointed because they are a Canadian company and I expected much better service. But at the end of the day, I was happy.

I am very impressed with rotary evaporators. Everything I expected. I have run approx. 13L solution thru it so far. Balls to the wall at first! Until my chiller shit the bed. It couldnt keep up for shit. Then I learned how to actually use one. Well hey, my chiller does just fine. Could be bigger, but it does the job. There is a little more to it than filling it up and 'lettin her rip'.

This unit is a RE-200B. Seems like a solid unit and well built. Altough I didnt receive even one piece of paper documenting the rotovap, assembly was a piece of piss. Pretty straight forward. The control panel is basic and easy to figure out. Not sure if there is any other function of the control panel other than setting temperature. RPM is controlled with a rheostat with digital read out. Would be nice to change temp display from F to C. No instructions so no idea.

The rotovap came with an adapter. With it, I can use any boiling flask that has a 24/40 neck and will fit in the bath. So far I have used a 2L, 1L, and 500ml flasks. Really nice because I can work my way down to the smallest flask when evaporating, reducing wastage. I have a 250ml flask on order and will test it as well.

Hoping for some tips from those that know WTF they are doing with one. One question I have is this. If I have an oil or glycol in the bath, can I bring temp up and decarb right inside the rotovap? Is this advisable?

What I have done is bring temp up to 78C at 25 TORR in an attempt to purge the solvent from oil inside the rotovap. Is this detrimental to the extract?

Pics coming.

 

[Godfish]

So I finally got a rotovap in my hands! All I can say is just "Wow!"

This is the shit. It was worth the trials and tribulations. With that said, this unit didnt come without a hitch. What I ordered was not what I received. I ordered it from LeDAB. What they sent me was used. Not just a little bit used. WELL USED! They hadnt even taken the time to clean the flasks. White shit all over the power cords. Unit dented and marred. Water bath housing has big crack in it and signs all over saying "I was rode hard and put away wet".

Contacted LeDAB and asked WTF?! Literally. "I ordered a brand new unit. Not some beat up piece of shit". I was told it was shipped by 'accident' by warehouse. I was also told they would have to source a new to send to me to replace the used one. So, back to the 'accident'. Was it really? There were only 3 resolutions I was interested in:
1) Replacement with brand new machine and return used unit at LeDAB expense.
2) Return unit at LeDAB expense and receive full refund of cost of unit.
3) Keep used unit and receive partial refund. (I was thinking half the cost given the condition.)

After putting the unit thru it's paces, it appeared to function as it should. So I went with option #3. I didnt want wait any longer. Was tired of getting the run-around trying to get one. Needless to say I was very disappointed with LeDAB at the time. This was the second order I had placed with them. The first order was a painless process. Only about $200 worth of stuff. They even threw in a bunch of graft which I thought was too cool. This order totaled $3583. Not only did I receive a used unit, not one stitch of graft. LOL! As a matter of fact, the 2.5kg bag of Celite that I ordered with it had a huge hole in the bag. About 1/3 emtied into box and all over rotovap.

Now, after talking with Zach at LeDAB, he offered me the same three resolutions I proposed. He wanted to do what he could to make things good. Except I would only get $1153 back as a refund. That was less than what half the cost was, but I was satisfied. He aslo said LeDAB would send me a 1kg bag of Celite to replace the loss. I accepted Option 3. This has restored some faith in LeDAB. Really disappointed because they are a Canadian company and I expected much better service. But at the end of the day, I was happy.

I am very impressed with rotary evaporators. Everything I expected. I have run approx. 13L solution thru it so far. Balls to the wall at first! Until my chiller shit the bed. It couldnt keep up for shit. Then I learned how to actually use one. Well hey, my chiller does just fine. Could be bigger, but it does the job. There is a little more to it than filling it up and 'lettin her rip'.

This unit is a RE-200B. Seems like a solid unit and well built. Altough I didnt receive even one piece of paper documenting the rotovap, assembly was a piece of piss. Pretty straight forward. The control panel is basic and easy to figure out. Not sure if there is any other function of the control panel other than setting temperature. RPM is controlled with a rheostat with digital read out. Would be nice to change temp display from F to C. No instructions so no idea.

The rotovap came with an adapter. With it, I can use any boiling flask that has a 24/40 neck and will fit in the bath. So far I have used a 2L, 1L, and 500ml flasks. Really nice because I can work my way down to the smallest flask when evaporating, reducing wastage. I have a 250ml flask on order and will test it as well.

