Getting the Green and Waxes Out Afterwards

Leocadius said:

Interesting topic



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Ethanol absolute 99.9% (UV-IR-HPLC) PAI (**) - Panreac
Powdered activated carbon N2 QP - Panreac
Nylon syringe filter 0.20 micron - Albet-Hahnemuehle


Grey Wolf, thanks for sharing

Greetings

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Leocadius,
I purchased one of those syringes. When I tried to use it though, the liquid just went right through it without retaining anything in the filter. Barely any color stayed in the filter. All of it went straight to the mixture below. Do you put much pressure on your syringes when pushing it through? At what point does the activated carbon come in? Do you place that into your syringe or something?

Thanks for sharing!

medicalgreen said:

Leocadius,
I purchased one of those syringes. When I tried to use it though, the liquid just went right through it without retaining anything in the filter. Barely any color stayed in the filter. All of it went straight to the mixture below. Do you put much pressure on your syringes when pushing it through? At what point does the activated carbon come in? Do you place that into your syringe or something?

Thanks for sharing!

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If the charcoal went right through, your pore size is either too large, or you ruptured the membrane.

Small diameter syringes can develop enough pressure to rupture the filter membrane, so some care is required.

neat!!

I had to push extremely hard just to get drops to trickle out.
The drops were not much different color than my original color. Actually not different at all.

I tried one run with a .2 micrometer, and slightly green alcohol only based solution, and nothing changed from the original to the drops that came through.

Im either doing it wrong, or i'm using liquid that's already cleaned up enough. It's prechilled, in the freezer with waxes removed to begin with. Maybe that's the case and there's nothing much more to filter through. I'm getting crystalized glass, anyways, but sometimes desire to clean that color up, and wondering what is wrong with my attempts.

Any thoughts, ideas, or suggestions?

Gray Wolf said:

If the charcoal went right through, your pore size is either too large, or you ruptured the membrane.

Small diameter syringes can develop enough pressure to rupture the filter membrane, so some care is required.

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HI Gray Wolf,
Appreciate your intellect and headiness. You are a chem major A. Much better than Chem D, I would say.
Are you supposed to do this very slow, to begin with, so as not to rupture the membrane? How do you know if you have ruptured it? What are the signs of that? Mine trickled very slowly from the beginning, even though alcohol was the base of the BHO liquid. Not very thick, to describe precise.

I used no carbon. Where does that go? Do you actually place the carbon in the syringe?

I just remembered, my alcohol run was without prechill, and it didn't change color at all I have a few more to experiment with, so I can easily try again. Maybe it's because there were no waxes to filter out, yet coagulated to remove?

Any suggestions? Thanks for sharing. This thread and your knowledge is very much appreciated.

medicalgreen said:

I had to push extremely hard just to get drops to trickle out.

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For more efficient use of a thin filter, it is reasonable first to make a coarser filtering, and then fine-cleaning.
I used paper coffee filter, it misses the coal dust, visible to the naked eye.
Repeated filtration through the same filter significantly reduces the amount of dust, but does not remove it altogether.

Another example of removing green and other dirt via charcoal filtration was illustrated in the recent past
by colleague Grassmann in the https://www.icmag.com/ic/showpost.php?p=2782172&postcount=28

medicalgreen said:

HI Gray Wolf,
Appreciate your intellect and headiness. You are a chem major A. Much better than Chem D, I would say.
Are you supposed to do this very slow, to begin with, so as not to rupture the membrane? How do you know if you have ruptured it? What are the signs of that? Mine trickled very slowly from the beginning, even though alcohol was the base of the BHO liquid. Not very thick, to describe precise.

I used no carbon. Where does that go? Do you actually place the carbon in the syringe?

I just remembered, my alcohol run was without prechill, and it didn't change color at all I have a few more to experiment with, so I can easily try again. Maybe it's because there were no waxes to filter out, yet coagulated to remove?

Any suggestions? Thanks for sharing. This thread and your knowledge is very much appreciated.

Click to expand...

Sorry MG, I was still tracking on LC's post using activated charcoal.

In the processes that I posted, there was no activated charcoal used. That is another technique that can be employed.

If you were to add it to the process, you could either pour it through a charcoal column or mix it with the alcohol oil solution in a separate container and then prefilter before syringe filtering.

Not sure I follow? At what step in the process was the alcohol run without prechill?

The process of removing the waxes by chilling and filtering, doesn't remove stuff that is still in solution. The waxes come away because they fall out of solution and clump together.

If you want to remove the green, which is a water soluble, try the salt water wash with hexane as the solvent.

What Jump said regarding prefiltration. 0.2 microns is the final polish. Something with a lot of suspended solids will plug one of them almost immediately.

I usually use a restaurant size coffee filter or a 150mm Whatman Grade 1 lab filter to rough filter small volumes, and then a 0.45 and 0.2 syringe filter. Depending on clarity of the solution, I may skip the first step and start with the 0.45.

