Experiments with Water Extraction

[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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

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.

[50YearsOfCigars]

CAAB:

Doing research on the ultrasonic bath. I see them on Amazon and such for around $80 with a heat setting. They go for 30 minutes. So do you just turn it back on every hour?

I take it you’ve tried this with other extractions. Does it make a significant difference? Do you place your extraction in a container inside the ultrasonic bath, or directly inside the cleaner itself? Seems like it would be convenient for all sorts of things.

[50YearsOfCigars]

CAAB:
Doing research on the ultrasonic bath.

All these home units have to be re-set every 30 minutes. I considered rewiring to constant ON then using a programmable timer to control the cycles, but thought better of that. For safety I never use the units unless I am around to supervise operation. You do not have to be EXACTLY there every 30 mins to re-set, a lot of ‘slop’ is OK. It is a casual thing.

Not sure if all the China product use the same transducers or not. many brand names on Amazon, not sure if all equal quality or not ??

Extraction is placed in Kerr glass jars then you stand them up in the Cleaner. Of course there is a power loss thu the glass, but actually the energy transfers very well, and I do not consider it an issue. You have to do it that way to seal off the extraction from the chamber environment inside the cleaner, because of the heater and the ultrasonic transducer they are generating a very high relative humidity at the surface of the water level. Can’t have that in the extraction jar !

EDIT: if you use 8oz Mason jars, it will fit 4ea at once, so very efficient space wise, but the energy is cut by proportion across those 4 jars, so max ultrasonic energy and efffect is to use 1 jar per session

I feel it makes a difference during the ‘hot bump’ stage in our classical PG extraction techniques. Your milage might vary. Kinnik does not use it, and it is true that if you are going to cold soak for 3-6-12 months after a regular hot bump without Ultrsonic, then the whole thing might be moot as to difference in eventual results obtained. However, in this Water extraction and Hot Ethanol, where it is intended to not use extended follow-on soak / infusions, I think then it is possibly very beneficial.

This one looks nice at the price, ($70) adjustable temp range, 60w transducer

amazon.com

Amazon.com: Mophorn Ultrasonic Cleaner Stainless Steel 3 L Commercial Ultrasonic...

[50YearsOfCigars]

50YearsOfCigars:
Then vacuum dehydrate down both extractions to some reasonable level

I am curious. I was looking into the vacuum chamber idea. As I understand it, the H2O would boil off in a sealed container. Does that cause problems in terms of all that vapor inside the chamber? Would it need to be purged on occasion to remove the excess water vapor?

I am also wondering if the chamber can be rigged to recover ethanol? I was looking into a distillation apparatus, but the cost of all related materials at this time exceeds what I would reasonably spend in a few years on Everclear.

[50YearsOfCigars]

CAAB:
problems in terms of all that vapor inside the chamber?
recover ethanol?
what I would reasonably spend in a few years on Everclear.

right on the chamber issues, but if you look at the design of that iBlaze cheepie you will notice that it has a filtered input ball valve that is vented to the outside room, so you just crack that ball valve from time to time, open the chamber and paper towel out the condensate. The issue is that we do not know how the vane pump will put up with all that on a continuous basis. It might not like it over extended use.
EDIT: I am trying to avoid the cost of expensive cold traps, so will be venting every once in a while. This will be a pain, sort of like dealing with the 30min re-set timer in the Ultra-Sonic, but I am trying to keep the cost very low on the kitchen equipt. -

Sure you can recover the ethanol. How big is the balance in your check book? Here is a link to a company that sells all the “goodies” we need to do this properly, including low temp refrigerators, rotovac, distillation recover, you name it they got it. They are a specialty supplier to the exploding cannabis industry. One good thing there is that they are selling 200proof EA for $65 a gallon, and if you are a new customer you get a 10% discount with a code, so that is a very good deal on EA. I plan to pick up a gallon or two at that price ! they are:

BVV
BVV - Vacuum Chambers & Ovens | Closed Loop Extractors

BVV provides the most economical and effective vacuum chambers, extractors, and material processing equipment on the market.
The only problem with that sort of stuff (besides the $$price), is that you better have a good cover story. Check your local laws. In California it is “presumed” that you are in the “drug business” if you have lab equipment like that your back bedroom.



I just sent them this email:



Their REPLY (this stuff look real good to me!)

[50YearsOfCigars]

23d
Well this is most interesting.

I cleared the Water Extract (Process Sample#1) by centrifuging for 1 hour at 4500RPM. The result was clear liquid, with a debris pellet thrown to the bottom of the centrifuge tube. The Clear supernatant was decanted off the top, then put in a clean tube and frozen for 12 hrs at 0F. Here is a picture of the result.


There is a large amount of some material that dropped out. The question is, of course, what is that dropped out material?

This type of fractional freezing will work with any (water) aqueous solution, regardless of the miscibility of the components, unless the component ratio is close the eutectic point. So I think we can assume the stuff that is ‘dropped out’ is probably material like slightly soluble oils, chlorophyll and complex protein chains. .

Later, I will experiment with examination and testing of the two fractions that this freezing produced. If I get very lucky, the flavonoids representing the ‘tobacco profile’ will be in the clear top layer, and the bottom solids will be undesirable material of the type that causes ‘coil gunking’ in conventions PG extracted NETs. Those would be solids containing just carbonaceous material that can be discarded. If that is the result it would be a very desirable outcome.

water-freeze
water-freeze.jpg
611×876 139 KB
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Testing the Layers:

Well because I do not have a Liquid chromatography–mass spectrometer handy (I need to start a Go-Fund-Me page), I had to do it the old fashioned way. That is, I withdrew samples from the top and bottom layer, mixed them with 1:2 Sample/VG and vaped them on the A/B Berserker setup.

What I got was:
from the top layer: A light sweet floral tobacco.
from the bottom layer: A dense smokie tobacco

So the take away is that:
Both sample contained definite components of the over all tobacco profile.

Since the ‘goal’ is to get a complete tobacco profile (in contrast to Str8vision goals of partial flavor profile extractions) I feel there is no choice but to leave the Water extraction ‘as-is’ and not attempt to stratify it into separate components.

The bottom layer could readily be identified as ‘latakia’ and the top layer could be taste sensed to be very similar to a ‘light Virginia’. So it is interesting that it seems to be possible to split out a professionally blended mixed tobacco by using water extraction then fractional freezing. This is interesting, but probably of little practical use.

This was an interesting diversion, and a test that needed to be performed, but the end result is that I am back on track with my original experimental plan and will proceed with the next step which is vacuum dehydration of each extractions complete sample. Since freeze fractional separation of EA extractions is known to work to separate waxes and oils, I will keep that in the experimental plan, but, for now, will not include freeze fractional separation as part of the Water Samples. (Remember: A little chenisty reminder: In contrast to Ethyl Alcohol, Water is a poor solvent of waxes and oils, so this should not be an issue from the start with Water Extractions)

[50YearsOfCigars]

CAAB:

50YearsOfCigars:
Later, I will experiment with examination and testing of the two fractions that this freezing produced.

Wouldn’t have thought of freezing the water myself. That is interesting. How do you separate out the two fractions? Did you allow the ice to thaw and then decant? Do they remain separate even when thawed? Or would the bottom solids no longer be separated out in liquid form?

50YearsOfCigars:
I cleared the Water Extract (Process Sample#1) by centrifuging for 1 hour at 4500RPM.

I assume here you are trying to remove sediment? Would a 1 micron filter accomplish the same goal? I remember you mentioning that some of the suspended solids are desirable in PG extractions.

50YearsOfCigars:
In contrast to Ethyl Alcohol, Water is a poor solvent of waxes and oils, so this should not be an issue from the start with Water Extractions

This was what I was hoping. That the water would do the job from the beginning.