Hoping for some tips from those that know WTF they are doing with one. One question I have is this. If I have an oil or glycol in the bath, can I bring temp up and decarb right inside the rotovap? Is this advisable?

What I have done is bring temp up to 78C at 25 TORR in an attempt to purge the solvent from oil inside the rotovap. Is this detrimental to the extract?

Pics coming.

Dude! This is so cool, can't wait to see the pics.

I can't really see getting one for myself unless I made it a business? But I'm sure it's way better. Forgive my ignorance but are these to lower the boiling temperature of your solution so that you don't decarb in the boiling flask until wanted?
I use a very small chemistry type distillation unit, and it has to heat up enough to get the alcohol solution to boil at 185 - 190° f I keep it as low as possible, but by the end I find my solution is almost fully decarbed.

 

[Moe.Red]

Hoping for some tips from those that know WTF they are doing with one. One question I have is this. If I have an oil or glycol in the bath, can I bring temp up and decarb right inside the rotovap? Is this advisable?

What I have done is bring temp up to 78C at 25 TORR in an attempt to purge the solvent from oil inside the rotovap. Is this detrimental to the extract?

Congrats, you waited long enough.

78C / 172F is high enough to destroy terpenes but too low to effectively decarb. To save terps, try not to exceed 40C.

 

[Eskander]

Congrats, you waited long enough.

78C / 172F is high enough to destroy terpenes but too low to effectively decarb. To save terps, try not to exceed 40C.

And that is 40 in the boiling flask not 40 as the bath temp for clarity.

The rotovap came with an adapter. With it, I can use any boiling flask that has a 24/40 neck and will fit in the bath. So far I have used a 2L, 1L, and 500ml flasks. Really nice because I can work my way down to the smallest flask when evaporating, reducing wastage. I have a 250ml flask on order and will test it as well.

You really don't want to be changing from one flask to the next as your volume reduces. It is essentially pointless unless you really like cleaning glassware. You aren't going to ever want to go completely to dry in the rotovap anyway. Chasing oil out of a flask with heat gun is a pain in the ass. Just find the flask size that nearly saturates your coil at just under boiling temp for the bath and then stick with it. Remember that you want at least a 40C differential between the bath and condensing column.

-Eskander

 

[cronicoldguy]

Dude! This is so cool, can't wait to see the pics.

I can't really see getting one for myself unless I made it a business? But I'm sure it's way better. Forgive my ignorance but are these to lower the boiling temperature of your solution so that you don't decarb in the boiling flask until wanted?
I use a very small chemistry type distillation unit, and it has to heat up enough to get the alcohol solution to boil at 185 - 190° f I keep it as low as possible, but by the end I find my solution is almost fully decarbed.

Ya, the rotovap is very cool.I am not a business. This is purely a hobby for me as well as serving my own needs. Mild to moderate ADHD. It may seem to be a stupid expensive hobby but my prerogative is 'Go Big or Go Home'. I hate doing things half-assed with half-assed ghetto equipment or components. Over the past 30 yrs, I have spent tens of thousands of dollars in the PC industry. I was not only a PC enthusiast. I was also custom building high end personal and client gaming PCs and workstations. More than I can remember. No PC I have built in last 10-12 yrs was delivered with air cooling. All custom liquid cooled. My PC lab has now been converted to a cannalab. Motocross racing in my younger years wasnt cheap either. That took a toll on my carcass and wallet thru time. Too many dirt samples. Hung up my MX helmet at 42 yrs and bought a cruiser motorcycle.

I have read this more than once from pros in the know from different industries; For a novice to have the best chance at success, one should be using the best suited tools that can be afforded. This greatly reduces the chances of user error. An experienced pro can wing it with most anything, and get the job done competently. I am not a pro by any means! My learning curve maybe longer than others. I also will admit the fact I am not the most sensible person, but certainly not stupid. I can learn......usually by my mistakes.

The rotovap allows a person to evaporate the solvent 'gently'. By that I mean at low temp and minimal agitation (please correct me if wrong). Decarbing in the boiling flask would be optimal if it could be done safely. But I dont think it can which leads me to a question I will ask below. I was using a fractional still prior to the rotovap to evaporate. It was under vacuum so I wasnt going to the temps you are. But I have in the past. The only real danger I see evaping at 180F-190F is as Moe.Red suggested to me in post above. Terpenes are very volatile and will be destroyed at those temps. They are one of the first compounds to vaporize at temp. That isnt all that big of a deal in my case. It mostly effects the flavor, not potency. Terpenes can be added after the fact if so desired. Again, somebody please correct me if wrong. Dont want to be spreading bad info.

