The trouble with filtering

[CokFLHX]

I'm hoping to get some advice here. Is there any benefit to me filtering my extract? Other than making it nicer to work with and a must for a separation funnel, the task of filtering takes me FOREVER. I probably don't have the right equipment. Any advice on this would be very helpful.

What I have been doing is mixing the bark and and acidic solution in mason jars. They go through three freeze thaw cycles, followed by as long as I can in a water bath in the crock pot. Ideally 6 or more hours. Anyways after this I have been using a Buckner filter cup and some cheesecloth, with a vacuum pump to get the bigger solids. Cheesecloth is the only filtration medium that doesn't take hours, or produce foam an bubbles that are impossible to deal with. I have some paper filter disks that fit the cup but they pull full vacuum and barely drip. Oh, yeah. My Buckner filter cup on only 60mm wide. So I've been at it literally by the spoonful. The problem is bubbles. Bubbles suck. They fill up the vacuum bottle and it wants to travel down the tube into my pump. When you break vacuum, these bubbles will not pop. I've tried mixing it with the filtered extract and that kind of works enough to pout an extract/bubble mix but it still takes up way too much volume.

I've run it without filtering, but it makes pipetting the pull a pain in the ass. I like using a separation funnel. I don't ever leave behind any solvent that way.

I figure the problem is I have no idea how to properly perform lab procedures., or don't have quite the right equipment.
So, I'm posing a few questions. Is there any benefit to filtering? If so, how in the hell do I do this that doesn't take all day or make too man bubbles to get anything done?

Here is what I have. One of those bucker funnel looking vacuum flasks. It has a nipple for the hose up in the neck that leads to an brake bleed bottle in line to the vacuum pump. The brake bleed bottle is used as a sort of catch for the bubble that get into the line. It give me time to kill the pump before they carry all that acidic goodness to the seals of my pump. I've got a 60mm Buckner filter cup, and I've also got a 5in diameter filter cup, but it gives the same issues at the little one.

The cheesecloth lets through the tiny particles that were the dust when dry. I can put the filtered extract in the fridge overnight and decant, but There is still a lot of extract in the sludgy, pink settled bark that is loaded with good stuff I'm sure, but that stuff is even worse to filter, almost impossible.

Maybe I need to give up the whole idea of filtering. I've had successful extractions without it, and am probably decreasing my yield by not ever basifying my filtered bark.

I did take my filtered bark, reacidify it in a jar, and put it in the pressure cooker at 15psi for an hour one time and after filtering got almost half the yield as the filtered extract. So I know I'm not getting all of it when I filter the bark.


I'm past the point of the novelty of doin it. Looking for the best combination quicker extraction, while maximizing yield.

What say you, wise and grizzled veterans with many extractions under their belt? What say you?

 

[illa]

Here is my advice I hope it helps. I am not sure what stage you are trying to filter but any bark mud and Buchner is no go. I always wished I had time to do a write up on my sequential procedures but am happy to donate an excerpt for now.

You can be very meticulous about decanting and my theory will still prove that it is not good enough.

Do an initial decant of solvents with your turkey baster and let sit in a mason jar. After a few hours you will see much residue settle to the bottom. Simply decant this mason jar into another by pouring slowly, and most of the residue you want to avoid will naturally stick to the bottom. Let this sit for 24 hours and decant a third time and you will still see a micro layer of mud/lye on the bottom of your second mason jar. At this point you are ready for a Buchner funnel with a fine crushed glass filter. Maybe the paper filters work too IDK. Use a 1000ML Buchner and dump it all in under vacuum until your solvent has passed through. Then I go to water wash, if you are interested in that step it uses a seperatory funnel and washing soda and if that doesn't make sense I can explain further.

 

[CokFLHX]

Thanks for taking the time to speak with me.

t seems as though you are talking about filtering the solvent. Im talking about the acidification/extraction stage of an acid base extraction. Specifically the max ion or salt tek by Cyb.

What I have been doing is first pulverizing the bark, then I add hydrochloric acid by dropper to RO water until the acidic solution has a pH of around 2. I add this to my bark. About 200ml-300ml for about 100g bark.

I put this acidic bark solution through three freeze/thaw cycles and finish with about a six hour heat bath.

After the cook, I filter. Or attempt to.
Usually at this point it resembles a chunky thick soup. I don’t think it would decant very well at this stage.

I’ve had the best luck so far with just donning nitrile gloves and pouring the entire jar into a funnel with enough cheesecloth to completely surround the bark and I squeeze out as much as I can. Then. I’ll try to put the semi-wet filtered bark in the small Buckner to vacuum as much liquid as I can. I usually reacidify the bark and extract a second time to be sure I got as much of the good stuff as I can.

If you don’t mind, could you elaborate on your process, or perhaps advise me on how to improve mine, as far as the filtering goes?

 

[CokFLHX]

Here is a picture of what I’m left with after decanting. I know there is valuable stuff in here. How can I filter this? It immediately clogs any sort of filter and won’t let anything through. Even with full vacuum underneath.