50YearsOfCigars:
The bottom layer could readily be identified as ‘latakia’ and the top layer could be taste sensed to be very similar to a ‘light Virginia’. So it is interesting that it seems to be possible to split out a professionally blended mixed tobacco by using water extraction then fractional freezing.

That’s very interesting! It makes me wonder how much flavor is removed with freeze filtering ethanol extractions… That was always a concern of mine. What is the flavor casualty inside that gunk? I noticed a lot of gunk especially in blends with Latakia and Dark Fired Kentucky. Will have to try an ethanol extract without freeze filtering.

50YearsOfCigars:
I am back on track with my original experimental plan and will proceed with the next step which is vacuum dehydration of each extractions complete sample

What are your thoughts on oxidation? I plan on evaporating over a dehumidifier. I want to have a large surface area this time around to speed up evaporation. I was concerned more with mold and bacteria growth, but I wonder if the constant airflow will cause some kind of undesirable effect on flavor through oxidation.

[50YearsOfCigars]

50YearsOfCigars

CAAB:
if the constant airflow will cause some kind of undesirable effect on flavor through oxidation.

No I don’t this is an issue. Water itself can act, under very particular and rare not commonly occurring circumstances, as an oxidizer in re-dox reactions, but water is very particular about what the molecule is that will cause it to do behave that way. For example, iron (rusting), but in the case of what we have going on here i think it is a non-issue. I would disregard it as a point of concern.

However, I think you want a HEPA filter over that air supply. I would be concerned about contamination from all the junk that floats around in room air.

Did you allow the ice to thaw and then decant? YES, they remian seperate . more or less. heating and convection currents cause them to ‘blend back’ a little, but as you can see from the pix, I was able to obtain two very separate fractions.

It makes me wonder how much flavor is removed with freeze filtering ethanol extractions:
Your question is good one.
I think this is a concern.
The difference between me and the guys that hang out over at ecig forum, is that I am an old ‘process engineer’ and I ‘ask the right question’ then proceed to experimentally test searching for an answer. They approach it more as a church, lead by pastor Str8vision, and sort of ‘devine’ the answers, or never ask the right questions in the first place.

… what I was hoping. That the water would do the job from the beginning.
Yes, the chemistry of Water as a Sovent is so well suited to our kitchen extractions of tobacco that I can not believe, as I have said several times already, that no one has given it a serious go.

[50YearsOfCigars]

CAAB:

50YearsOfCigars:
However, I think you want a HEPA filter over that air supply. I would be concerned about contamination from all the junk that floats around in room air.

Good point. The fan has a filter, but not HEPA. I have folded cheese cloth over the bowls, but that’s more for bugs and other large stray particles.

Thanks for the clarification on the other items. Very interesting process you have going.

[50YearsOfCigars]

50YearsOfCigars:
So here is something that you can put together for under $20 Actually, most people have the parts hanging around in a junk box anyway. I scrounge my local ‘thrift store’ and get this type of stuff for pennies.

Very clever. Something very affordable. If the finished e-liquid has a good flavor profile, the H2O method will turn out to be a very approachable. Distilled water is less than a dollar a gallon here.

Your shopping list gave me the idea to put some air conditioner filters over the pyrex dishes I use for evaporation. Better than cheesecloth I am thinking and less likely to fall in the dish if properly weighted. Hopefully they won’t hinder airflow too much.

I am thinking the H2O extraction method will need a name when completed, if it works out well. Maybe just ‘H2O Extraction Method,’ lol. Sounds fancier with a Russian name or something. Like the ‘Cherenkov Extraction Method.’ Anyone Russian here?

[50YearsOfCigars]

50YearsOfCigars:

Test A/B with known good sample of previously PG extracted Sample.
Do I have everyone address?
I have @Kinnikinnick but need @anon13011326 and @CAAB please send me your Postal address to PeterRamish@iCloud.com I will send out samples of the first round of this experiment, along with a sample of the Control Extract, and you can do your own TIS

OVERALL “TIS” personal impression:
I, personally, miss the throat hit and the ‘thick mouth-feel’ of a pure multi month PG extraction, but that’s just me. From a 10,000 foot overview the abstracted and absolute flavor profile is a very close match between the ‘experimental stuff’ and the ‘Control PG extract’. An impressive result for a “rapid extraction” (no multi month extended infusion time) and a PG-FREE infusion. No question but that this method will be of use to PG sensitive persons

NEXT: When I get time I will try this with some H&H Dark Fired Kentucky

===============================================

Flavor testing 6/19/2019

METHOD: My standard Dual atty A/B Berserker 18mm 2.5mm SS A/B test protcol

Control Extract Basis Comparison Mix: Atty “A”
MTL: 2.5mmSS on Berserker: 15w
25% Original Standard multi month PG Extraction
25% PG
50% VG
0.7% added over top Nic 100mg/ml

Rated BEST
Test-1 Atty “B”
MTL: 2.5mmSS on Berserker: 16w
30% Sample #3
70% VG
0.7% added over top
A good vape.
This is the best mix-ratio of those tried. The flavor profile is almost identical to Basis Comparison Mix:.
The difference is that there is little throat hit. and the mouth feel is “lighter”. I attribute that to lack of PG.
But this Mix, for a totally non PG mix and considering it is a “rapid extraction” (no multi month extended infusion time) is a very impressive result. It puts the whole experiment solidly in the frame of a successful outcome. (considering it was an initial ‘shot in the dark experiment.)
My take-away: Would have benefited from a further evap down of both the EA and the Water by another 20% reduction.

Test-2 Atty “B”
MTL: 2.5mmSS on Berserker: 16w
50%-Sample #3
50% VG
no nic
Not a usable vape.
This ratio the Sample is too high a percentage of the mix and therefore:
Harder to pick up flavor profile only because there is really not enough vaporized carrier

Test-3 Atty “B”
MTL: 2.5mmSS on Berserker: 16w
50%-Sample #3
12%-PG
38% VG
no nic
Not a usable vape.
At this ratio the Sample is too high a percentage of the mix and therefore:
Harder to pick up flavor profile only because there is really no vaporized carrier volatilized
material. Very little ‘plume effect” to carry into and around taste buds and nostril.
Not a satisfactory vaping experience, only because of the lack of volatilization.

Test-4 Atty “C”
DL Cloud Blow - Wotofo Lush Plus Dual Coil Atty (25w)
30% Sample #3
70% VG
0.7% added over top
Useable if you’re a Minotaur
Whew! Too much for me! This will put hair on you chest!

NOTE: Here is how the Control Sample was made:
Missouri Meerschaum: American Patriot 45g
Batch#-25 8/20/2017 Combined finished and Filtered on 11/06/2017:
130F-8HRS Heat Start
on 10/3/2017 UltraSonic 10hrs Processing
Propylene Glycol 200mls
Batch#-50 10/17/2017
Missouri Meerschaum: American Patriot 45g
200ml EA on 10/17/2017:
UltraSonic 10hrs Processing Start Only

Experimental Process steps as of 06/19/2019 Results in "SAMPLE #3**

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.

[50YearsOfCigars]

CAAB

50YearsOfCigars:
This is the best mix-ratio of those tried. The flavor profile is almost identical to Basis Comparison Mix

Sounds exciting. I think I may need a cliff notes version of this. I think I get where you’re coming from, but I wanted to summarize in a different way.

The Test-1 Atty “B” was a 30% sample of a 50/50 blend of H20 and ethyl alcohol? Each a separate extraction of American Patriot? H20 evaporated down from 160 ml to 60 ml and ethyl alcohol evaporated from 90 ml to 40 ml.

