[mobin]

Originally Posted by BigJohnny

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.

to "water wash" bho it'd have to either be heated water (steam ) that melted the resinous crude well enough to interact and mix or the crude would need to be diluted in a solvent immiscible with water like pentane or heptane. Then the water could interact with more of the crude extract as it is dissolved in the nonpolar allowing polar contaminants to be rejected into the water. Regular water tends to form a larger emulsion section and takes longer to seperate into layers. Adding salt to the water shortens sep times while also aiding in converting non-hydrateable phosphitides(normally not pulled into the water/salt phase) into hydrateable.

In this picture you can see an example of residual gums(NHP) being pulled out of 1st pass distillate.



you can see how those gums will stick to the walls of the glass....highly annoying chasing that crap out of there.

these procedures usually involve a lot of prep or expensive media/chems so for me its beneficial to work with cleaner starting material when aiming for good purity. Also working from a decarb'd start means i shouldn't have to worry about acidic compounds being lost to hydration.

typical freezer winterization is not as efficient as what the OP is demonstrating. the chromo/filter media present will slow the flow of polar substances allowing for retention and separation. IE if the alumina filtered extract were placed in the freezer there would probably be little to no visual chelation of lipids.

there are still many other methods to accomplish the same task at room temperature none the less.

additions of acids/bases can make a whole new pathway to pure compounds.

removing the acidic constituents of a crude extract and working from there is a fantastic way to ensure excellent distillate

[BigJohnny]

so water washing would be pointless. Hypothetically, if I were to soak/wash then dry the plant matter before spraying would that have any effect? would that just be pointless as the same thing would be done in later steps to the oil?

[mobin]

Originally Posted by BigJohnny

so water washing would be pointless. Hypothetically, if I were to soak/wash then dry the plant matter before spraying would that have any effect? would that just be pointless as the same thing would be done in later steps to the oil?

no that would be highly productive, just time consuming.

if you take fresh uncured, this works for cured as well but additional losses from triches floating away will happen if you're not careful.

take your material and fill a see-thru container of some sort, add DI/distilled water and soak for 24 hours. replace the water every day until no visible change occurs. Now test ph and if it's the same as the water you put in you're golden. Dry and extract without terpenes, chorophyll, and a lot of polar shit in the mix and it's a terrific place to start.

Got the idea from my trials at "water curing" flower. It made a smoke that smelled like papers burning, flowers that smell like tea leaves, and was potent and smooth as silk.

[SkyHighLer]

Originally Posted by EugeneOregon

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.

I bought a hard copy of a book G.O. Joe had referenced, it's not the detailed, concise source for much of anything, but what a roundup!!

Many of the edition's are available online to download, including 2017's, which I just noticed and copped.

Purification of Laboratory Chemicals - Armarego

Library Genesis will link you to free high speed downloads (huge book, it's still going to take a few minutes.)

gen.lib.rus.ec


Here's a sample,

Flash Chromatography (FC and HPFC)
A faster method of separating components of a mixture is flash chromatography (see Still et al. J Org Chem 43 2923 1978, DOI: 10.1021/jo00408a041). Flash chromatography has become an extremely useful and popular means of purification of small as well as large quantities of compounds. In flash chromatography the eluent flows through the column under a pressure of ca 1 to 4 atmospheres. The lower end of the chromatographic column has a relatively long taper closed with a tap. The upper end of the column is connected through a ball joint to a tap. Alternatively, a specially designed chromatographic column with a solvent reservoir can also be used (for an example, see the Aldrich Chemical Catalog-glassware section). The tapered portion is plugged with cotton, or quartz wool and ca 1 cm length of fine washed sand (the latter is optional). The adsorbent is then placed in the column as a dry powder or as a slurry in a solvent and allowed to fill to about one-third of the column. A fine grade of adsorbent is required in order to slow the flow rate at the higher pressure, e.g. Silica 60, 230 to 400 mesh with particle size 0.040-0.063mm (e.g. from Merck). The top of the adsorbent is layered with ca 1 cm length of fine washed sand. The mixture in the smallest volume of solvent is applied at the top of the column and allowed to flow into the adsorbent under gravity by opening the lower tap momentarily. The top of the column is filled with eluent, the upper tap is connected by a tube to a nitrogen supply from a cylinder, or to compressed air, and turned on to the desired pressure (monitor with a gauge). The lower tap is turned on and fractions are collected rapidly until the level of eluent has reached the top of the adsorbent (do not allow the column to run dry). If further elution is desired then both taps are turned off, the column is filled with more eluting solvent and the process repeated. The top of the column can be modified so that gradient elution can be performed.

https://en.wikipedia.org/wiki/High-p...adient_elution

[EugeneOregon]

Originally Posted by mobin

View Image

but i don't think it's available at that price anymore

Thin Layer Chromatography is not meant for columns. TLC is done on small plates with the sorbent attatched to the plate. It is best to do a TLC plate prior to a seperation I am led to believe but I never got started with that.