If you put steady even pressure on the syringe filter, and don't force it, you can feel what is happening. With a large syringe there is less difference between the filter size and the piston size, so you are less likely to rupure a membrane.

With a small syringe, with a smaller piston, the difference between the area of the piston and the area of the filter is how many times the piston force is multiplied against the filter face.

If you will start with a little air in the syringe, so that it is last to be sqeezed out, it will purge the filter and you will feel the change in resistance.

Really great reading read in your threads/posts Graywolf....Thanks for taking the time to type this up.

Iam going to be trying this soon but on a small scale; from a small personal med. stash.

The above pic shows the hexane mix layered above the salinated water. The larger jar is just the salinated water. You can see in the bottom layer of the smaller jar the difference in color from the clean water in the other jar.

Unfortunately for me the starting mix wasn't that great so I ended up with a less than desirable product at the end anyways, but I'll try this again sometime in the future.

Psuper said:

The above pic shows the hexane mix layered above the salinated water. The larger jar is just the salinated water. You can see in the bottom layer of the smaller jar the difference in color from the clean water in the other jar.

Unfortunately for me the starting mix wasn't that great so I ended up with a less than desirable product at the end anyways, but I'll try this again sometime in the future.

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Glad to see you getting your feet wet and trying things PS!

If you continue to mix more salt water and hexane and shake it throughly before letting settle out, as well as repeat the step until satisfied, you can remove that remaining green color.

lots of amazing info in this thread! I am constantly reading and researching to find out how to make the best highest % final product, now if only i had more product in the beginning to experiment with

What about doing a distilled water cure to get some of the water solubles out before doing an extraction?

Just curious...

Best Regards,

BT

Blue Tail said:

What about doing a distilled water cure to get some of the water solubles out before doing an extraction?

Just curious...

Best Regards,

BT

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Yup. Lots of ways to start with a cleaner extract, but his thread is about how to get it out afterwards.

A fresh water cure will eliminate some of the water solubles beforehand, but not all and doesn't do much for the waxes.

...but this thread is about how to get it out afterwards.

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oops... I did mean to bring the thread back to its original point, but got lost: meaning, after a pre-extraction distilled water cure, then pick up where Gray Wolf got things going in the first place to get the waxes, and other low-temperature coagulable gunk out.

If the extraction just needs final polishing, we may simply re-dissolve it in 190 proof (~95.5% azeotropic) ethanol and stick it in the freezer overnight at 0F, for the waxes to coagulate and the excess water solubles to precipitate out.

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Thanks Gray Wolf.

Best Regards,

BT

I've a question thats sorta on this topic. I recently did an extraction with 95% iso, then after driving it off I washed with Everclear as per this thread. It worked great and loads of flocculent was filtered out leaving nice clean oil behind, first and second wash were both nice amber color. third wash hasn't been boiled off or cleaned up yet but its much dirtier and greener, going into topical for my knees with it. So what's this question already?
Is there a point to doing the primary extraction with iso other than cost? Would the final extract be as good if it was all done with Ethanol. filtered well then frozen/coagulated and filtered again before driving off?
From what I've been reading (most of it written by spurr or Gray wolf...) it seems the etOH has both polar and non-polar properties, not sure about the iso though.
Seems most of you guru types favor non-polar alkane solvents for primary extraction(hexane, butane, n-pentane...)
Where does denatured alcohol(lazyman's primary solvent of choice i think) figure in? Haven't found any denatured alcohol around yet, though I haven't tried the home de-pot.

Im thinking long term I want to set up a solvent recovery system and wondering if it would be gravy to use only ethanol or if there really is benefit to using other solvents for primary extracting first.

many thanks

after rereading the first pages again I picked out this from spurr's post

"Flavonoid aglycones (no attached sugar) are non-polar (and thus fairly water insoluble), and flavonoid glycosides (sugar attached) are polar (water soluble). Thus cannabis flavonoid aglycones should be present in BHO/BHC because n-butane is non-polar and the non-polar flavonoids are soluble in n-butane; as are most terpenoids/terpenes because they are fairly non-polar too. EtOH is both polar and non-polar, so a EtOH wash of butane concrete works well solublize flavonoid aglycones. Examples of flavone molecules that can be aglycones are quercetin, luteolin, hesperitin, apigenin; as well as some anthocyanidins and isoflavones (aka isoflavonoids). Using EtOH as the primary solvent yeilds a less pure concrete due to inclusion of polar substances such as flavonoid glycosides, chlorophyll, etc"
So this seems to suggest to me that the Ethanol should bring along some flavonoid gylcosides but maybe would not bring as many of the non-polar flavonoid aglycones and terpenes as a highly non-polar solvent like alkanes? plus the water solubles come too of course. Though in the OP Graywolf states

"If the extraction just needs final polishing, we may simply re-dissolve it in 190 proof (~95.5% azeotropic) ethanol and stick it in the freezer overnight at 0F, for the waxes to coagulate and the excess water solubles to precipitate out.