Congrats, you waited long enough.

78C / 172F is high enough to destroy terpenes but too low to effectively decarb. To save terps, try not to exceed 40C.

THANKS! Yes, too long!

This has me confused. In order to decarb, flower or extract is heated to 115C-120C for a given amount of time. Typically 20mins? I have been running the rotovap at 38C-42C, so I should be safe? I only raised the temp to 78C near the end-point. I wasnt expecting decarb, but wanted to purge the solvent. I was asking if decarb can be accomplished safely in the rotovap if so desired.

How are terps retained when decarbing? Or are terps evaped away and new terps added post decard? Also, what is the most desirable way of decarbing? Vac oven, heated magnetic stirrer? I have both. I was able to acquire a used Across International AccuTemp-19 vacuum oven with pump at a great price. Didnt really need it. But most canna labs I seen on the web had one. Couldnt pass it up. Is that the best way?

I also have an Ardent Nova Decarboxylator. I bought it and a Source Turbo after graduating from a hotplate and double boiler. I dont fully trust the Nova as it is 100% automated and no temp display. I used it once to decarb an oz of bud. Consumed 3.5g of the decarbed bud in a yogurt and berry smoothie with absolutely no effect. Oh, other than the toilet smelling the same as the bud the next day. Havent used it since.

Anyone use a Nova? Are they safe? The bud was still somewhat moist when decarb cycle was finished. Just dont trust it.

And that is 40 in the boiling flask not 40 as the bath temp for clarity.


You really don't want to be changing from one flask to the next as your volume reduces. It is essentially pointless unless you really like cleaning glassware. You aren't going to ever want to go completely to dry in the rotovap anyway. Chasing oil out of a flask with heat gun is a pain in the ass. Just find the flask size that nearly saturates your coil at just under boiling temp for the bath and then stick with it. Remember that you want at least a 40C differential between the bath and condensing column.

-Eskander

I found this makes retrieving the extract easier and more complete. With the finishing flask upright and held in heating bath with a stand and clamp, the 'finished' extract can be sucked out with a syringe. That is why I was hoping to decarb inside the rotovap. Not much wastage to flask. And doesnt seem to be a hassle at all. Changing out flasks is simple and fast. No heat gun used to transfer from flask to flask. Solution is still very fluid when transferring to next smaller flask for that reason. A simple rinse with solvent in bigger flask and poured into smaller flask leaves bigger flask clean. The only flask getting 'dirty' is the final flask. The other flasks used, clean up easy with dish soap and water when finished. Udino, its what works for me. Seems logical. But you guys are the pros. So if this is not good practice, please let me know. I want to be doing things properly.

Now to the 40 deg differential. I have seen this mentioned several times before. My chiller only goes down to -5C. So my optimal bath temp would be 35C-40C? That is the range I was running the rotovap in. Except when I attempted to purge the solvent.

This is my procedure. Please correct my mistakes Moe, Eskander, or other experienced users:

Depending on batch size, I will start with the 1L flask or the 2L flask. I have even started and finished a small batch in the 500ml flask. Other than the 2L flask that came with the machine, all other flasks I used are just regular Stoney Labs 24/40 necked boiling flasks. Nothing special.

1) Get chiller (-5C) and bath (38C-40C) to temp. Lower vacuum pressure to 75 TORR. Rotary RPM at 100.
2) Slowly introduce solution thru injection valve to boiling flask to approx. 500ml and then close valve.
3) Once temps stabilize, I begin injecting solution again, trying to match the intake with the evaporation rate.
4) Once everything is happy, I will increase RPMs and reduce vac pressure until condenser cant keep up, then relax settings a bit until happy again.
5) As solution evaporates and volume reduced but still very fluid, I transfer the solution to smallest suitable flask. Usually just one change in flask size. I have a 250ml flask coming from Amazon to experiment with.
6) Near end-point, I reduce RPM and allow extract to become somewhat 'thick'. I reduce the RPMs at that point so extract isnt being spead all over inside of flask. Then I increase RPMs up to approx. 120-140 so extract is 'spread' across the spinning bottom of flask. Reduce vac press. to 25 TORR if not already there. I leave it here til no more bubbles present, my end-point in rotovap. As an experiment, I did raise boiling temp to 78C to attempt purging solvent at end-point. But Moe advised this can be detrimental to terps.