I was thinking of adding the alcohol in pure form at the end in hope of avoiding the coil killing aspect of an alcohol NET extract. Understanding of course this is all new territory, so that may be one of those 10,000 mistakes.

50YearsOfCigars:
Useable if you’re a Minotaur
Whew! Too much for me! This will put hair on you chest!
Test-4 appears to be different in terms of the atomizer? And the vapor production of the atomizer is growing strands of keratin on your thorax?

[50YearsOfCigars]

The Test-1 Atty “B” was a 30% sample of a 50/50 blend of H20 and ethyl alcohol?


EDIT:
Let’s look at it this way

a 10 grams amount of “vapable Liquid in Test#1” is composed of these amounts:

1.2 grams of Reduced Alcohol Extract
1.8 grams of Reduced Water Extract
7.0 grams of Pure VG

to crunch the number above;
3.0 grams of combined flavoring extract
7.0 grams of VG carrier

so the ‘base’ (called Sample#3) is an extract mix of 60/40
60% flavored water /into/
40% flavored alcohol

and the “final vape mix” is
30% combined flavor component
70% VG carrier liquid

CAAB:
I was thinking of adding the alcohol in pure form at the end in hope of avoiding the coil killing aspect of an alcohol NET extract
well yes, but, supposedly, freeze filtered Alcohol NETs are less of a ‘coil killer’… Not sure if that is something you can hang your hat on. Your milage might vary.

If we went the route you suggest (add pure alcohol later) You sould have to go at the 40% rate achieve disinfectant properties, and therefore, to prevent unwanted extreme dilution of the final vape, you would have to reduce the water extract to very high flavor concentrations. But that may be entirely possible and we can put it on the “2DO” list of Mr Edison’s 10,000 items… Thanks for the input ! I will give that a go with my next extraction on this test series (C&D dark Fired Kentucky)

CAAB:
Test-4 appears to be different in terms of the atomizer? And the vapor production of the atomizer is growing strands of keratin on your thorax?
Yes, I sometimes do Direct Lung cloud blowing tests, because the largest percentage of vapers is, by far, that type of user. Whenever I do those test I hate it, but the science got to be done !!! hahaha I think I can make a blanket statment that DL is not a good match for Tobacco NET !!!

[50YearsOfCigars]

CAAB

Hey, a lot to think about here regarding the ELR forum. I will do research.

In any case, I’ve been delayed due to car issues on the H2O extraction method. But I am finally on round 2 of reduction. I tripled evaporation surface area. Still struggling to get down to 75% reduction in 4 hour safety window (self-imposed, just general food advise).

But it got me thinking about my other dehydration projects. I used to do a lot of dehydrated foods. One DIY method was to put your jerky or what have you in the oven on warm with door propped open. I am thinking of doing that for the third attempt. That way the temperature is always kept in a safe range to prevent microbial growth.

I was even considering rigging up my dehydrator for a higher volume of liquids. They sell fruit roll up trays that would be perfect for fast evaporation. But I figure a tobacco product inside the dehydrator would render it unusable for food.

I am thinking that I already am heating the hell out of the tobacco to extract the flavors, so a little more heat in the evaporation phase shouldn’t be a big deal in terms of undesirable effect on flavors.

[50YearsOfCigars]

anon13011326:

A small dehydrator would probably work, it is really nothing more than a low temperature oven with a fan I have a pretty good one and make jerky now and then. Your oven set at the lowest temp might be above what a dehydrator can work at between mid 90F and 155F, the lower temps are best for herb dehydration so I would guess that would be the best for your purpose.

[50YearsOfCigars]

50YearsOfCigars

CAAB:
I am thinking that I already am heating the hell out of the tobacco to extract the flavors, so a little more heat in the evaporation phase shouldn’t be a big deal in terms of undesirable effect on flavors.

Humm, well that is a “cut and try thing”… If it works OK but… I have a food dehyreator the type with trays to make beef jerky and so forth. I tested it witl a very accurate lab thermometer I had hanging around and it was 160F. So I guess Sr8vision would “approve” hahaha -

I would watch out for the home oven with the door open. I would not trust the temp controlers.

I assume you saw my DIY coffee cup warmer gimmick. It works real well. Cruze your local thrift store and se how many parts you can pick up for spare change. I have had very good luck with it.

[50YearsOfCigars]

anon13011326:

yogurt makers run around 115F it was quite a craze and I have seen plenty in thrift stores very cheap, think that would work

[50YearsOfCigars]

CAAB:

So this was very weird. I reduced the Perique H2O extract by 75%, performed a 1 micron filtration. Then added 190 proof PGA at a ratio of 60%H20/40%PGA.

Immediately, the extract ‘curdled’ for lack of a better word. You can see it on the glass a little, but it’s throughout the extract too. Putting it in the refrigerator a while to see what happens.

Any guesses what happened? Should I filter it out? I have guesses, but thought I wouldn’t bias anyone.

[50YearsOfCigars]

anon13011326

Looks like oils separating from water to me

[50YearsOfCigars]

50YearsOfCigars

CAAB:
Perique H2O

Humm, Perique is such an unusual material that this one is really hard to say. Oil is a possibility but in theory the water should not have pick up much if any oil in its part of the extraction.

My best guess is that it is some sort of cellular-protein structures (possible even bacterial or molds which are used in the making of perique which is a fermentation process) that was picked up by the Water (either actually dissolved, partially dissolved, or most likely just suspended), then when you added alcohol they dropped out as cell-proteins like that are non soluble in alcohol. Additionally alcohol acts on cell structures by drawing water out of the inside of the cell barrier. Then you would be left with a lot of “wall debris” which possibly then agglomerated into the visible things you see there. Previously they were there but too small to see as they were very small non aglomerated “intact structures”.

Test: slowly heat the vial up and gently shake. Does the stuff “dissolve” and the liquid clear up?
Test: filter out at say 2.5u and examine the filtrate under a microscope. (seriously, even a 10x jewelers loupe might be good enough)

[50YearsOfCigars]

Here is the extract heated to approx 160 degrees F for 7 minutes or so. Very rough guess here. Gently agitated. Heating it seemed to darken it. Perhaps reduce the layer of whatever that curdled stuff is. But what remains is pretty tenacious.

[50YearsOfCigars]

anon13011326

Question, the heating process of using water, can it be that it is producing an essential oil distillation or should I say extraction. I have read that low temp distillation is being accomplished for waste water removal (oils) etc. as low as 45-50c (120 +/- f), with rather simple means. So removing the pure water from the solution would still leave the oils that were on (not in) the leafs in your solution

[50YearsOfCigars]

anon13011326

50YearsOfCigars:
Perique

I think you hit the nail there the processing of that tobacco uses pressure and moisture which brings out the oils, time, moisture and pressure ferment it.

[50YearsOfCigars]

50YearsOfCigars

I am looking at your two pictures. Although this looks like a precipitate from a chemical reaction process, but I can’t imagine what organic reaction that might be. In inorganic chemistry (what I much more familiar with) it would take things like permanganates to get reactions with alcohols that throw large precipitate matter like what you have there. I keep thinking this must just be oil and debris from the organic processes that were created during the making of the Perique and carried thru . You said you filtered the perique at 1 micron, so what you must have there is oils that are agglomerating, then dropping out

You have me stumped here. Without being there and observing the whole process that got you to where you are at this point I would just be guessing about what exactly is going on. My best guess is oils and proteins that became dissolved in the water/Perique extraction and made it through the 1 micron filter stage, then dropp out when mixed with the alcohol. I am sure it is probably all harmless, but maybe it should be ‘trash canned’ anway . Sorry I can not be of more help.