 

[illa]

I believer he writes to freeze thaw before acid. I hate the hydrofloric its gross I use white vinegar 1ml per G of bark. If you want to filter after acid, use the cheese bags in this youtube it will make it easier in the end but I do not filter I do not need to. Add base to either filtered or not filtered bark. I believe the base will pull more out of your bark soup if unfiltered. Mud/soup can be used with jar flip tek and solvents will rise and able to be decanted. Do not deviate from Cybs directions is my best advice.

Astro nails the filter in this if you choose this route.

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[CokFLHX]

I believer he writes to freeze thaw before acid. I hate the hydrofloric its gross I use white vinegar 1ml per G of bark. If you want to filter after acid, use the cheese bags in this youtube it will make it easier in the end but I do not filter I do not need to. Add base to either filtered or not filtered bark. I believe the base will pull more out of your bark soup if unfiltered. Mud/soup can be used with jar flip tek and solvents will rise and able to be decanted. Do not deviate from Cybs directions is my best advice.

Astro nails the filter in this if you choose this route.

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Hey! Thanks for replying to my thread. I wanted to ask you some questions.

Why do you say hydrochloric acid is gross? I want to learn as much as I can and I am curious to know what makes you say that.

For me, I small jar of concentrated HCI is much more convenient.

I freeze/thaw the bark in the acid solution.

First, pulverize, then make a soup with the bark and the acidic solution of water and HCI. Then I place in the freezer to freeze.

I guess I thought it would be more effective at breaking down the bark if the freeze/thaw was done with an acidic solution rather than just water.

 

[CokFLHX]

Wanted to post an update. I should have taken pictures…..

I break extractions up into "runs" of 100g-150g of bark per run. I decided not to filter one of my runs so I can compare and see if there is a significant difference in yield….

I just siphoned off the first pull on a non filtered run and the solvent was cloudy as hell. It looked like a re-ex!

I’ll know for sure in about 8hours but I’m thinking I’m done with filtering. Separation funnel is convienent if you’re like me and hate siphoning, but shit fire! I think I e been losing a lot of yield and making waaaaaay too much wirk for myself.

 

[drpotato]

I'm hoping to get some advice here. Is there any benefit to me filtering my extract? Other than making it nicer to work with and a must for a separation funnel, the task of filtering takes me FOREVER. I probably don't have the right equipment. Any advice on this would be very helpful.

What I have been doing is mixing the bark and and acidic solution in mason jars. They go through three freeze thaw cycles, followed by as long as I can in a water bath in the crock pot. Ideally 6 or more hours. Anyways after this I have been using a Buckner filter cup and some cheesecloth, with a vacuum pump to get the bigger solids. Cheesecloth is the only filtration medium that doesn't take hours, or produce foam an bubbles that are impossible to deal with. I have some paper filter disks that fit the cup but they pull full vacuum and barely drip. Oh, yeah. My Buckner filter cup on only 60mm wide. So I've been at it literally by the spoonful. The problem is bubbles. Bubbles suck. They fill up the vacuum bottle and it wants to travel down the tube into my pump. When you break vacuum, these bubbles will not pop. I've tried mixing it with the filtered extract and that kind of works enough to pout an extract/bubble mix but it still takes up way too much volume.

I've run it without filtering, but it makes pipetting the pull a pain in the ass. I like using a separation funnel. I don't ever leave behind any solvent that way.

I figure the problem is I have no idea how to properly perform lab procedures., or don't have quite the right equipment.
So, I'm posing a few questions. Is there any benefit to filtering? If so, how in the hell do I do this that doesn't take all day or make too man bubbles to get anything done?

Here is what I have. One of those bucker funnel looking vacuum flasks. It has a nipple for the hose up in the neck that leads to an brake bleed bottle in line to the vacuum pump. The brake bleed bottle is used as a sort of catch for the bubble that get into the line. It give me time to kill the pump before they carry all that acidic goodness to the seals of my pump. I've got a 60mm Buckner filter cup, and I've also got a 5in diameter filter cup, but it gives the same issues at the little one.

The cheesecloth lets through the tiny particles that were the dust when dry. I can put the filtered extract in the fridge overnight and decant, but There is still a lot of extract in the sludgy, pink settled bark that is loaded with good stuff I'm sure, but that stuff is even worse to filter, almost impossible.

Maybe I need to give up the whole idea of filtering. I've had successful extractions without it, and am probably decreasing my yield by not ever basifying my filtered bark.

I did take my filtered bark, reacidify it in a jar, and put it in the pressure cooker at 15psi for an hour one time and after filtering got almost half the yield as the filtered extract. So I know I'm not getting all of it when I filter the bark.


I'm past the point of the novelty of doin it. Looking for the best combination quicker extraction, while maximizing yield.

What say you, wise and grizzled veterans with many extractions under their belt? What say you?

the reason your filter paper is getting clogged is that you are getting micro-precipitates in your soup. you can pull tannins dry on even a medium vacuum, it wont matter, i turned them into solid waxy blocks that would wonder and amaze how all the fluid was slurped out.