POST EVAPORATION

So with the limited equipment and knowledge I have, what are the next steps in having a completed FSO extract? Decarboxylation is definitely on the list. What is the best way to go about decarbing it with the extract? Or should I decarb the flower prior to extraction? Is there other 'final' processes?

One last question for this post. I have so many more questions, but those will be in another post I will make. If extract is to be used in a vape cart or bong, is there any point even worrying about decarbing? Any oil I have made and vaped had a great effect. Would it be better if decarbed?

PICS! Not the greatest pics, but hey. More later. Gotta rush.

 

[Eskander]

Optimal takes some playing with cause it is a balance of vacuum depth, bath temp, chiller temp, chiller pump speed, rotation speed, fill percentage and flask size. Essentially you want to get condensation up about 90% of the condensing coil and have it be stable there. Smaller flasks will never saturate the coil. Large flasks can do so easily and then you will be sucking solvent vapor out the vacuum pump. Just take notes and you will find your optimums quickly enough.

So you can totally decarb in the same flask. You have a mantle right there. Just pop it over to that and drop a thermometer in it. This will also boil off any residual ethanol and water so you can skip your purge step. It will suck up into a syringe easily while hot but the last little bit will be a PITA to get. If you want to do anoxic decarb, you can purge the flask with argon. Probably over the top but if you are around roughnecks, it shouldn't be hard to get.

I know it is one more damn thing but, a diaphragm pump is a solid quality of life improvement. Quieter, no changing oil and no oil fog getting blown off into the air.

Amazon.com

Lastly, a larger collection flask will let you run longer with without breaking vacuum.

Deschem 3000ml,S35 Spherical Joint,Glass Flask,Receiving Vessel,3L 35/20 Lab Ball Socket Reservoir Bottle: Amazon.com: Industrial & Scientific

Deschem 3000ml,S35 Spherical Joint,Glass Flask,Receiving Vessel,3L 35/20 Lab Ball Socket Reservoir Bottle: Amazon.com: Industrial & Scientific

www.amazon.com

Then to support it:

Amazon.com

Amazon.com

-Eskander

 

[cronicoldguy]

So here it is again. But with the different size boiling flasks. The 2000ml is clean and on the rotovap. The 250ml just delivered - washed and rinsed, 500ml, fresh of the rotovap, and 1000ml washed and rinsed. I am actually glad I chose this rotovap. It is quite versatile given the different flask sizes that can be utilized. I really like and wanted the rotovap Moe.Red has (R-1005). But just couldnt justify the cost for myself.

Now the rotovap.
I am saying this as a novice user. This is, to the best of my experience, my opinion of this particular rotovap.

It is a RE-2000B. Is it a clone or the real deal? I couldnt tell you. No manufacturer tag anywhere that I noticed. Just a tag on the back from BVV with model number and some other info. What I can tell you is that it appears to be a solid unit and well built. Nothing feels or looks cheap. And from what I have done with it so far, meets all expectations. It was easy to assemble without any instructions. The machine works and functions as it should. What scares me about it is the fact I have absolutely no warranty because it is used. LeDAB offered no warranty and I never thought to ask until after the fact. SOL I guess. Who knows? Hopefuly LeDAB has more integrity than I have experienced with them so far.

The motorized lift rises and lowers smoothly with the thumb control on the handle. The heating bath is controlled with the digital control panel. It was simple to figure out how to set the temperature. What other features the panel has if any, again, I couldnt tell you. There was no documentation whatsoever shipped with the rotovap. The rotary RPM is controlled by a rheostat with a digital display. Rotary speed of 170 RPM is max.

The heating bath holds temperature steady at set temp. I only noticed maybe a 1-2 degree fluctuation while running rotovap. It is seperate from the main unit so it can be positioned optimally. All sizes of flasks I have submerge into bath adequately. I havent tested the temperature range on it, so I cant vouch for that. I have only had it as high as 78C. There is only a 1-2 degree difference in the temperature displayed by the rotovap and the temperature displayed by the traceable thermometer I had in the bath. So can we assume the temp displayed by the rotovap is kinda accurate? LeDAB sells the heating bath for this unit separately as well. So I am not sure if that is an indication of it's longevity. One that note, you can also purchase the boiling flask adapter separately.

