Experiments with Water Extraction

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50YearsOfCigars
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Experiments with Water Extraction

Post by 50YearsOfCigars »

===============================================================
NOTE:
At resting between any active process on Sample#1 (the water based extraction) that jar and its content are placed in a home refrigerator about 40F. This is an effort to control any possible mold / bacteria growth;

Process steps as of 06/19/2019

Hold for 12hrs (Process sample#1 = 10g AP / 100ml Distilled Water) at 115F in Utra-Sonic water bath 30 min ON/ 30min Rest
Hold for 12 hrs (Process Sample#2 = 10g AP / 100ml 100% Ethyl Alcohol) at 135F in Utra-Sonic water bath 30 min ON/ 30min Rest
Re-Hold for 12hrs (Process sample#1 = 10g AP / 200ml+added 100ml Distilled Water ) at 135F in Utra-Sonic water bath 30 min ON/ 30min Rest
Extract supernatant fluid from Process Sample#2
Spin down supernatant fluid from Process Sample#2 4500RPM / 1 Hour
HOLD for 4 days: supernatant fluid from Process Sample#2 in 0F home freezer
Evap- Reduce Process sample#1 from 160mls to 60mls
Evap- Reduce Process sample#2 from 90mls to 40mls
Combine Mix Process sample#2 & 1
Spin Down combined sample 4500RPM / 1 Hour
Test A/B with known good sample of previously PG extracted Sample.
====================================================

Flavor Test at end of Process Step 11

isee seperate post at end of the thread 6/19/2019
====================================================

here is where I started: (the experimental “plan”)

the plan would be to do two parallel extractions, one with 100% anhydrous ethyl alcohol, the other with distilled water. Then vacuum dehydrate down both extractions to some reasonable level and experiment with flavor blending of the two, and adding back PG at 50% to get a final concentrate that will store for extended periods. i am concerned about the water extract with mold and bacterial growth. The ‘blending’ with the water extract is to beat the flavor profile issues noted above, as in theory, water ~ should~ extract all flavor elements. But that remains to be seen. Also it reduces the overall water percentage in the final concentrate product and provide a bacteriologic and mold resistant product… Maybe you wind up with in your case with (no added PG) 50% alcohol 50% water. That should store at room temps for long periods, or on the shelf ofyour refrigerator for even longer periods.
I will update this daily or as the state of the Processes change:

“I am making excellent progress on my light bulb invention, I now know 10,000 things that will not work” -Thomas Edison.

I am using 10g of American Patriot as the test tobacco, as I am very familiar with the flavor profile from many previous infusions with PG and EA. For this type of experiment I didn’t want to use a SVL (Single Varietal Leaf). I wanted blend that hits a bunch of broad spectrum flavor profile points, and one that my taste bud are familiar with from past extractions.

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Re: Ongoing Project - Experiments with Water Extraction

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Screen Shot 2019-07-10 at 9.15.57 AM.png
This is way above my pay grade but I came across this paper, you may have seen it and it may be no good anymore. It deals with bacteria growth from organic (soil) in various glycols.
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Re: Ongoing Project - Experiments with Water Extraction

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anon13011326:
you may have seen it and it may be no good anymore
no I have not seen it before, but then again discussion of this potential hazard in our vape extracts and liquids never crossed my radar until now with this water extraction.

Please keep these type of references comming. If you spot any just drop the link here. I want to accumulate some amount of reference material on the subject. I will drop a email to drfarsalinos@ecigarette-research.org and tell him what we are up to here with the water extracts and ask if he has any input.

This issue is in his type of wheel house. i will be interested to see what he has to say.

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Re: Ongoing Project - Experiments with Water Extraction

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CAAB:


I have taken a decidedly unscientific approach to the concept of preservation regarding water-based extracts. I looked in my liquor cabinet for shelf-stable liquors. They were all 80 proof (40% alcohol). That’s what I may aim for. Although for my first extraction, I am going to avoid the alcohol altogether, just to get a better A/B test.