[EugeneOregon]

Originally Posted by BigJohnny

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.

The problem you face with trying a water wash is the fact that so much of the water soluable stuff is wrapped up inside of (entrained) the stuff that is completely immiscible in water. This is why chemists LOVE solvents. It is because once a product is in solution in a solvent that can disolve everything in a compound THEN it is possible to get intimate contact with a different liquid solvent to achieve their ends.

You can indeed get at the water soluable stuff by first disolving everything in a solvent first that is itself miscible in water. Any alcohol will do it. Once the water is added to the alcohol, especially methanol which does not form an azeotrope with water, the alcohol is easily removed by boiling. The alcohol boils away first leaving the water. If pinene is present it leaves the water a telltale white. Anything even slightly miscible in water will be in the water at that point. Cannabinoid will not disolve into water in any quantities that make a difference, so the water then pours off easily along with the soluables.

Let me speak to winterizing as well. That is a process meant to speed the precipitation of "waxes" from the extract. "Wax" can mean a single identifiable compound but usually not. It is a generic term for a group of compounds which contribute to the properties of the "wax" as a whole. Like the word "Hexane" is not the name of a single compound or solvent but rather the name of a group of very similar solvents with very similar properties. So similar in fact that for most purposes they are called by the same group name when mixed together.

So wax also means the proteins present and there are a TON of proteins present in an extraction in the form of DNA strands. These strands are tightly woven helix structures and are tiny. They disolve into methanol easily. Any alcohol will attack certain parts of the DNA strand and has the effect of unravelling the neat helix coil into a long strangly looking wispy white goo looking things. This now unwound strand will be seen as it precipitates out of solution and being sticky and stringy the white strands tend to clump together.

The denaturing of proteins can be witnessed the following way; place a small qty of extract in a white ceramic dish. Put an ounce or so of alcohol into the dish and stir on low heat. Once disolved keep heating slowly and watch. You must pay careful attention because in heated alcohol those wispy strands last about one minute tops. Heat gently and watch the bowl. You will see faint helix strands begin to appear and unravel and seem to just "roll" out of solution before your eyes (assuming the extract has not already been denatured). Then as I mentioned, once the DNA is completely unravelled in the hot alcohol it will begin to shrivel. As it gets smaller it turns black. Then is disappears from view as the tiny black dot it shrinks into gets too small to see. It is destroyed at that point.

Logically of course, a disolved substance normally does not precipitate with heat but by chilling. This is where winterizing comes in. The proteins still denature in alcohol but not very fast when chilled. However they are not destroyed by the heat either. This gives the other parts of the "wax" something to precipitate onto. Sprinkling a pinch of aluminum oxide into dissolved extract will also provide a "precipitation nuclei" as well as just adding some common dust will.

Winterizing for me is not necessary because the alumina seems to also force the "waxes" out of solution, just as lowering the temperature will. The problem you face with winterizing alone is that it is nearly impossible to lower the temp of alcohol down low enough to precipitate out all of the waxes. This style of precipitation is an attempt to selectively fraction the compound in solution but it is problematic if the goal is complete removal of the wax fraction. This is verified by winterizing. Waiting one day. Adding a few pinches of aluminum oxide for nuclei, stir well, and winterize again. Likely you will see more "waxes".

This is really why I switched to the alumina. It just seems like winterizing cannot do a complete job because it solely relies on partial precipitation of a total compound. It is nearly impossible to get a clean and complete wax fraction off this way alone.

[BigJohnny]

Originally Posted by mobin

no that would be highly productive, just time consuming.

if you take fresh uncured, this works for cured as well but additional losses from triches floating away will happen if you're not careful.

take your material and fill a see-thru container of some sort, add DI/distilled water and soak for 24 hours. replace the water every day until no visible change occurs. Now test ph and if it's the same as the water you put in you're golden. Dry and extract without terpenes, chorophyll, and a lot of polar shit in the mix and it's a terrific place to start.

Got the idea from my trials at "water curing" flower. It made a smoke that smelled like papers burning, flowers that smell like tea leaves, and was potent and smooth as silk.

I've thought about doing this, but the question becomes how to dry it and keep it from going moldy....and I'm talking some large quantities.

It would be fairly easy to dump a bunch into a 55 gal bucket, and drain it everyday.....but the drying of such a large amount becomes a daunting task.....and also like you mentioned the loss of trichs which I would mostly likely experience.

[Thomas@LRL]

Originally Posted by EugeneOregon

100% wax removal, no freezer.
Significant alpha pinene removal.
Takes just minutes.
https://www.youtube.com/watch?v=51HJGXaKBDE

Video not available :(

[gaiusmarius]

the video seems to be gone, bummer.

[dabboy]

Um, silly question , why we removal pinene ?