The receiving flask could be bigger for sure. It has a ball connection and clamp, so no other flask I have will work. It does however have a drain valve on the bottom. Nothing to take apart to drain. Just kill vacuum, release vac pressure, and open valve. Unfortunately, the valve cock I received is missing it's o-ring. I have to keep the drain hose on the receiving flask and pinched to seal. I am hoping Zach at LeDAB remembers this and ships the o-ring with the replacement of Celite. I did receive the refunded amount for the rotovap. But no shipping confirmation for the Celite as of this posting.

The condenser, from my little experience, seems to be adequate. Quite robust actually. Note: The inlet and outlet of the condenser are not side by side as I thought. I didnt realize this. Just assumed. NOT! I had coolant all over! The inlet is at the top of the condenser and outlet at bottom, with vacuum connection beside it. Everything disassembles easily for cleaning.

It seems to seal well. I was able to pull vacuum down to 23 TORR with the Vevor circulating pump. Couldnt get that low with the pump shipped with the rotovap. Used and fucked?

Overall, I have to say this is a great unit and recommend it if looking for a rotovap this size. I am sure it can be bought cheaper than I got mine for. I paid a premium to get one available in Canada. I could have got a brand new one for the amount I paid for this one used. That is if I wanted to wait another month and hope it was actually shipped. I think I mentioned above somewhere to the effect of nobody has ever accused me of being overly sensible. Hence the venture into this hobby of mine.

I am pretty sure I need a cold trap of sorts to protect my vacuum regulator. Can somebody recommend an affordable one that will do the job? I was thinking I could fashion a cold trap from metal, place it in the chiller reservoir at -5C and have it effective. But that would cut down the coolant volume of the reservoir making it less efficient. So I scrapped that idea.
I run a fractional still as well so a cold trap is a necessity I think. I have been running the still without the regulator, but a major pain in the ass. But have been using it with the rotovap. What would the minimum temp for a cold trap be in this application? Is there a rule of thumb for that?

Optimal takes some playing with cause it is a balance of vacuum depth, bath temp, chiller temp, chiller pump speed, rotation speed, fill percentage and flask size. Essentially you want to get condensation up about 90% of the condensing coil and have it be stable there. Smaller flasks will never saturate the coil. Large flasks can do so easily and then you will be sucking solvent vapor out the vacuum pump. Just take notes and you will find your optimums quickly enough.

So you can totally decarb in the same flask. You have a mantle right there. Just pop it over to that and drop a thermometer in it. This will also boil off any residual ethanol and water so you can skip your purge step. It will suck up into a syringe easily while hot but the last little bit will be a PITA to get. If you want to do anoxic decarb, you can purge the flask with argon. Probably over the top but if you are around roughnecks, it shouldn't be hard to get.

I know it is one more damn thing but, a diaphragm pump is a solid quality of life improvement. Quieter, no changing oil and no oil fog getting blown off into the air.

Amazon.com

Lastly, a larger collection flask will let you run longer with without breaking vacuum.

Deschem 3000ml,S35 Spherical Joint,Glass Flask,Receiving Vessel,3L 35/20 Lab Ball Socket Reservoir Bottle: Amazon.com: Industrial & Scientific

Deschem 3000ml,S35 Spherical Joint,Glass Flask,Receiving Vessel,3L 35/20 Lab Ball Socket Reservoir Bottle: Amazon.com: Industrial & Scientific

www.amazon.com

Then to support it:

Amazon.com

Amazon.com

-Eskander

Again, very grateful for your help. Sorry if some of my questions seem dumb.

As you said above, its a balancing act from what I have seen so far. Chiller pump speed is the only variable I cant control. If it is like PC water cooling, higher flow rate for better cooling. I can control the temp though. My chiller only goes down to -5C and only has a 5L capacity.

You mention getting condensation up 90% of the condensing coil. Forgive my ignorance. How do I know this? What is the indication? And what variable sets that? Or is it the combination? Sucking back solvent vapor is going to fuck my vacuum reg sooner or later. Is a cold trap absolutely necessary to run a rotovap? And is a simple trap sufficient? Could you recommend an affordable one?

The reason I am shying away from using the heating mantle(s) I got is the fact both are complete garbage. Cant control temp for shit. That is the reason you see the J-KEM 210 (ebay) above the vac reg in picture. It came with a probe. But not a thermal probe for a heating mantle. However, the probe is available from J-KEM. I also purchased a PolyScience Professional Creative Series Sous Vide to replace the mantle. But there is no stirrer and temp only goes to 99C. I bought it for my fractional still. But rotovap arrived before I had a chance to use it. It is still unopened in the box. Might be a Christmas present to my son and his wife now.