Going forward, I may dilute my extract 40% with 190 proof Everclear for longer term storage. Which would mean that I may need to evaporate the extract that much more to account for the dilution from the alcohol.

I did a Google search on shelf life of wine and spirits. Wines, which typically have a lower alcohol content, are less shelf stable and more prone to degradation in quality if not properly stored. Spirits I believe still benefit from proper storage, but are more resilient.

That said, you want to keep the bottle pretty tightly capped to prevent evaporation and unwanted oxidation.

If you have a bottle of extract that is only half full, you may want to consider using this: https://www.amazon.com/Private-Preserve ... B00IB7PHSE 2

It is used in wines to remove oxygen and replace with inert gas. A little goes a long way.

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Re: Ongoing Project - Experiments with Water Extraction

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CAAB:
a decidedly unscientific approach

I don’t think that’ unscientific at all. There are other things that will keep food borne bacterial and mold at bay. Besides your liquor cabinet, look at your pickle jar. They drop the Ph with acetic acid. bacterial hate low Ph ! The service tray at your neighborhood buffet is required to keep the food above 140F. Same reason, bacterial hate higher temps. or lower temps for that matter, in my fridge. That’s why us vapers sort of “lucked-out” on the PG, as it has been used for years as a way to disinfect ducting and heating / cooling systems in hospitals and operating rooms. It has been know for years that it is a very effective bactericide.

We just have to find a way to get the water based carrier to be bacteria unfriendly. I am going to go the route of 50 % alcohol and that’s why I am bothering to do the EA extraction along side. It is sort of a win-win. I get the bactericide and i get the top note flavor profile that EA is famous for.

EDIT PS: I just posted an email to Dr. Farsalinos, Hopefully we get lucky and he has time to respond.

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Re: Ongoing Project - Experiments with Water Extraction

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I will drop a email to drfarsalinos@ecigarette-research.org and tell him what we are up to here with the water extracts and ask if he has any input.

well, unfortunately that was not very productive:

email
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Re: Ongoing Project - Experiments with Water Extraction

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My Dr. said it was fine. Dr. Daniels, Jack Daniels…

I am working on an H2O extract now, it took a little over 4 hours to reduce by 60% using a dehumidifier with fan in a small enclosed room. So that is an area to work on in terms of a bacteria risk.

I started like a normal ethanol evaporation, but after realizing how slow it was going, I doubled the surface area. I am thinking of tripling the surface area next round. For a 4oz jelly jar of extract (around 80 ml after filtering), I started with a Pyrex 6-cup food storage dish: 6.80 x 8.75 x 1.93 Inches. I am thinking of 3 of those Pyrex containers next time, just so I am minimizing the time in a general bacterial danger zone temperature.

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Re: Ongoing Project - Experiments with Water Extraction

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CAAB:

Can’t rush a good thing I suppose. I tried filling a 4oz mason jar with a straight Virginia. Added distilled water at 195 degrees F for 10 minutes, stirring frequently. This is how I do herbal infusions. Relying on my tea background here. Literally brewed over a thousand pots of tea by my estimates.

Ended up with 80ml extract when pressed in the potato masher. Looked promising, the color was very dark, not like the light amber of an ethanol extract. Also, the leaves were mushier in the press. With ethanol, the leaves are still springy.

Evaporated that down to around 30ml. Would have done more, but lost patience. Need to triple the evaporation surface area next time.

Blended 10% H20 extract with 90% VG. Heated up and shaked a little to get a uniform consistently. Vaped it in SXK doggystyle, as mentioned previously. Not the most ideal, but the only atomizer I have free right now. It tasted like VG basically. Almost no Virginia flavor. Tried pouring some extract directly on coil, very very minimal flavor. That could just be that the water wasn’t a good carrier on the coil I suppose.