PS: I certainly got no such similar occurrence with my American patriot experiment. It’s somehting in the Perique. Haha. maybe I need to stop vaping Perique!

[50YearsOfCigars]

CAAB
19d
Stuck it in the freezer a couple of hours. Not much difference. Filtered it in 1 micron again. Very slow going, very mucky. Surprising because just straight water, it filtered through quickly. Something about the alcohol…

I should mention the 1 micron filter is a polyester filter felt. They say 1 micron, not sure how it performs in the real world. I like it because it is thick and grabs oils. Plus forms a better seal on my funnel.



Once filtered, the extract lightened up a bit and looked very clean. I stuck it in the freezer again, will see what happens. Made a finished eliquid at ratio of 80/20 VG/Extract in the meantime. Have to shelve it for the day before I can try it out. Hoping for good flavor and longer coil life.

Next up is Oriental and Dark Fired Kentucky. If the Perique is good enough, I’ll jump straight into @anon13011326 tobaccos.

I don’t know, there’s something fun about exploring new techniques. I like the surprises and mysteries.

[50YearsOfCigars]

I thnk you have seen the famous factory tour. After you see how they make this stuff you can understand that most anything might be in that jar of yours. hahaha

https://www.youtube.com/watch?v=LYYqB4oSa7Q

https://www.youtube.com/watch?v=QXkuquLnXEQ

[50YearsOfCigars]

CAAB

Well I’m probably going to die, because I read on the ELR forum that anything water is going to kill me. At 12:15 in video one, listen to what he says. He hydrates it with water. And how many months does it sit there? So obviously that’s going to kill anyone who smokes perique in a pipe too.

It’s got me thinking though. Those juices that he speaks of, what if the fermentation can be extended in distilled water in a canning jar? This would be a room temperature extraction for several months. So instead of killing everything in the tobacco, you would feed it in an anaerobic environment.

Similar to the concept of cellaring tobaccos. You don’t want your tobacco bone dry, nor do you want it vacuum sealed. You want it a little loose to let the microbes do their job. Especially with Virginias.

Could even throw some bourbon soaked oak chips in there or something to emulate the oak cask feel.

I think I will try this, a six month extraction at room temperature of a few tobaccos in H2O. Have to do a little more research though. You’d have to get the environment right so you weren’t growing the wrong stuff.

[50YearsOfCigars]

50YearsOfCigars:
So going forward, will just cut and paste the relevant parts of the PM Water Extraction thread, the EA thread, and the soon to be release thread on my Ferris Wheel contraption (which is almost finished). Then the plan is make a brief post listing the fact that they exist and that if anyone is interested they can contact @Kinnikinnick for a “password”. He has been around here so long that he knows who the trouble makers are, and hopefully we can keep the “technical type” posts free and clear of the nonsense.

I took me a little while to understand how to work the software to accomplish this goal, but I think Ihave it working now.

So you all understand how this will work there will the an INVITEES VIEW of this thread available to certain selected persons that @Kinnikinnick vets and says are not trouble makers. However so you understand clearly all the “side chatter” that we engage in here, like humous ad hominem attacks, and other “under the radar” stuff will be EDITED OUT of what the INVITEE sees in his “special version” of this thread. So don’t feel like you can not wander off topic here in this PM or just make whatever comments you like. Just continue on as usual. I will EDIT OUT everything but the “nuts and bolts” technical comments for the INVITEES VIEW.

I will send you an INVITE to that view so you can see what is happening there, so you can see how an INVTEES VIEW works, If you see any comments in that view that you want deleted just let me know and I will “zap” it.

Because to accomplish the goal of “having control” the formatting will be a little different in the INVITEES VIEW. -You will see ALL POSTS as if they come from @50YearsOfCigars with your referenced post cut and pasted inside.

Let me know what you think.

A this time I have just done the first “translated thread” to INVITEES VIEW of this PM - Water Extraction Experiments but over the next few days will create will create the following:

Methods of Speeding Up Extraction Times
In depth considerations of Ethyl Alcohol Extractions
Tobacco NET Samples Exchange
Advanced Solvent Carrier Reduction Techniques

PS: I think what will happen is that this will be a ‘hierarchical" proving ground, and if the new INVITEES behave and prove themselves over time’ then they can be advanced to access to the real PM thread like this one. We will see how it goes…

[50YearsOfCigars]

CAAB:
I think I will try this, a six month extraction at room temperature of a few tobaccos in H2O. Have to do a little more research though.

Right. I assume you mean researching the possible heath related issues. I will be very curious to see what you turn up. Post any information on that you find, thanks !!!

On the extended steep time for Perique you mention :“what if the fermentation can be extended in distilled water in a canning jar? This would be a room temperature extraction for several months. So instead of killing everything in the tobacco, you would feed it in an anaerobic environment.” - I almost wonder what if you first “autoclaved” the Perique sample? No question that there is a lot of “native bugs” living in the stuff that comes from the little factory buried deep in the woods of Louisiana . Not sure I want to recreate that in an ‘extended way’ in my maceration jar. I jsut want to grab the already existing ‘flavor’, I will leave the actual fermentation steps to those guys you saw in the video

[50YearsOfCigars]

CAAB

Just vaped the Perique pretty hardcore. There is no question that the freeze-filtered hot ethanol extraction is inferior in terms of flavor extraction. The water-extracted Perique has a very distinct flavor. I performed a very similar extraction process.

Unfortunately, I’ve never smoked or vaped a Perique other than the ethanol extraction, so I am not a good judge. But what I am getting here is a very distinct almost fermented hay like flavor, with an oak like undertone. After a good few hits, there is a spicy note on the sides of my tongues, and I lose a little of that fermented hay due to sensory overstimulation. Takes a good 30 minutes to reset the senses and get that fermented hay note. It’s really indescribable. It’s a higher note if you know what I mean, not like a deep Latakia or dark fired Kentucky, but its still very in your face.

Anyway, does that sound about right? Or am did I come up with some local strain of microbes during my evaporation, lol? Or did I filter out too much? I might have to send this to someone more experienced with the flavor.

[50YearsOfCigars]

CAAB

50YearsOfCigars:
On the extended steep time for Perique you mention : “what if the fermentation can be extended in distilled water in a canning jar? This would be a room temperature extraction for several months. So instead of killing everything in the tobacco, you would feed it in an anaerobic environment.” - I almost wonder what if you first “autoclaved” the Perique sample? No question that there is a lot of “native bugs” living in the stuff that comes from the little factory buried deep in the woods of Louisiana . Not sure I want to recreate that in an ‘extended way’ in my maceration jar. I jsut want to grab the already existing ‘flavor’, I will leave the actual fermentation steps to those guys you saw in the video

I’m thinking of going all the way. Extending whatever fermentation is in the tobacco I receive. I would kill off whatever was there by the end of the extended extraction. Problem being that there’s a lot of microbes that might get in between Louisiana and my house, as an example. Also, killing off the microbes may leave any unwanted byproducts. An analogy being rancid meat. You can cook it all you want, but the unhealthy byproducts are there.

I don’t know, a lot of risk and reward there… It’s going to take careful work. But it could be a class of high-end tobacco extractions. A fermented water extraction.

[50YearsOfCigars]

50YearsOfCigars

CAAB:
. There is no question that the freeze-filtered hot ethanol extraction is inferior in terms of flavor extraction

BINGO !!!

CAAB:
Anyway, does that sound about right?

Yep, sounds like you have Perique there !!! hahaha… @Kinnikinnick is the Periques expert around here.

If you want to trade a sample i have a jar of PG Perique going. I can send you some, no problem.