Now to the diaphragm pump. I bought a 2-stage rotary vain pump because I read that diaphragm pumps wear out fast and cant take solvent vapors well, not that it should be. Bad info? I have noticed a lot of robust canna labs utilize them. What are the pros and cons? Can you recommend a suitable one for me that doesnt break the bank? Something middle of the road. If it is going to serve me better and has longevity, I will certainly consider one.

And yes, I already have a couple of lab jacks. So good there.

One last question for the night if I can ask. If raising the temp inside the rotovap to 78C to purge solvent is going to destroy the terps, how are terps retained when decarbing typically at 115C-120C. Or are they lost during decarbing as well?

Again, thanks for the reply.

 

[cronicoldguy]

Filtering

I am having issues with particulate getting past filter paper. Can I get a finer filtering process? Mechanical seal in funnel?

I want to filter down to the finest micron possible. My current filtering process is this:
1) After extraction, course biomass removed with screened strainer.
2) Buchner Funnel prepared with filter paper on bottom. Wetted with solvent under vacuum. While wet and with vacuum, I use my finger and run it around the edge of filter paper to seal to funnel.
3) Scoop in Celite 545, pour in solvent to make a slurry. Mix well in Buchner then apply vacuum to remove solvent and dry the 1/2" cake.
4) I repeat the above using Activated Charcoal to make a second cake above the Celite. Into freezer to freeze.
5) Activated Charcoal mixed into canna solution prior to winterization.
6) After winterization, I filter solution thru the Buchner as quickly as possible to stay low temp.

After this, solution looks crystal clear. But prior to evaporation, I prepare a clean Buchner funnel once more with just a wetted filter paper. Then I triple up 3 coffee filters, place in Buchner, and filter once more before evaporating. Again, solution looks pristine. But after the majority of solvent has been evaped, I can see particulate in the extract. Not exactly sure what it is, but looks like charcoal.

This was the roach experiment. Also, any idea what this is collecting on side of rotovap flask? Is this goodness or is it garbage? Poor winterization - fats, sugars? I do believe this is the run I brought rotovap up to 78C

Different run using bud.

A good buddy with a medical grow permit, gifted me 1.5LB of Chemo to experiment with. In return, I would help him make a batch or two in the future. The bud is so-so to smoke. Nothing stellar. Although very low yielding, it produces a pleasant oil. Nice medium hit and tastes like root beer. It has been great material to learn with. Very grateful to him.
Being this is experimental, I dont want to waste pricey Everclear. So I opted to use e-nrg to save cost. This oil will be for personal vaping only, if used at all. Is this solvent going to extract any different then Everclear/95% ethanol? Meaning; is it going to pull more from the plant, leave desirable compounds behind, or extract the same? Couldnt find much info on it other than a MSDS. If purged properly, can extract be safely vaped?
I burned up the first HP in one batch, trying to establish yield potential. It was very low. I thought I fucked up somewhere, so I did 2x 30g experiments. I used the solvent to flower ratio from the chart below. One 30g batch with entire extraction and filtering process at -21C in the my garage. The second experiment was performed the same, but at room temperature. Both yeilds were very low in my opinion. With that, I am confident I didnt fuck up with the HP extraction. I did 2x washes on the HP extraction in my reactor with constant stirring. Pretty sure I used excessive solvent, so I should have got it all. The room temp experiment did yield a bit more than the sub-zero extraction, but that is to be expected. No?

View attachment 1312387


DRYING FLOWER PRIOR TO EXTRACTION
From what I understand, drying flower prior to extraction is optimally done by freeze drying. I dont have a freeze dryer, but I do have a vacuum oven. Is this a good alternative to freeze drying? If so, can somebody recommend a safe temperature, vacuum pressure, and duration? Or should I just use kitchen oven (lowest setting) as I have been?

SOLVENT TO FLOWER RATIO WHEN EXTRACTING
I have been trying to find some reference as to how much solvent is required for a given weight of flower. Nothing written in stone. Actually, I have found nothing written in stone as far as cannabis extraction goes. What I was able to find is this. Can I safely assume I pulled all desirable compounds available using this method? And once both washes performed, is only squeezing/pressing residual solvent from biomass sufficient? Or is there going to be gold left behind?

I will attach entire article also. Taken from: (Wont let me attach a file. Cant find the link.)

