Chromatography and molecular distillation - Cannabis Concentrates - International Cannagraphic Magazine Forums

EugeneOregon · 08-29-2017, 01:31 PM

Hello,

I am a patient and user of extract. I needed purity levels not normally found in Oregon Dispensaries so I have developed my own rig to take dispensary extracts and purify them. I judge potency from vaping the product. I believe that my rig and methods produce nearly pure THC if care is taken on when to switch fractions.

I have many videos created in an attempt to disiminate information. They are listed on Yotube in the same place as these videos. The first video shows my chromatography methods. These four vids are all the same extract but at different phases. The time lapse shows the first fraction collecting as the molecular distillation starts and the second fraction collected much more quickly from an already hot boiling flask.

A Pirani sensor is used on my Vacuubrand vscuum gauge unit. and are listed as accurate down to one micron. My Vacuubrand unit displays ¾ of one micron (.00075 Torr) as the low end so any deepeer vacuum cannot be measured, however my Edwards EM-28 vacuum pump lists an ultimate vacuum at that level (how would they measure it deeper lolz?) so this value is taken as an accurate value understanding that the actual value is likely somewhat lower than the limits of detection.

I post the links below and also use the forum media button to attempt to post them that way too (I am having trouble with Youtube loading the video on preview with the Youtube forum button tool)

IMPORTANT NOTICE: No media files are hosted on these forums. By clicking the link below you agree to view content from an external website. We can not be held responsible for the suitability or legality of this material. If the video does not play, wait a minute or try again later.

I AGREE

IMPORTANT NOTICE: No media files are hosted on these forums. By clicking the link below you agree to view content from an external website. We can not be held responsible for the suitability or legality of this material. If the video does not play, wait a minute or try again later.

I AGREE

IMPORTANT NOTICE: No media files are hosted on these forums. By clicking the link below you agree to view content from an external website. We can not be held responsible for the suitability or legality of this material. If the video does not play, wait a minute or try again later.

I AGREE

IMPORTANT NOTICE: No media files are hosted on these forums. By clicking the link below you agree to view content from an external website. We can not be held responsible for the suitability or legality of this material. If the video does not play, wait a minute or try again later.

I AGREE

https://www.youtube.com/watch?v=BIsiCfcLBL4
https://www.youtube.com/watch?v=D-A-ZsU8ZxQ
https://www.youtube.com/watch?v=tEqoAVjnJZA
https://www.youtube.com/watch?v=uBpuKVaXynE

EugeneOregon · 08-29-2017, 01:33 PM

The youtube media links do not work using the forum youtube tool. Only the links below it work.

mobin · 08-30-2017, 03:01 AM

i like redundancy in my gauges. piranis can corrode or get contaminated. thermocouples are pretty slow and inaccurate but are also limited to 1micronish. Try a cold cathode gauge. Is your gauge properly cleaned and calibrated? Rotary vanes are limited to about a mtorr. Going further requires jumping into new gear/procedures...sorption/getters, diffusion, turbo, etc. The next levels of vac require a shiton of dollars in equipment, parts, etc. As well as cleanliness, a system devoid of outgassy materials (ya.....not around here) and so much more. Wheeeeeeeeee.

EugeneOregon · 08-30-2017, 02:28 PM

Quote:

Originally Posted by mobin

i like redundancy in my gauges. piranis can corrode or get contaminated. thermocouples are pretty slow and inaccurate but are also limited to 1micronish. Try a cold cathode gauge. Is your gauge properly cleaned and calibrated? Rotary vanes are limited to about a mtorr. Going further requires jumping into new gear/procedures...sorption/getters, diffusion, turbo, etc. The next levels of vac require a shiton of dollars in equipment, parts, etc. As well as cleanliness, a system devoid of outgassy materials (ya.....not around here) and so much more. Wheeeeeeeeee.

Can you post the proper cleaning and calibration procedures for a pirani sensor?

mobin · 08-30-2017, 07:49 PM

Quote:

Originally Posted by EugeneOregon

Can you post the proper cleaning and calibration procedures for a pirani sensor?

lookup the max bakeout temp of your gauge.
clean with solvent.
bakeout/vac dry.
check the types of filaments used and check resistance accordingly.
use a zero calibration tube.
return to service.

Old Gold · 10-31-2017, 07:29 AM

I frinally ran my chromatography column with some magnesium silicate in it. As some of you have heard, this - along with other polishing methods like saline washing, acid-degumming, and steam distilling - is largely being used in pesticide cleanup.

I am waiting on silica gel and I have acid-activated and neutral bentonite clays available too.