We then carefully decant and filter the alcohol mixture, to remove the coagulated waxes, as well as the chlorophyll, and plant alkaloids which precipitated out as sludge in the bottom of the container."

So bringing along chlorophyl and other undesireable water solubles in the primary extraction, while obviously not ideal, isn't too bad since they will precipitate out in the freezer? But then too might the flavonoid glycosides.
I've been trying to figure out why the waxes and lipids would coagulate out of the ethanol, but not he isopropyl.
There certainly is a lot of gunk that settled out when I collected the isopropyl but a fair amount of it was particulates that made it through the pantyhose on the way into the collection jar...that went through pantyhose again and a coffee filter when I put it into the pan to boil off. still got a lot more gunk(flocculant?) when I redissolved that concrete in ethanol and froze it.
If Ethanol is both polar and non-polar what about iso? is it both as well? I know it must be polar since its water soluble.
The waxes and lipids if I recall my biology are not polar and thus not water soluble. This suggests using an alkane(highly non-polar) solvent would strip waxes and lipid readily thus making the ethanol wash technique highly desirable for the resulting concrete. yes?

Thanks to all helping me to understand

gOurd^jr. said:

I've a question thats sorta on this topic. I recently did an extraction with 95% iso, then after driving it off I washed with Everclear as per this thread. It worked great and loads of flocculent was filtered out leaving nice clean oil behind, first and second wash were both nice amber color. third wash hasn't been boiled off or cleaned up yet but its much dirtier and greener, going into topical for my knees with it. So what's this question already?
Is there a point to doing the primary extraction with iso other than cost? Would the final extract be as good if it was all done with Ethanol. filtered well then frozen/coagulated and filtered again before driving off?
From what I've been reading (most of it written by spurr or Gray wolf...) it seems the etOH has both polar and non-polar properties, not sure about the iso though.
Seems most of you guru types favor non-polar alkane solvents for primary extraction(hexane, butane, n-pentane...)
Where does denatured alcohol(lazyman's primary solvent of choice i think) figure in? Haven't found any denatured alcohol around yet, though I haven't tried the home de-pot.

Im thinking long term I want to set up a solvent recovery system and wondering if it would be gravy to use only ethanol or if there really is benefit to using other solvents for primary extracting first.

many thanks

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Hi bro!

Most folks that I know around these parts that use ISO or denatured (with Methanol?), do so for cost reasons and because they work well. In simple Economics 101 terms, the greatest utility at the margin.

The fish trap exists only because of the fish! Ohmmmmmmmmm!!!!1

More directly, for what ever reasons, both ISO and Methanol are more aggressive than Ethanol and therefore a subsequent wash in Ethanol drops out more non solubles than if you had started with ethanol in the first place.

Starting with ethanol doesn't necessarily produce a better product, but it does produce less fallout in step two.

Each alcohol produces a different product, but which is better, a Chevrolet, or a Ford (Honda/Toyota), coffee or tea? When it comes to individual tastes, there may be no right answer.

All three of the above mentioned alcohols produce a damn tasty and potent extractions, that are all higher in floral essences than an alkane extraction.

I personally love and covet those flavors, without in any way detracting from my appreciation of a good alkane extraction. Alkane extractions just belong to a totally different "health food group".

Well now, that certainly turned out good! Hee, hee, hee................

Lab Fried day at the pharm and we turned a bottle of pot wash into a delightfully smooth and heady vaporized oil, using a variation of our salt water wash.

Way smoother and headier than the original oil it came from. Snicker, snark, snort..........

Here is how we did it:

When I extract oil, I clean my oil process vessels by adding a dash of 190 proof and heating them to the point of boiling, at which point the condensing alcohol vapors clean the vessel walls and scavenge the remaining oil from the vessel. I call that pot wash and save it to wash out other pots, until it gets pretty dense and roily.

Since it typically contains the denser less soluble portions of the oil, if simply reduced it can be harsh to vaporize.

What we did was pour the pot wash in a separatory funnel, to which we added saturated salt water, a dash of 5% white distilled vinegar to increase the polarity of the water, and hexane.

After shaking well we allowed that to separate and bled off the lower turbid water layer.

We then added more salt water and vinegar, shook it well and repeated the process. After repeating that process a dozen times, or so, we placed the remaining hexane mixture on a stirring hot plate and reduced it down.

When it was for the most part gone, we added Isopropyl and cooked the mixture until it reached 110C/230F at which point we pulled off a sample and tested it by vaporization.

I was delightfully smooth, with a mostly hash taste, and was more potent than the extractions that it was made from, ostensibly because of its higher concentration of active ingredients.

Dude,
I just had a flashback to my chem labs in college.

Rednick said:

Dude,
I just had a flashback to my chem labs in college.

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Hee, hee, hee, me too!