Cannabis Oil: chemical evaluation of an upcoming cannabis-based medicine
Luigi L Romano, Arno Hazeka
Department of Pharmacy, University of Siena, Italy Plant Metabolomics group, Institute of Biology, Leiden University, The Netherlands

View attachment 1312369

Presently weather is -26C. It is expected to drop to below -30C in next couple of days, for about a week. I have one remaining HP (minus the 60g for the 2 mentioned 30g experiments) in garage soaking at -26C. The other full HP is soaking at room temp. I am going to let the sub-zero batch soak for a few days for each wash. Two washes as per the chart above (#3 Ethanol).

In your guys opinion, is 100ml:5g solvent to flower ratio with 2X washes excessive? Not enough? Would it be better to do 4x washes using 1/4 of total solvent volume for each wash? Or is end result going to be the same?

DECARBOXYLATION / PURGING SOLVENT
As I mentioned above, I have a vacuum oven. Could somebody recommend a safe temperature, vacuum pressure, and duration? From what others here suggested, decarbing and purging are complete when no more bubbles present. This is a good rule of thumb to follow? Or are there exceptions?

I realize there are a lot of questions asked. But it is my hope that by the time the average person reads this entire thread, one can competently and successfully make themself a batch of quality FSO at home.

 

[cronicoldguy]

Wow. I guess I should have previewed it prior to posting. Could an admin please delete the last 2 pics below "DECARBOXYLATION / PURGING SOLVENT" in post #94? Not sure what happened there.

 

[cronicoldguy]

WTF?

Was filtering some solution into a 2000ml StonyLab vacuum flask. Flask was almost full and BANG! Fucking bottom broke into the flask. Almost 2L of solution lost to the table and floor. Fortunately it was the Chemo that I had been given, and not primo shit.

I am not sure what the vacuum pressure was at the moment it broke. But I dont believe it was maxed out. There was good flow when it broke. Has anyone had that happen? Cheap glassware? This was the first time this particular flask was put under vacuum. I am the only one who has handled it since delivery. So I know it has not been abused or banged since I have had it. It has never been heated and was at room temp when it broke. It has only ever contained ethanol solution.

Can somebody recommend a decent glassware brand? How does StonyLab rank among glassware? Not too sure I will buy any more of their stuff.

Lesson learned. From now on I will place flask in a catch pan when filtering.

 

[Moe.Red]

Not aware of any issues with StonyLab glass, but I'd bet anything it is made in China right next to all the other glassware companies and private labeled.

So is this one

United Scientific FG5340-2000 Borosilicate Glass Heavy Wall Filtering Flask, Bolt Neck with Tubulation, 2000ml Capacity: Science Lab Filtering Flasks: Amazon.com: Industrial & Scientific

United Scientific FG5340-2000 Borosilicate Glass Heavy Wall Filtering Flask, Bolt Neck with Tubulation, 2000ml Capacity: Science Lab Filtering Flasks: Amazon.com: Industrial & Scientific

www.amazon.com

Which I have used for years under heavy vacuum without issue.

Your vacuum found the weak spot. I doubt if you got a replacement from Stony that it would happen again.

 

[cronicoldguy]

Not aware of any issues with StonyLab glass, but I'd bet anything it is made in China right next to all the other glassware companies and private labeled.

So is this one

United Scientific FG5340-2000 Borosilicate Glass Heavy Wall Filtering Flask, Bolt Neck with Tubulation, 2000ml Capacity: Science Lab Filtering Flasks: Amazon.com: Industrial & Scientific

United Scientific FG5340-2000 Borosilicate Glass Heavy Wall Filtering Flask, Bolt Neck with Tubulation, 2000ml Capacity: Science Lab Filtering Flasks: Amazon.com: Industrial & Scientific

www.amazon.com

Which I have used for years under heavy vacuum without issue.

Your vacuum found the weak spot. I doubt if you got a replacement from Stony that it would happen again.

Thanks for the reply Moe.

Actually, StonyLab is a US company out of NY. That is why I went with StonyLab. I figured a bit better quality coming from the States. Maybe it was a dud, and I got the turd of the batch. Not sure.

I will submit a request for replacement. I doubt I will get it, but worth a try at $120 a piece. As I said, this was the first time it was ever under vacuum.

Given United Scientific is a US company, I will replace the flask with one of theirs. Hell, it even costs less. Thanks for the link.