Also where did you get your Perique Leaf sample? Is it a real leaf sample? I know C&D tins some, but not sure if they process it in anyway.

This is the real leaf sample I got. Fro here:
https://www.wholeleaftobacco.com/product/perique/
It is unadulterated:

Whole Leaf Tobacco
Buy Perique Tobacco - A fruity tobacco grown and processed in Louisiana
Perique is a rare, slow burning tobacco. Because of high nicotine, blend it with other tobaccos. Used as a condiment tobacco with a fruity/spice flavor.

[50YearsOfCigars]

50YearsOfCigars

CAAB:
I don’t know, a lot of risk and reward there… It’s going to take careful work. But it could be a class of high-end tobacco extractions. A fermented water extraction.

Humm… well good luck. Do you have a background in biology? You mentioned cross contamination, and so forth. And I thnk you are well aware of the risks. -I am just an ‘engineer type’ but I remember some of the ‘biology stuff’ they forced down my throat in school. So it is a world in itself. If you are professionally involved or trained then you will be well ahead of the game and probably it will be ‘safe to proceed’ .

[50YearsOfCigars]

Kinnikinnick

50YearsOfCigars:
@Kinnikinnick is the Periques expert around here

Errrm, I don’t know about that. I do love a good Va/Per blend though. The Perique which I have extracted is from the Pipes & Cigars site; just your plain old “blending” Perique. I did a heated PG with a couple of months on the shelf… turned out OK.

Edit:
I do have a C&D Perique extract as well.

[50YearsOfCigars]

50YearsOfCigars

Kinnikinnick:
So, you’ll need to explain to me what I’ve received.

Here is how the “Control PG” was made:

NOTE: Here is how the Control Sample was made:
Missouri Meerschaum: American Patriot 45g
Batch#-25 8/20/2017 Combined finished and Filtered on 11/06/2017:
130F-8HRS Heat Start
on 10/3/2017 UltraSonic 10hrs Processing
Propylene Glycol 200mls
Batch#-50 10/17/2017
Missouri Meerschaum: American Patriot 45g
200ml EA on 10/17/2017:
UltraSonic 10hrs Processing Start Only

Here is what the Sample #3 is:

a 3 gram amount of Sample#3 is composed of these amounts:
1.2 gram of Reduced Alcohol Extract of Missouri Meerschaum: American Patriot
1.8 gram of Reduced Water Extract of Missouri Meerschaum: American Patriot

the idea is to get at least 40% Alcohol in the concentrate as a bactericide.
Then (hopefully) the concentrate could be handled as we handle our normal PG concentrate extractions and used in a recipe. As I mentioned, I keep ALL my concentrates and final mixed vape reciepies in a little apartment fridge at 40F. But that’s just me.

[50YearsOfCigars]

CAAB

I think with the water extracts, certain microbial contaminates need to be considered and addressed throughout the whole process.

I’ve tried to keep everything out of the 40 - 140° F range throughout the extraction process.

Of particular concern at this time is botulism. Due to the low oxygen environment of a canning jar and the higher pH content of the tobacco leaf, any naturally present botulism spores would grow at temperatures under 37° F above under 118° F. (Perique?)

From https://www.fsai.ie/faq/botulism.html: 1 Pasteurisation: 70°C 2min or equivalent will kill Cl.botulinum bacteria but not its spores. To kill the spores of Cl.botulinum a sterilisation process equivalent to 121°C for 3 min is required. The botulinum toxin itself is inactivated (denatured) rapidly at temperatures greater than 80°C .

I am working on finding out what kind of effect ethanol has on botulism.

I am thinking we need a cheat sheet of different types of potential microbial contaminates and their operating range. Or just a general rule of thumb of keeping water extracts safe. Botulism, Listeria, Salmonella, E. Coli, Campylobacter come to mind.

Also to keep in mind, the finished extracts are hitting the lungs and not the intestinal tract. It is also making contact in a heated vapor for the most part. Although oral contact with e-liquid happens for various reasons (leaks, spills, etc…).

[50YearsOfCigars]

CAAB

I also found this article which touches upon pH. It explores the different chemical compounds found in the tobacco leaf as well.

https://www.leffingwell.com/download/Le ... nology.pdf 1

[50YearsOfCigars]

CAAB:

50YearsOfCigars:
I will need to accumulate some items from Amazon like pH test strips and so forth.

The lab grows…

50YearsOfCigars:
I agree with you. Let me spend a day or two seeing what I can turn up and then we should discuss this topic in detail. I have a bunch of personal stuff today, so will not be around, but I will bring this to the top of my personal “2DO” list.

Glad you have time to take a look. It sort of hit me, the memory of the whole botulism thing with canning. Even though I’m not canning, I’m following a lot of the same processes.

50YearsOfCigars:
PS: I have a batch of parallel Water/EA going now with some C&D Kentucky Dark Fired. It’s on the Ferris Wheel right now. will leave it spinning 'till next Wed !

I have a few blends going myself. American Patriot is on the list. I will compare with your two samples, and if I don’t botch things, send out samples to anyone interested. BTW, I’ve tried your H2O American Patriot and it’s very flavorful, gives me hope that you don’t need heavy casing for a good NET vape. I have yet to compare with PG control. It’s next on the list. I went a little overboard on the H2O version, lol. Overloaded taste buds on that one.

I have the redneck version of the ferris wheel. About hourly, I take canning jar tongs and rotate the canning jars + give them a good shake. In substitute of ultrasonic bath, I freeze the tobacco in a ziploc bag prior to extraction. Perhaps to encourage cell wall penetration with ice crystals, perhaps to waste my time.

[50YearsOfCigars]

50YearsOfCigars

CAAB:
I think with the water extracts, certain microbial contaminates need to be considered and addressed throughout the whole process.
Here is just a first shot across the bow,… Let me hear you guys feed back on this.

-========================================================
The optimum growth pH is the most favorable pH for the growth of an organism. The lowest pH value that an organism can tolerate is called the minimum growth pH and the highest pH is the maximum growth pH. These values can cover a wide range, which is important for the preservation of food. For example, the optimum growth pH of Salmonella spp. is 7.0–7.5, but the minimum growth pH is closer to 4.2.

What Bacteria and Mold should we test our Water Extracted Tobacco For ?

No concerns for and eliminate these first A & B class of pH group:

A.) Acidophiles growth curve peaks at pH 7 and drops to 0 at pH 5.5 so we can eliminate them from our testing. Acidophiles have optimal growth at pH values near 3

B.) alkaliphile type bacteria that grow in pH roughly 8.5–11 can be disregarded for out testing purposes. alkaliphiles have optimal growth at pH values above 9. so we can eliminate them from our testing.

But must be concerned about this pH group C & D:

AS Most bacteria are neutrophiles and grow best at near-neutral pH (center curve) or plus or munus 2 points.

Of course we only need to be concerned with Pathogenic Bacteria. Since we know from the chart below that most tobacco samples are between 5.2. and 8.5 then we are concerned with bacteria that are are neutrophiles, meaning they grow optimally at a pH within one or two pH units of the neutral pH of 7. Most familiar bacteria, like Escherichia coli, staphylococci, and Salmonella spp. are neutrophils and do not fare well in the acidic pH

C.) First and highest on our list must be bacteria celled neutrophile. Most bacteria are neutrophiles and grow best at near-neutral pH (center curve) within 2 points so takes in a good piece of the pH range we have for tobacco.

