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Old 09-14-2017, 01:48 AM #11
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i've messed around with 1st and 2nd pass distillate in a column before, less messy

ive been messing around with degumming agents like edta and have used citric acid for room temp measures after a warm carbon/alc/canna slurry was poured over glass wool, cotton, merek60a silica and DE.

whats after waxes? gums and phosphitides right? degumming time!
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Old 09-14-2017, 03:07 AM #12
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Originally Posted by mobin View Post
a lot of people are paying consultants, which makes it kinda dumb to shit the info out for free or their signature on some paper prevents it.

a good cook can taste food and know how the flavors got there without a recipe, or with some practice figure it out themselves.
yes dollar above all...

and yes because some don't have the exact techniques and knowledge in Chemistry to figure out how to bring out said flavors deserve purity
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Old 09-14-2017, 08:31 PM #13
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At the beginning of the video you show the label of a bottle of silica gel:

"Analtech Catalog #B12050

Silica gel 60 Angstrom pore size

35-75 micron

500 grams"


Is the preferred mesh/micron size for filtering cannabinoids 200-400/37-74?


I found these two, and placed standing orders on each (Amazon doesn't charge you until it ships.)

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

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

Attached screen shots of the product information sheets for the above, and the silica gel HiMedia catalog page.


This stuff is expensive, what's the best deal??
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Old 09-14-2017, 10:04 PM #14
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how does thcA interact with the alumina?

or is your extract decarbed i dont recall.
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Old 09-14-2017, 10:12 PM #15
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Originally Posted by SkyHighLer View Post

This stuff is expensive, what's the best deal??


but i don't think it's available at that price anymore
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Old 09-15-2017, 02:35 AM #16
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See the attachment of the Certificate of Analysis for that specific product below. It contains CaSO4, calcium sulphate, I think you want just pure silica gel like I referenced by HiMedia, check out the catalog page I attached, they clearly differentiate between their silica gels with and without additives, and the product specification sheets indicate nothing but silica gel.
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Old 09-15-2017, 04:39 AM #17
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Depends what he's doing with it. Maybe homemade preparative TLC.

The plain TLC silica is of course useful for dry column flash and pressure chromatography.

General column chromatography size is 70-230, less than that can be used to absorb the sample, adsorb, whatever. Higher mesh numbers are used for vacuum and pressure and TLC. Plain flash is the 230-400, the others can be as fine as 1250. The finer sizes are just ground down more.

Pore size may be important because it usually is, whether silica gel, carbon, zeolite, or alumina. This and surface area varies with the preparation and later degree of heat treatment. These items when sold for labs are often rather different than cheaper goods for other uses. Maybe the Indians are capable of making silica gel that performs the same as Millipore-Sigma products, maybe not. An unspecified pore size is not encouraging.

There are many options and materials for adsorption and desorption experiments on cannabis extracts. It should especially not be difficult to get very good separation of cannabinoids from traces of other components if the acid form is available and is to be decarboxylated.

Haven't seen any of these videos, but one way to remove mono and sesquiterpenes is add steam until they're gone.
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Old 09-15-2017, 10:54 AM #18
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Originally Posted by mobin View Post
how does thcA interact with the alumina?

or is your extract decarbed i dont recall.
I do not believe THCA reacts with alumina. It only interacts.

THC A typically comes through mostly with the first part of the THC fraction but after the orangest and first fractions containing flavinoids/carotanoids/terps in my epxerience on gel. This is apparent when running a silica gel column which is similar to alumina. I have more specific experience with the silica gel to seperate, but alumina works pretty much the same way on a seperation like this. Alumina is better at some things than silica and vice versa.

When running a gradient elution on silica using hexane and ethyl acetate in standard phase mode, at just 10%EA/90% hexane you will see at that gradient a thin orange line (carotanoids) precede all other color bands as it elutes off the column. The THCA will follow this fraction in my experience. Catching 20 ml at a time and ramping up the % of EA per the video on DCVC, at about fractions 4,5,6 you will elute off the THCA typically.

I identify this visually. I allow all solvents to evap at room temp. The sheer beauty of hexane and even EA is how easily they are evaporated away. EA will suck up some water but not like alcohol and it is easy to deal with. When you leave out the seperated fractions overnight enough of the solvent evaporates away to thicken up the oil. In the fraction(s) that has THCA, usually about 20% into the run, the oil will be riddled with bubbles like swiss cheese after leaving out overnight. Like alumina the fractions with just a single pass through the column will overlap (unless you have a breakthrough and figure out how to prevent this).