@Eskander
Thanks for you replies as well. I think I asked you a 'stupid question'. It wasnt stupid to me at the time, but I am sure you were shaking your head. I think I have answered that question with more hands on time with the rotovap. That question was about condenser saturation.
I wasnt sure exactly what you meant by that or how to determine. But with more time actually running the machine, I believe I now know what you were referring to. If I am correct, it is how high upon the condenser coils the solvent is very visible and condensed and flowing?

The more I learn to use the rotovap, the more I am amazed at what it does. The more I use it, the more I learn to tweak it. When I first ran it, I had no real clue. I basically filled the boiling flask half full of solution, got it to temp, rotary at 120rpm, then hit it with vacuum. W R O N G !
It was evaporating like a motherfucker, but the chiller couldnt keep up for shit. Went from -5C to 10C in about 15 mins. WTF? Figured my chiller was a piece of shit and needed a bigger one. Fuck, a chiller bigger than the one I have will cost more than the rotovap did!

Well, my chiller handles it just fine. It could be a bit bigger, but oh well. It will just barely keep up with the condenser saturated at about 60%-70%. But the evap rate is very acceptable in my opinion. I will time it next time and see how long it talkes to evap a liter of solvent.

All in all, I am happy with the purchase. Although it was used and beat when I got it, the rotovap works exactly as it should. It is a quality unit in my opinion. There is nothing about it that seems or feels cheap. The powered lift works smoothly and precisely. The heating bath maintains a consistent temp no problem. I have no problem recommending it.

What I really like about it is the different boiling flask sizes that can be utilized. Use the best size suited to batch size. I usually evap the bulk off in the 2L flask, then while still very liquid, I transfer it to either a 500ml or 250ml flask, rinse the 2L with solvent back into the smaller flask, and complete the task. Little wastage.

And yes, most certainly getting a bigger receiving flask. Pain in the ass shutting down to drain it.

I have so many questions in my quest to learn. But I also dont want to be overwhelming to the point you guys wont reply.

MERRY CHRISTMAS!

 

[cronicoldguy]

WTF?

Was filtering some solution into a 2000ml StonyLab vacuum flask. Flask was almost full and BANG! Fucking bottom broke into the flask. Almost 2L of solution lost to the table and floor. Fortunately it was the Chemo that I had been given, and not primo shit.

I am not sure what the vacuum pressure was at the moment it broke. But I dont believe it was maxed out. There was good flow when it broke. Has anyone had that happen? Cheap glassware? This was the first time this particular flask was put under vacuum. I am the only one who has handled it since delivery. So I know it has not been abused or banged since I have had it. It has never been heated and was at room temp when it broke. It has only ever contained ethanol solution.
View attachment 1313675View attachment 1313676

Can somebody recommend a decent glassware brand? How does StonyLab rank among glassware? Not too sure I will buy any more of their stuff.

Lesson learned. From now on I will place flask in a catch pan when filtering.

UPDATE

Well, StonyLab or the Amazon seller came through. I submitted a request for a replacement. I received a full refund without hassle.

 

[cronicoldguy]

So I am having issues with filtering. I cant for the life of me figure out what this shit is and where its coming from. Are these fats or sugars precipitating out during rotovaping?
My solution looks crystal clear when feeding into rotovap. But after solution becomes concentrated in evap flask, a white crystalline looking substance starts to appear. This is happening with almost every batch.
At first I was thinking it was Celite that got past the filter. So I added another filtering step prior to feeding rotovap. But I am not so sure anymore this is Celite.

Last night I was reducing some solution in the rotovap. This solution was from the night before. I was rotovaping , had a bump and oil splattered all over the inside of flask. So I shut down and used a pipette and solvent to wash oil back down into the pool. Once I added the fresh Everclear to the flask and swished it around, it seemed the 'white crystalline' shit precipitating out again. WTF?
This was after

I am doing extractions at room temp so I can pull all I can from the plant. Maybe winterization issues? My freezer only goes down to -18C. I leave it there for 4 days with Activated Charcoal mixed into it. I also have this issue with sub-zero extractions.

My filtering process is as follows.
1) Wet filter paper with solvent with vac pump running and seal around edges with finger.
2) Mix Celite into slurry in beaker, then pour into Buchner funnel. Turn pump on and draw as much solvent out as possible.
3) Let stand and dry. Then into freezer to -18C.
4) Pour winterized solution thru Buchner.
5) Then prior to rotovap, I filter once more. I use a clean Buchner with a wetted filter paper on bottom. Then I use 3 coffee filters together on top of filter paper.

I am lost with this one. Any help would be appreciated. Any idea what is all over the inside of flask? Poor winterization?