D.) Additionally we should be concerned about Aflatoxins which are poisonous carcinogens that are produced by certain molds which grow in soil, decaying vegetation, hay, and grains. They are regularly found in improperly stored staple commodities such as cassava, chili peppers, corn, cotton seed, millet, peanuts, rice, sesame seeds, sorghum, sunflower seeds, tree nuts, wheat, and a variety of spices

We can get these tested for at a local lab (IEH) at a reasonable cost:

http://www.iehinc.com/food-microbiology/

I under lined some suggested stating points in RED

[50YearsOfCigars]

50YearsOfCigars

CAAB:
I also found this article

Oh yes that article has been my Bible for many months now I consult it often, tons of valuable information !

[50YearsOfCigars]

50YearsOfCigars

More on this:

“ I think with the water extracts, certain microbial contaminates need to be considered and addressed throughout the whole process.”

from: https://www.cdc.gov/infectioncontrol/gu ... mical.html

“alcohol” refers to two water-soluble chemical compounds—ethyl alcohol and isopropyl alcohol—that have generally underrated germicidal characteristics. FDA has not cleared any liquid chemical sterilant or high-level disinfectant with alcohol as the main active ingredient. These alcohols are rapidly bactericidal rather than bacteriostatic against vegetative forms of bacteria; they also are tuberculocidal, fungicidal, and virucidal but do not destroy bacterial spores. Their cidal activity drops sharply when diluted below 50% concentration, and the optimum bactericidal concentration is 60%–90% solutions in water (volume/volume)

I propose a method of processing the extracts that goes like this:

1.) after the initial extraction of both the water and the alcohol parallel extracts of the same feedstock tobacco has reached the stage when it the we have now: TWO jars like these:

1.) one of the filtered Alcohol extract
2.) one of the filtered Water extract

We then:

3.) measure the volume of each
4.) Reduce the volume (by evaporation) of the water jar to now measure 30% of the volume of the Alcohol jar
5.) Mix the two in a combining jar and let rest for 24 hrs.
The reason to proceed this way is to obtain the optimum bactericidal concentration is 60%–90% solutions in water (volume/volume) as noted from the CDC paper on “Chemical Disinfectants -Guideline for Disinfection and Sterilization in Healthcare Facilities (2008)”

Hopefully we can assume that at this point we have a combined extract that is free of common pathogens.

The temptation is to proceed to a further step like the following, but it is frought with problems:

Consider if we now do this:
and proceed to further step:

6.) Reduce the Combined Liquid by 50% for final vape Concentrate use.
We now have a problem: It is important to note that rates of evaporation of each ingredient even in azeotropic mixtures like Alcohol and Water. change at a varying rate as a forced evaporation process is used. From the chart below we can see that if the mixture we start with in item 6.) above is, say for example 100mls, and it is composed of 30% Water and 70% Alcohol, then after evaporation to 1/2 total volume of 50 mls, we now have 56.7% by volume of Alcohol. This is marginally below our cutoff for “cidal activity”, but still might be acceptable.

from: https://bayblab.blogspot.com/2009/01/ev ... tions.html

NOTE YELLOW Line= / 70% Alcohol Start Concentration; Terminates at 50% Volume after evaporation.



Which Means:

[50YearsOfCigars]

CAAB

50YearsOfCigars:
Hopefully we can assume that at this point we have a combined extract that is free of common pathogens.

That’s great to know a little more about the alcohol concentration cutoff point. My only thought is that during the processing of the H2O extract, it should still remain in a certain safety range of temperature, because although the pathogens may be destroyed in an alcohol based solution, certain harmful byproducts may remain, such as botulism toxin. So in the case that the H2O extract was in a non-safe temperature range for an extended period, these contaminates may remain even after the addition of alcohol.

That said, an alcohol solution of 60%+ may in fact render these toxins inactive. I haven’t had time to research that.

[50YearsOfCigars]

CAAB:

50YearsOfCigars:
We can get these tested for at a local lab (IEH) at a reasonable cost:

Do you know what a reasonable cost is? What are your thoughts, test one sample or set of samples, or is this a recurring thing?

[50YearsOfCigars]

50YearsOfCigars

CAAB:
certain harmful byproducts may remain, such as botulism toxin.
(…)
Do you know what a reasonable cost is? What are your thoughts, test one sample or set of samples, or is this a recurring thing?

We can get a test for just the botulism toxin. I think it would remain, as it is a very robust compound, and since it is extremely toxic, we probably would not have to lab test for it, as if you ingest even micro-grams during handling there would be no need to test further. Actually, that thought crossed my mind when I found the test listed at EIH.inc, I wondered if anyone actually was able to get a sample to them that tested positive? hahaha…

The ‘reasonable cost’ is $35 per each test, so that does add up fast. And yes, the way this would be done properly is testing each batch cycle, so that is a tremendous ongoing cost. I guess I was thinking this would be reasonable for a commercial ‘for profit’ company, and like everything else in this kitchen hobby it is out of reach for us.

[50YearsOfCigars]

CAAB: So this was very weird. I reduced the Perique H2O extract by 75%, performed a 1 micron filtration. Then added 190 proof PGA at a ratio of 60%H20/40%PGA.

Immediately, the extract ‘curdled’ for lack of a better word. You can see it on the glass a little, but it’s throughout the extract too. Putting it in the refrigerator a while to see what happens.

Any guesses what happened? Should I filter it out? I have guesses, but thought I wouldn’t bias anyone.

I just had the exact same experience with my latest Test of CD Kentucky. I added 140mls of the alcohol extract to 60 mls of reduced water extract and got a classic chemistry class milky white oil emulsion result. But, since I was there to observe the reaction, it was clear what was happening: that is: the Alcohol must have been loaded with oil. A classic oil in water emulsion was formed ! No mystery to what was happening there. That is not surprising as alcohol is an excellent solvent for plant oils.

So I put it in the 0F freezer overnight and it is nicely dropping clear, with the oils at the bottom.

[50YearsOfCigars]

So I put it in the 0F freezer overnight and it is nicely dropping clear, with the oils at the bottom.

It is really clearing nicely.

Of course the logical question (which we have asked previously) is

1.) what is the debris composed of? I suspect oils, waxes
2.) we intend to discard the debris material, but the $64 question is: Is there flavor components in there?

[50YearsOfCigars]

Of course the logical question (which we have asked previously) is
1.) what is the debris composed of? I suspect oils, waxes
2.) we intend to discard the debris material, but the $64 question is: Is there flavor components in there?

Yes, this is one of the things I am encountering so far with a cigar extract, a dark fired Kentucky. and a Nicaraguan Seco Jalapa (spelling that one off memory). The substance is a light brown, with a texture that varies from extract to extract. In the Seco Jalapa, it was like cottage cheese. In the cigar extract, it was a little more soupy. I did smell and taste the substance from the cigar extract. Didn't want to go too overboard, because I don't know the nicotine content or really anything about it. Although it was just one cigar. the taste was mild, cigar like. Muted. The smell was more pronounced.

It appears when I add 190 proof Everclear to the reduced water extract. I heated it up to 160 degrees F for about 5 minutes or so and agitated by hand with the Perique, if I recall correctly. It did not dissolve.

The thing is, I am adding straight up Everclear to the water extract. I did not use the Everclear as an extraction medium. I am using the alcohol simply as a preservative. So I don't think the alcohol has any oils in it to start with.

I am wondering if the alcohol and the water interact in such a way as to preferentially bond with one another over this substance. As a result, the substance is left as the odd man out, as it were, and drops out.

As for the flavor question, I created a pure water extract based e-liquid with the cigar and dark fired Kentucky. My plan is then to create a H2O/PGA extract e-liquid where the gunk has been filtered out and see what the difference is in terms of flavor and coil gunking. That's probably going to take a good week or so to get around to.