When using the alumina in reverse phase mode by prewetting it then running from polar towards non polar as shown I do not know when the THCA would elute, but it could easily be identified the same way. I hope somebody will run with it and post something about it because I have been wanting to try a more technical seperation on alumina. The problem is that there is so bloody little data on using alumina for something like this. I am eager to try new things, but also have experience with chromatography enough to know just how many runs it would take to perfect such a new system. It can take months or years to dial in a new solvent system just right and I am spending more time on other aspects of the hobby.

You might discover a GREAT way to seperate this stuff on alumina and doubtless many will but the data is sketchy on this so you might be on your own that way. I bet somebody figures it out. Abrasive grade alumina is pretty cheap so even with a botched experiment you can just dump the alumina, rinse off the extract from it and start over without real expense. Silica is not hideously expensive but it is pricier than alumina by far.
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Old 09-15-2017, 11:30 AM #19
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Originally Posted by SkyHighLer View Post
At the beginning of the video you show the label of a bottle of silica gel:

"Analtech Catalog #B12050

Silica gel 60 Angstrom pore size

35-75 micron

500 grams"


Is the preferred mesh/micron size for filtering cannabinoids 200-400/37-74?


I found these two, and placed standing orders on each (Amazon doesn't charge you until it ships.)

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

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

Attached screen shots of the product information sheets for the above, and the silica gel HiMedia catalog page.


This stuff is expensive, what's the best deal??
I cannot give a specific answer to this.

There are many different products because there are many different opinions.

Generally silica gel is either considered normal phase or reverse phase. I use normal phase gel. Silica gel sold as "C18" is reverse phase. It is spendy stuff but is legendary for organic seperations of difficult compounds. On reverse phase gel the solvent system goes from polar like methanol to non-polar like hexane instead of the other way around of non-polar to polar (hence, reverse phase).

I use standard phase gel. The pore sizes listed and such obviously impact the product but my experience is with just the standard off the shelf stuff at 35-75 microns. There is no "best way" really but since so much data about the use of silica gel is out there I chose to run with standard stuff.

At my hobby level of seperation I have a hard time visualizing any real difference between slightly different grades of standard gel. The finer you get the slower it goes so can be better seperation. Coarse grades elute faster with poorer seperation. However in the hands of a skilled operator each grade can and is used in a highly effective manner.

Every single thing in chromatography will impact each and every seperation. Type of gel, solvents used, rate through column used (vacuum), packing technique, gel type, column width and depth, wet vs. dry loading, and so on. The idea is to select a method that you can repeat PRECISELY on each and every run. This is a core concept. With each run mental notes are taken and a strategy is formed to make the next run better by tuning just one aspect of your setup. Then repeat. Chromatography is easy and pretty cheap but it is very delicate. You are placing a "stain" onto a gel that almost does not wah off. Then you are trying to wash it off one layer at a time, so to speak with the goal to eventually wash it all through.

With hexane and extract alone, the extract WlLL NOT budge through even the top layer of silica gel. I use this phenomena to my advantage. I run much heavier loads than dry loading can accomodate through my column so I "wet load" the sample onto the gel now. This means that I disolve the extract in the minimum hexane need to disolve it. Then I can easily transfer that onto my column without any rush to get the column going becaue it all stays on top.

Then, to get it going and to start the run, I take a pipette and squirt about ½ ml of Ethyl Acetate onto the mix. EA is the polar solvent in this scenario and once even a drop of polar solvent hits it then the comound will begin to move through the column and gradient elution then proceds like normal.

It takes just a teeny tiny bit of the polar solvent to get the stain moving. Add too much and the whole stain washes through all at once. Add too little and the stain just begins to spread out and diffuse with time and seperating it then becomes impossible. So the "dance" you play is a delicate balancing act.

You may pick a gel type and solvent system that turns out to be the industry standard and may work better than any other known procedure. We actually have an opportunity as hobbyists/entrepenuers here. Since all research money is hogtied by prohibition there is no available research online about how to do this with 420 extracts. We get to be pioneers with this. This is why I post. Once a knowledge base of years is built then there will be definitive answers to your questions but for now I suggest being confident in what you do know, make a choice, and then do the grunt work and see what you need to adjust to make it all work
That is the essence of chromatography.

Good luck and post often.
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Old 09-15-2017, 05:34 PM #20
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so I have some questions....like so many all just swirling around.

but long story short I think, would this same effect be achieved by winterizing the BHO?
It seems to effectively be the same process, except that you're just pulling one thing out.

I'm honestly so confused about the steps and orders in which certain things are done, and I'm not in the best position to randomly experiment.

For instance, if I gave my BHO a water wash first to remvoe some water soluables, and then did ethanol winterizing would that have any beneficial effect at all?


Thats just one of many questions.... there are so many steps involved to produce clear tasty(tasteless) extract that it can be a bit daunting at times.
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