I ran a small sample of about 7g winterized crude oil dissolved in 50 mL hexane and 5 mL methanol/ethanol mixture. My plan was to wash the column clean with a gradually more polar solvent ratio as it runs. I used 20g magnesium silicate on the first run, in which nothing seemed to separate (I gave it a nitrogen push to get it to drip steadily). Then I re-ran it with twice as much magnesium silicate, and was able to clearly see one darker "band" for a brief moment. As the column ran, that band seemed to dissipate, and the upper portion of the magnesium silicate bed remained coated darker brown. So something got filtered, whether or not I truly eluted any fractions. I opted to not even wash the column clean.

Question for any folks running chromatography columns. How can an optimal flow rate be determined? Prior to running the column...
I believe I ran it way too fast. Would something like 1-5 ml per minute sound right? I was certainly above that...

Also, since I'm on this topic: Is anyone isolating their terpenes via flash chromatography? It seems like the most promising method to me, aside from perhaps what CO2 can do. I have no experience running CO2 extracts, nor do I hang around many people who do. It does seem like a most logical solvent, considering lack of toxicity and ease of evaporation. Not to mention that is an inefficient solvent by nature, thus, actually making it extremely selective, which can be of great benefit. If anything heavier has to be used (e.g. boils above 0 C), then chromatography still seems like a sure bet for isolation. The only fear would be of residual solvent still in the collected terpene fractions, unless the sample size is large enough that you can collect a fraction of entirely terpenes (as they are liquid solvents on their own).

Edit: Oh, and EugeneOregon: Many many thanks for having taken the time to share your findings with us. It didn't go overlooked! People tend to get real "dick-swingy" on the interwebs, so it's too bad [for us] if you no longer care to share anything here haha.

I am having upload issues, so these are the only pictures I have up right now:

First run with 20g magnesium silicate.

Second run with about 40g magnesium silicate.

I think more important than the quantity of adsorbent might be the actual height of the bed relative to the amount of extract running through it. Also, I am going to concentrate the extract down further. Perhaps too much solvent meant little separation. Clarification would be cool!

SkyHighLer · 10-31-2017, 06:32 PM

Old Gold, "I am waiting on silica gel"

They finally have it listed as in stock,

"HiMedia
HiMedia GRM7481-500G Silica Gel 200-400 Mesh, 500 g
Be the first to review this item
Price: $27.00 & FREE Shipping. Details
Only 1 left in stock (more on the way).
Want it Thursday, Nov. 2? Order within 23 hrs 45 mins and choose One-Day Shipping at checkout. Details
Ships from and sold by Amazon.com. Gift-wrap available.
New (1) from $27.00 & FREE shipping. Details"

https://www.amazon.com/HiMedia-GRM74...ca+gel+himedia

Old Gold · 10-31-2017, 07:25 PM

With the money I just spent in the last two days, I'll have to hilariously pass... Unless you wanna grab it for me and give me a reason to come out your way for a long-overdue sesh!

Luckily I have a friend who has excess silikatepulverado-whodenberg gel or whatever the fuck Summit calls that shit.

Thomas@LRL · 10-31-2017, 08:39 PM

I'm looking at adding some acid activated Bentonite to my procedure in the near future, along with some MagSil. I have read that acid activated clays work better for carotenoids and chlorophyll than naturally activated clays, do you have any advice insofar as use? I have seen it as a filter aid and in the boiling flask during distillation but can be problematic if you bump it over into the receiving flask.

mobin · 10-31-2017, 09:35 PM

Quote:

Originally Posted by Old Gold

Also, since I'm on this topic: Is anyone isolating their terpenes via flash chromatography?
If anything heavier has to be used (e.g. boils above 0 C), then chromatography still seems like a sure bet for isolation.

pull some DCM out of some jaspers stripper, water wash the methanol out, dry over calchloride or similar. or get about 10% of whatever you order shippped

08-30-2017, 03:01 AM	#3
mobin Member Join Date: May 2016 Posts: 233	i like redundancy in my gauges. piranis can corrode or get contaminated. thermocouples are pretty slow and inaccurate but are also limited to 1micronish. Try a cold cathode gauge. Is your gauge properly cleaned and calibrated? Rotary vanes are limited to about a mtorr. Going further requires jumping into new gear/procedures...sorption/getters, diffusion, turbo, etc. The next levels of vac require a shiton of dollars in equipment, parts, etc. As well as cleanliness, a system devoid of outgassy materials (ya.....not around here) and so much more. Wheeeeeeeeee. __________________ fully retarded and still can do shit.
	Quote 1 members found this post helpful.