I may proceed with adding PGA to the rest of my water extracts and filtering this substance out, whether or not there is a flavor profile hit. Simply because I am not sure how to proceed at this point, and I don't want to sit on these water extracts too long in the refrigerator. I could find a way to perhaps blend this substance back in if needed, or skip the addition of ethanol and transfer to a bacteriostatic medium like VG.

This opens up a new can of worms though because then I have to find out at what ratio of water to vg that bacteriostatic properties remain. Also, there is the question of what microbial contaminates may be in the water extract. The PGA would wipe that out most likely. But if no PGA, then it may be necessary to heat the water extract to kill anything off before transferring to a bacteriostatic medium. That is, if the water extract has been out of the food safety window temperature for an extended period.

I am pretty sure my extracts have now exceeded the 4 hour window that is generally advised. This is due to the extended period of cooling off from the 3 heating cycles I put the extracts through. It took me some time to figure out how to best cool off multiple canning jars of extracts while minimizing stress on the glass. There was also a short interval where the cooler was above optimum temperatures. So I am looking at a total of perhaps 6-8 hours of time within the 40°F-140°F temperature range.</r>

[50YearsOfCigars]

CAAB<

Hopefully we can assume that at this point we have a combined extract that is free of common pathogens.

That’s great to know a little more about the alcohol concentration cutoff point. My only thought is that during the processing of the H2O extract, it should still remain in a certain safety range of temperature, because although the pathogens may be destroyed in an alcohol based solution, certain harmful byproducts may remain, such as botulism toxin. So in the case that the H2O extract was in a non-safe temperature range for an extended period, these contaminates may remain even after the addition of alcohol.<br/>

That said, an alcohol solution of 60%+ may in fact render these toxins inactive. I haven’t had time to research that.</r>

[CAAB]

Hey, somewhat tangental. Do you think there is a significant amount of nicotine in an H2O extraction? What about ethanol or PG? I wonder how much nicotine is actually transferred over depending on the method.

[Peter_Ramish]

Do you think there is a significant amount of nicotine in an H2O extraction? What about ethanol or PG? I wonder how much nicotine is actually transferred over depending on the method.

Nicotine is readily soluble in all three: Water; PG; EA.

On the question of 'significant' I would say not. The various feed stocks vary widely in Nicotine content. Depending on the plant variety the leaf content can vary by 500% or more, in certain hybrid that are specifically bred for very high nicotine content the leaf can have as much as 18% but those are never used for combustable blending, so we would never see them or have access to them, so we can disregard them as part of our discussion here.

Because of the low rates of recovery and high rate of dilution involved you are very unlikely to see any meaningful amounts in your extractions.

Nicotiana tabacum is cultivated throughout the world for preparation of cigars, cigarettes, pipe and chewing tobacco. Nicotine constitutes 2-8% of the dry weigh of the cured leaf, although a much larger range exists in some Nicotiana plants. It occurs mainly as the (S)-(-) isomer although 11 % of (R)-(+)-nicotine has been found in smoke condensate from cigarettes due to pyrrolytic racemization of the (S)-isomer. (S)-Nicotine will be referred as nicotine for further discussion

So for example if you have leaf with 3% by weight then in an infusion where you are using 30g you have less than 1.0g of recoverable Nicotine. Diluted into your 150ml PG extraction you will have 0.0067 g/ml. So that is pretty insignificant. You can do the math for other solvent that might be reduced after extract like EA or Water.

[Peter_Ramish]

Because I have been exploring the possibility of using a parallel extraction of Alcohol alongside the Water extraction, then combining the two with a ratio of 60/40 Alcohol/Water, it might be a good idea to look at the Antimicrobial properties of both Alcohol and Tobacco itself:

Here is some information on that:

From: this link: http://bit.ly/2YXlIIi at the CDC "Chemical Disinfectants
Guideline for Disinfection and Sterilization in Healthcare Facilities (2008)"

In the healthcare setting, “alcohol” refers to two water-soluble chemical compounds—ethyl alcohol and isopropyl alcohol—that have generally underrated germicidal characteristics 482. FDA has not cleared any liquid chemical sterilant or high-level disinfectant with alcohol as the main active ingredient. These alcohols are rapidly bactericidal rather than bacteriostatic against vegetative forms of bacteria; they also are tuberculocidal, fungicidal, and virucidal but do not destroy bacterial spores. Their cidal activity drops sharply when diluted below 50% concentration, and the optimum bactericidal concentration is 60%–90% solutions in water (volume/volume) 483, 484.

Ethyl alcohol, at concentrations of 60%–80%, is a potent virucidal agent inactivating all of the lipophilic viruses (e.g., herpes, vaccinia, and influenza virus) and many hydrophilic viruses (e.g., adenovirus, enterovirus, rhinovirus, and rotaviruses but not hepatitis A virus (HAV) 58 or poliovirus) 49. Isopropyl alcohol is not active against the nonlipid enteroviruses but is fully active against the lipid viruses 72. Studies also have demonstrated the ability of ethyl and isopropyl alcohol to inactivate the hepatitis B virus(HBV) 224, 225 and the herpes virus, 490 and ethyl alcohol to inactivate human immunodeficiency virus (HIV) 227, rotavirus, echovirus, and astrovirus 491.

There have been several papers published about the anti-microbial properties of Tobacco and its extracts:
For Example: As an example See the paper at this link http://bit.ly/2ShGIH2

ISSN: 2329-891X
Journal of Tropical Diseases
Anumudu et al., J Trop Dis 2019, 7:2
DOI: 10.4172/2329-891X.1000300
Research Article Open Access
Antimicrobial Activities of Extracts of Tobacco Leaf (Nicotiana tabacum) and Its Grounded Snuff (Utaba) on Candida albicans and Streptococcus pyogenes, tobacco extract compounds that are identified as testing antimicrobials against several strains of microbes. Several studies have demonstrated the antimicrobial properties of tobacco extracts against E coli and S aureus and P aeruginosa.

"Our research is proving the antimicrobial extracts of tobacco to be applied as an antiseptic. It is as an effort to find common ground that can benefit any health-related elements of society and culture grow tobacco," he said.

"Tobacco extract has potential in inhibiting the growth of bacteria E coli and S aureus. The results indicate that extracts the ethanol extraction of essential oil of tobacco is the most widely extracts obtained during the extraction process carried out and the most effective to inhibit bacterial growth," he said.

[Peter_Ramish]

Because a couple of my posts were lost in a 'system crash' I thought I would re-trace a few comments about my impressions, so far, with the Water extractions when combined with a parallel alcohol extraction:

First I would say that on the basis of only one extraction of this type, that is Missouri Meerschaum: American Patriot, it would be not wise to characterize the whole methods ability to produce a desirable flavor profile.

But, at the risk of jumping to conclusions, that I would later have to retract, I will say the following:
It appears that the Water extraction have a similar profile to extraction made only with Alcohol: That is: they pull the lighter top and middle notes of a profile and the bottom or more well rounded tobacco essence is noticeably missing.

I think this is in part due to the fact that I processed the Water extraction with multiple filtering stages. Additionally, the Alcohol extraction was similarly processed with multiple filtration, and also a freeze separation technique before combining with the Water extract. Then the combined Water/Alcohol extraction was put through a final filtration and a freeze separation stage.

I think all this is just too much filtration, and the flavor profile may have very well "took a hit" as a result.

In order to sort out some of these issues with the flavor profile, I have now put in the jars a single Leaf Water Only extraction of a sample of mixed scrap FRONTO leaf that was obtained from LeafOnly. This leaf has been in my cellar for a long time and I have made several PG extractions with it so I am familiar with the profile when extracted classically.