I just don’t see the value of ‘steeping’ this e liquid, but I’ll give it a go.

I am going to try to evaporate the Virginia extract down to 15ml, see if that helps.

I am going to try a Perique next in H20. I am going to do a 12 hour extraction at 160 degrees F. Going to evaporate down to 15ml. This will be a better comparison to the ethanol method, as that’s exactly what I do in that area.

I am also thinking of doing a 50/50 PGA/H2O for the third round. I may be able to freeze filter in that case. Probably not down to dry ice temperatures because of the water content. The only thing I can’t wrap my head around at this time is the idea of how the PGA and H20 interact with each other that may enhance or diminish their extraction capabilities.

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Re: Ongoing Project - Experiments with Water Extraction

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CAAB:
Added distilled water at 195 degrees F for 10 minutes, stirring frequently.
Evaporated that down to around 30ml.
Blended 10% H20 extract with 90% VG
Vaped it in SXK doggystyle,
Almost no Virginia flavor.
how the PGA and H20 interact

10 minutes? I am at 24hrs in Utra-Sonic. I think you are going to need more than 10 mins. even though the Water is a better solvent across a wider temp range (see my tech charts from the other PM thread) the cell wall structure is not a trivial barrier. As I always point out “that’s the way Mother Nature made it”, and for good reason, the cell and their contents are to be protected. The only thing she wants flowing into and out past the cell wall barrier is what she has determined to be “OK to Pass”…

The multi solvent system will “extract” from a “chemistry point of view” Their downfall is that you, as the compounding process production chemist will “loose control of certain aspects of the overall process”, as the combined solvent chemistry takes control away from you.

Example is the lowering of temp (freezing stage) to drop out oil/wax. There are other points of issue, I think the most important is that you will not be able to independently control the “reduction percentage”, Once you combine the solvents, in the case of EA and Water it forms an Azeotrope, and read the link, you will see the problem there as it applies to what we are trying to do here. You will also not be able to control the eventual percentage of alcohol on the final mix that is destined for long term storage. I am looking for a target of 50% EA as a bactericide.

But don’t let me thow a road block in your experiments. Please continue whatever approach you feel is interesting. This is uncharted territory, so as per my quote above from Thomas Edison, every “try” is important in building the overall knowledge base of how this water extraction thing might work.

It is kind of amazing, as a great deal of knowledge has been built up over time about how to do EA and PG extractions in the NET world, but for some reason I can not find reference “studies” of NET experimenters that have tinkered with Water and documented their procedures.

I am using the “EDIT” feature of this sites software to continually up date my particular experimental approach. Keep an eye on it. If you want to start a similar “updatable post” that would be productive. Eventually, if all this goes anywhere we can use that to easily write up a little monograph and post it over in the public forum.e-cig to contribute to the overall knowledge-base.

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Re: Ongoing Project - Experiments with Water Extraction

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50YearsOfCigars:
I think you are going to need more than 10 mins. even though the Water is a better solvent across a wider temp range (see my tech charts from the other PM thread) the cell wall structure is not a trivial barrier. As I always point out “that’s the way Mother Nature made it”, and for good reason, the cell and their contents are to be protected.
I thought it might be possible to create an extraction using similar methods to herbal tea, as both are dried leaves. Black tea flavor is extracted rather easily in 195 degree water. Anything over 5 minutes becomes bitter.

In addition, over at the e-cigarette forum, they seemed to do rather quick extractions. I am thinking though that they probably used something with casings and top dressings.

I am not familiar with tobacco processing. I can only assume that the compounds responsible for flavor are more difficult to release. Reminds me more of certain culinary herbs that work better in a slow cooker.

I imagine there are a lot of blind alleys ahead. I am well on my way to knowing 10,000 ways that NET will not work. In case anyone is interested, if 1 mistake equals one ounce of tobacco, you will need 625 pounds of tobacco to discover 10,000 mistakes.

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