10-31-2017, 07:29 AM	#6
Old Gold Member Join Date: Aug 2015 Location: N/A Posts: 743	I frinally ran my chromatography column with some magnesium silicate in it. As some of you have heard, this - along with other polishing methods like saline washing, acid-degumming, and steam distilling - is largely being used in pesticide cleanup. I am waiting on silica gel and I have acid-activated and neutral bentonite clays available too. I ran a small sample of about 7g winterized crude oil dissolved in 50 mL hexane and 5 mL methanol/ethanol mixture. My plan was to wash the column clean with a gradually more polar solvent ratio as it runs. I used 20g magnesium silicate on the first run, in which nothing seemed to separate (I gave it a nitrogen push to get it to drip steadily). Then I re-ran it with twice as much magnesium silicate, and was able to clearly see one darker "band" for a brief moment. As the column ran, that band seemed to dissipate, and the upper portion of the magnesium silicate bed remained coated darker brown. So something got filtered, whether or not I truly eluted any fractions. I opted to not even wash the column clean. Question for any folks running chromatography columns. How can an optimal flow rate be determined? Prior to running the column... I believe I ran it way too fast. Would something like 1-5 ml per minute sound right? I was certainly above that... Also, since I'm on this topic: Is anyone isolating their terpenes via flash chromatography? It seems like the most promising method to me, aside from perhaps what CO2 can do. I have no experience running CO2 extracts, nor do I hang around many people who do. It does seem like a most logical solvent, considering lack of toxicity and ease of evaporation. Not to mention that is an inefficient solvent by nature, thus, actually making it extremely selective, which can be of great benefit. If anything heavier has to be used (e.g. boils above 0 C), then chromatography still seems like a sure bet for isolation. The only fear would be of residual solvent still in the collected terpene fractions, unless the sample size is large enough that you can collect a fraction of entirely terpenes (as they are liquid solvents on their own). Edit: Oh, and EugeneOregon: Many many thanks for having taken the time to share your findings with us. It didn't go overlooked! People tend to get real "dick-swingy" on the interwebs, so it's too bad [for us] if you no longer care to share anything here haha. I am having upload issues, so these are the only pictures I have up right now: First run with 20g magnesium silicate. Second run with about 40g magnesium silicate. I think more important than the quantity of adsorbent might be the actual height of the bed relative to the amount of extract running through it. Also, I am going to concentrate the extract down further. Perhaps too much solvent meant little separation. Clarification would be cool! Last edited by Old Gold; 10-31-2017 at 07:58 PM..
	Quote 1 members found this post helpful.

10-31-2017, 06:32 PM	#7
SkyHighLer Got me a stone bad Mana Join Date: Jul 2013 Location: Southern California Posts: 2,266	Old Gold, "I am waiting on silica gel" They finally have it listed as in stock, "HiMedia HiMedia GRM7481-500G Silica Gel 200-400 Mesh, 500 g Be the first to review this item Price: $27.00 & FREE Shipping. Details Only 1 left in stock (more on the way). Want it Thursday, Nov. 2? Order within 23 hrs 45 mins and choose One-Day Shipping at checkout. Details Ships from and sold by Amazon.com. Gift-wrap available. New (1) from $27.00 & FREE shipping. Details" https://www.amazon.com/HiMedia-GRM74...ca+gel+himedia __________________ Link won't open? 1. Click on the link. 2. Click in the address bar, and use backspace to remove the s in https. 3. Click on the 'reload this page' icon, or hit the return key. Best to Worst Canned Butane List https://www.icmag.com/ic/showpost.ph...6&postcount=28 Cannabis Alchemy by D. Gold https://calgarycmmc.com/E-books/E%20B...0D.%20Gold.pdf Hash oil techniques and solvents for non BHO hash oil? https://www.icmag.com/ic/showthread.php?t=338633 Solvents listed as to polarity https://www.icmag.com/ic/showpost.ph...&postcount=162 The Truth Machine by James L. Halperin (free read provided by the author) https://coins.ha.com/information/ttm.s
	Quote

10-31-2017, 07:25 PM	#8
Old Gold Member Join Date: Aug 2015 Location: N/A Posts: 743	With the money I just spent in the last two days, I'll have to hilariously pass... Unless you wanna grab it for me and give me a reason to come out your way for a long-overdue sesh! Luckily I have a friend who has excess silikatepulverado-whodenberg gel or whatever the fuck Summit calls that shit.
	Quote 1 members found this post helpful.

08-29-2017, 01:33 PM	#2
EugeneOregon Newbie Join Date: Aug 2017 Posts: 47	The youtube media links do not work using the forum youtube tool. Only the links below it work.
	Quote

10-31-2017, 08:39 PM	#9
Thomas@LRL Member Join Date: Oct 2015 Posts: 141	I'm looking at adding some acid activated Bentonite to my procedure in the near future, along with some MagSil. I have read that acid activated clays work better for carotenoids and chlorophyll than naturally activated clays, do you have any advice insofar as use? I have seen it as a filter aid and in the boiling flask during distillation but can be problematic if you bump it over into the receiving flask.
	Quote