First pass, boil and strain in something that just removes the bark, i use these filter-socks used for pool-filters, its cheap and heat resistant. now you concentrate your acidified soup down. at some point tannins and gunk will precipitate. let them.
dmt acetate wont precipitate its insanely hygroscopic, so no worries.

second pass:
cool the soup and earn more precipitation. it also should help everything settle, the addition of gelatin (beer finings) may help, as could certain aluminum salts provided they work in acidic conditions. you want a flocculant. making micro particles that stick to other microparticles and make them less micro and settle out. beer finings (gelatin) on the other hand i dont believe can be filtered, but you can decant like 96% of it. and either discard or reprocess that remaining gunk much quicker than vacuum filtering multiple volume-capacities of your vacuum filter, plus pouring it out, youll see a bias of, cleanest liquid first, worst last, minimal lossage in your yield.

third pass:
boil even more to reach the concentration youd like to work at, refrigerate again to maximize any precipitation, and then vacuum filter while its cold. since its warming up, particles wil be dissolving actively with response to water temp increasing its solute capacity.

especially if you decant again (let stuff settle but this time pour, not syphon, gently), you should have little issue vacuum filtering most of this fluid.


It also helps a lot to avoid tap water, period. fluoride-complexes and whatever other crap is in the local water supply, or eroding from your water pipes, produces micro particles, when this meets soluble calcium sometimes the particles formed are great at forming a sort of impermeable film over filter paper.
a displacement reaction occurs when two soluble salts meet that, if they were to swap ions, would form a salt where one was now much more soluble than it is, and the other forms a salt which is insoluble entirely in the given solvent. whem solubility is decreasing, such as if you put a hot solution on the filter and now its cooling, more solids are able to form since the product of the exchange can now saturate itself out of the solution.

Heres an example. a while ago i bought a bag of copper sulfate horse supplement, i wanted to make it nice and pure, so i dissolved a bunch in hot tap water and attempted to filter it. for the 5kg bag i had, there was maybe 2 tablespoons of white sediment that formed not including the other 2-3 worth which was the contaminant i wanted to remove, and this is fluffed out volume, it was very little, maybe a gram at most.

every single time i tried to recrystalize and clean it up (since i was adding more tap water at times to rinse and etc), my filter paper clogged immediately with almost no visible particulates doing it, just enough to barely cause discoloration of the paper, despite working with essentially just a moderately pure water soluble salt.
the copper sulfate displaced the calcium in the water, and probably other stuff like iron, forming 2 things: a weird light blue copper complex, and calcium sulfate in a form so fluffy that it formed some sort of gel.

upon using demineralized water, i ceased to have any issues, normal sediments (or what little remained) filtered out no problem. i could have poured that through my high flow filter paper in a normal funnel even.



Using nothing but your distilled vinegar as the water source is a good place to start. get a wash bottle with distilled water and use that than be tempted to collect rinses and such with free tap water.
If you have an AC, you can collect perfectly usable distilled water from that, smelly as it may be sometimes.

Using ammonia as a base can help but ammonia salts can be a little too friendly with solvents, and they also react in an unhelpful way with tannins, however, at least as far as minerals go, theyll end up bound even harder to the water than precipitating out as the tannates saturate the solution upon basifying.

Look up teks that minimize tannins by careful ph control and temp control, avoiding tap water and following methods like that, will give you nice easy to filter slurries and soups every time, it also is like 90% of what causes emulsions, these particles. I found that rinsing my organic phase with demineralized water instead of tap water, totally eliminated permanent emulsion-skin flakes floating around, i noticed that no matter how much i rinsed and filtered it kept happening, albeit to lesser degrees each time, but still. from then on, settle time after shaking in the sep funnel went from 6 hours to 3 minutes.


One last thing. you can also be lazy and just dilute your solutions with 10% of demineralized water and heat for a little while, before any given stage of filtration and that also reduces their formation without addressing the underlying cause.

 

[Sakkadelic]

Since you're doing freeze thaw cycles and long hot water baths, the easy solution to make filtering simpler is to work with shredded bark and not powder, and instead of water baths do gentle simmers.

 

[CokFLHX]

Hey guys thanks for the replies.

Can you explain what you mean by tannins? Are you saying that the bark ground up into a powder and the freeze thaw cycles causes tannins or extremely small particles in solution that clog up the filter paper?

I just quit filtering it. When filtered well, a separation funnel makes it easy to collect the solvent, but the amount of time and work involved to get the bark solution to a point where it will run through the funnel is way more work than just using a seocological pipette with a thumb wheel pump. The only real downside to this is when you are trying to get the last bit, the pipette tends to suck up bits of solid bark which clog the end of the pipette. But even so, it’s way more efficient that going to sll
The trouble of filtering.
That, and all of the material stays in the vessel to be exposed to the solvent so there isn’t that little nagging feeling that you’re wasting the spice that might still be in the filtered bark.

 

[CokFLHX]

Also, to your point about water…. I don’t ever use tap water. Where I work, they have a water treatment facility to make up condensate. It’s R.O. water. Reverse osmosis. It’s completely pure water. I just fill up jugs and use that. I’ve been told that the water out of the RO is cleaner and more pure than anything you could go out and buy.

 

[Transform]

Can you explain what you mean by tannins?

Tannin - Wikipedia

en.wikipedia.org