I am going to 'skim sample' this from week to week and see how it goes. When, and if, it gets to the stage that I think it deserves a 'final filtration', I will proceed very slowly and carefully with these filtrations and SFT at each point along that road. FYI this is on my Ferris Wheel, so hopefully the extraction proceeds rapidly.

[Peter_Ramish]

In order to sort out some of these issues with the flavor profile, I have now put in the jars a single Leaf Water Only extraction of a sample of mixed scrap FRONTO leaf that was obtained from LeafOnly. This leaf has been in my cellar for a long time and I have made several PG extractions with it so I am familiar with the profile when extracted classically.

Well I have bad news to report on this experiment:
The short of the long of it is stated in my notes;

30g Fronto WATER extraction 7/08/2019
Discontinued -Dumped on 7/19/2019
Showed signs of Bacterial Growth
Expanded the Cap on Jar, vinegar like off smell

What ever was happening in the jar, it created a positive vapor pressure (gas generation), but upon opening the jar and examining the contents there was no observable signs of growth, no discoloration, no foreign physical structure of growth colonies. However, there was a distinct vinegar like odor and when removing the contents of the Jar the liquid appeared to have a slightly thick and viscous quality which was unlike the expected, and what should have been, thin liquid water.

So at this point, I have decided to discontinue my further experiments with water extraction until I can get guidance from a lab that is in a position to participate in the project. This brings up the ever recurring statements about kitchen chemistry and home extractions, and that is that in many cases there is a need for professional level equipment and testing. It is the cost that becomes the barrier.

However, if you are continuing to experiment with Water Extractions, or you know of documents or references to the topic, please post that information here. Thank You.

[CAAB]

I have a number of 'finished' H2O extracts that I've been sitting on here. There is a microbial safety question that remains unanswered. I believe the addition of ethanol may not deactivate spores. And then there is the problem of the addition of adding the extract to vegetable glycerine for a vapable e-liquid. At certain concentrations of H2O to VG, the VG may actually feed whatever spores remain. That ratio is unclear at this juncture.

It would be difficult to test the extracts I imagine because I am not sure what exactly you would test for. I am thinking of a full dump of all H2O extracts unless I can think of a way to determine they are in fact safe.

Sadly I will have to start all over again if this is the case with some of the excellent recommendations of non-cased pipe tobaccos. This time with a 6 month extraction using PG or VG. Back to square one maybe...

[Peter_Ramish]

I have a number of 'finished' H2O extracts that I've been sitting on here. (..) I am thinking of a full dump of all H2O extracts unless I can think of a way to determine they are in fact safe.

Yes, even if you autoclaved them (a home pressure cooker can do this job ) the problem is still that they may become recontaminated over time. Not to mention that you would probably destroy the flavor profile. So one of the issues with the H20 extractions is that they seem to not be a practical solution (no pun intended..)

I have given a little thought to how I would re approach using water as a flavor solvent. Unfortunately, all methods of approach that seem reasonable to me involve expensive equipment and are well out of the 'kitchen class'. Also the results (from a flavor perspective) are possibly very uncertain as I now would use much higher temps and repeated cycle extractions much like what you see with soxhlet extractors. There are well established methods and existing equipment available for obtaining essential oils from steam distillation. My approach would be similar. But I suggest modifying that type of equipment to obtain cyclic liquid state extractions. Then roto-vap to reduce the extractions to very high concentrations with remaining water at 20% or less. There are well tested and well established (FDA) known levels for food stuffs with low moisture content. They can remain bacteria free and stable for long periods of time.

So, as you can imagine, I don't have the budget to pursue any of that and, again, results (flavor) might be very uncertain.

Another approach, that actually was suggested much earlier on in this set of experiments, was to somehow lower the pH of the water to very low levels. This, however, seems like another dead end, as the result would be un-vapable.

[CAAB]

You gave me an idea. What if I were to evaporate the finished H2O extracts down to 0 moisture content, heat that to a certain temperature, not sure what, and then add ethanol afterwards for recovery of the solid. Of course flavor may be destroyed. Just hate to dump all this. Although sometimes you just have to cut your losses...

[Peter_Ramish]

evaporate the finished H2O extracts down to 0 moisture content, heat that to a certain temperature, not sure what, and then add ethanol afterwards for recovery of the solid.

I suspect you will wind up with so-called 'tobacco concrete'. This is the process whereby Tobacco Absolute is made. This 'concrete' is notoriously hard to re-constitue to a usable form once it has been reduced to a solid. But it is worth a try.

I have about 40mls here of my C&D Kentucky water/EA extract. This was one of my 'parallel' extractions. It has been in the fridge now for over 2 weeks and is in fine shape. it is crystal clear, shows no signs of contamination. But I think I will try exactly what you say and reduce it to a concrete then deal with the effort of trying to re-constitue it. I sure wish I had a vacuum dehydration setup. But I have the 'coffee cup warmer' setup and it holds at about 110F, which is reasonable.

Understand that by doing this, you have a little chemistry issue, you are essentially putting the sample through a liquid/liquid seperation even though there is a drying stage in between the two solvents. The various compounds extracted during the water will remain in the dried concrete and then you will not be able to re-con certain compound that have no solubility in EA. This is the 'tricky part' that makes it such a headache to re-con TA. Apparently it can be done, more or less. I remember reading some anecdotal reports of people that tried the TA re-con, but I don't have those saved on disk so I am just going by memory.

Give it a try and let me know how you make out. I will also perform the same experiment. I agree: something has to be done with these water extractions, because at our present state of knowledge and skill levels with them they probably do pose a certain risk.

[Peter_Ramish]

evaporate the finished H2O extracts down to 0 moisture content,

I suspect you will wind up with so-called 'tobacco concrete'.

Well, good news! I evaped 40mls of my Water Extracted C&D Kentucky Dark Fired overnight and got it down to a very thick oily film on the bottom of my 'coffee cup' dehydrator. It did not make it all the way to a solid 'concrete'. I am sure there was a very little moisture left in there, but not much. The only way to completely dehydrate a material like this to 0 is in a vacuum setup. The good news is that whatever this oily film is, turns out it is readily soluble in 100% Pure VG ! I added 30mls of Pure VG and warmed up the mixture back to 100F and all of it readily dissolved with a small amount of stirring. I then decanted it into a bottle and topped up with 5mls of 100% EA, this was in an effort get the result less viscous so that it could be handled in a vape recipe.

I withdrew a 1ml sample into a tester 'ant-cup' and diluted it 1:1 with 1ml of Pure VG. Then dripped that in my Beserker RDA for a test. I would say the flavor is really very good. It actually compares very well with a PG extraction of the same feedstock. So I consider all this to be real progress and maybe this is a way out of the water contamination issues.

So my next test in this ongoing series of experiments is to extract this same feedstock again (C&D Dark Fired Kentucky) without the parallel EA, but Utra-Sonic 30g/150ml Distilled Water @ 160F for 10hrs, then spin that down, then evap and re-con as per above technique. The 64 dollar question is to find out the quality of the flavor profile using that preparation. As far as mitigating bacterial issues, if the sample is held at 160F and then we rapidly move to a spin down and evap, there should be no chance for bad things to happen.

FYI this Water Extract was a combined parallel EA extraction, with an intermediate freeze separation stage. See page 6 of this thread and scroll down a couple of posts to see how this was prepared: http://diy-tobacco-net.epizy.com/viewto ... 9&start=50

[CAAB]

That sounds very promising. I am surprised to hear that the flavor is comparable to PG extraction.

I'm still on the fence myself with my existing H2O extractions because they were outside the food safety window longer than 4 hours. So I am pretty sure I can kill anything living in there and remove the potential for it to grow again, but I wonder about any undesirable toxins left behind.

I think with the H2O method, you are on the right track. The full evaporation is an important step.