Vacuum dehydration of VG extracts

[Str8vision]

I use blended solvents when extracting flavor from tobacco and vanilla beans, cloves and etc. A recent addition to my extraction methodology, I use a small portion of purified water in all solvent blends to enhance and expedite flavor extraction. Once the extraction and filtering process is complete, the benefits of water cease and as a statistically significant ingredient in an extract it isn't advantageous for "stable" long term storage. Just my personal opinion but for long term storage of extract I want only PG and or VG as a base.

In the past I have used low heat and open air evaporation to remove free water and PGA from extracts prior to storage. This method isn't ideal and isn't able to remove dissolved water (water absorbed at the molecular level), just the free water that exists above the saturation point of the solvents in play. VG is hygroscopic with a relatively high saturation point and readily absorbs water, this dissolved water is - very - difficult to remove.

I am familiar with several methods capable of removing dissolved water from oils but only have the equipment and capability of performing one of those methods, vacuum dehydration. Once the extraction and filtering processes are complete I will warm the extract to 160F (71C), and subject it to a high vacuum while being magnetically stirred. Stirring isn't really necessary for such a small quantity but should help. Most of the dissolved water should boil off and exit through the vacuum circuit. In "theory" anyway.....

As an amusing side note, I "inadvertently" boiled the PGA in a blended PGA/PG extract last September while vacuum filtering it. This occurred at room temperature with only a moderate (~20"), vacuum. The PGA boiled vigorously.

 

[Bagazo]

From what I have seen both VG and PG, particularly PG, are antibacterial and antifungal, so I'm not sure why you think small amounts of water, in mostly pg and/or vg mixtures, is going to be detrimental to long term storage.

Then again, you can't put a price on peace of mind and, if vacuum distillation (I think that is the proper term) gives you that, then more power to you.

 

[dodari]

I use blended solvents when extracting flavor from tobacco and vanilla beans, cloves and etc. A recent addition to my extraction methodology, I use a small portion of purified water in all solvent blends to enhance and expedite flavor extraction. Once the extraction and filtering process is complete, the benefits of water cease and as a statistically significant ingredient in an extract it isn't advantageous for "stable" long term storage. Just my personal opinion but for long term storage of extract I want only PG and or VG as a base.

In the past I have used low heat and open air evaporation to remove free water and PGA from extracts prior to storage. This method isn't ideal and isn't able to remove dissolved water (water absorbed at the molecular level), just the free water that exists above the saturation point of the solvents in play. VG is hygroscopic with a relatively high saturation point and readily absorbs water, this dissolved water is - very - difficult to remove.

I am familiar with several methods capable of removing dissolved water from oils but only have the equipment and capability of performing one of those methods, vacuum dehydration. Once the extraction and filtering processes are complete I will warm the extract to 160F (71C), and subject it to a high vacuum while being magnetically stirred. Stirring isn't really necessary for such a small quantity but should help. Most of the dissolved water should boil off and exit through the vacuum circuit. In "theory" anyway.....

As an amusing side note, I "inadvertently" boiled the PGA in a blended PGA/PG extract last September while vacuum filtering it. This occurred at room temperature with only a moderate (~20"), vacuum. The PGA boiled vigorously.

Hi,

What are you using for a vacuum source? Just wondering, I want to do something like what you mention but can't affford a fancy electric vac. pump right now. Retirement has its definite limitations.

Thanks

 

[asmcriminal]

I use blended solvents when extracting flavor from tobacco and vanilla beans, cloves and etc. A recent addition to my extraction methodology, I use a small portion of purified water in all solvent blends to enhance and expedite flavor extraction. Once the extraction and filtering process is complete, the benefits of water cease and as a statistically significant ingredient in an extract it isn't advantageous for "stable" long term storage. Just my personal opinion but for long term storage of extract I want only PG and or VG as a base.

In the past I have used low heat and open air evaporation to remove free water and PGA from extracts prior to storage. This method isn't ideal and isn't able to remove dissolved water (water absorbed at the molecular level), just the free water that exists above the saturation point of the solvents in play. VG is hygroscopic with a relatively high saturation point and readily absorbs water, this dissolved water is - very - difficult to remove.

I am familiar with several methods capable of removing dissolved water from oils but only have the equipment and capability of performing one of those methods, vacuum dehydration. Once the extraction and filtering processes are complete I will warm the extract to 160F (71C), and subject it to a high vacuum while being magnetically stirred. Stirring isn't really necessary for such a small quantity but should help. Most of the dissolved water should boil off and exit through the vacuum circuit. In "theory" anyway.....

As an amusing side note, I "inadvertently" boiled the PGA in a blended PGA/PG extract last September while vacuum filtering it. This occurred at room temperature with only a moderate (~20"), vacuum. The PGA boiled vigorously.

If you're using a vacuum pump, you need a chemistry kit... You need to do a distillation, but... i highly doubt you're using the amount of water required to have any significant difference. I doubt it would even distill. It will just vaporize up the distillation shaft and not come over. You also need to know the temperature you're distilling at, you don't want to biol off PG. The easiest way to get rid of the water is just, boil it off in a open container. Put your solution in to a container and your heating source, have stiring (or stir manually). Use a therometer, get the thing up to about 110-120 degree's C. Water boils at 100 degree's C. and let it boil till it stops boiling. Once it stops boiling all the water is gone.

 

[asmcriminal]

The cheapest way is to use an aspirator.



It works like this.




The middle piece is the asperator, You can get the water source from an aquarium fish pump. Put it in a bucket, and let the aspirator point in to the bucket. So the water goes back in to the bucket. The water will just cycle. The side arm of the aspirator is where you connect a hose for a vacuum. You can also attach the asperator to a hose or faucet. It will just end up wasting water. In chemistry, we use a sink. Our lab faucets have asperators attached, so the water just gets wasted. At home, I use the bucket method.

 

[Str8vision]

The filtered extract used for this endeavor was 112ml of 70/30 VG/water. While VG is bacteriostatic it's not bactericidal
in that it doesn't harm bacteria, just stops it from reproducing. Water on the other hand readily supports the growth of
bacteria, mold and other microbial undesirables. I'm not sure at what point of dilution the bacteriostatic properties of VG
would be compromised so for my peace of mind when it comes to long term room temperature storage of extracts,
reducing water content below 10% just seems prudent and was my goal. As VG and PG are both hygroscopic (readily
absorbing water directly from the air), I store extracts in airtight containers to insure water content remains at
acceptable/stable levels.

Fractional distillation is what made me consider this approach and when conducted in a vacuum it is considered
vacuum distillation. Vacuum dehydration differs from vacuum distillation mainly in that the extracted water vapor is
not condensed back into a liquid (distillate), separated or collected but is instead dispersed directly into the ambient
atmosphere while still a gas. Same principle used in the industrial vacuum dehydration units used for oil purification.
Lowering the atmospheric pressure lowers the boiling point of water to temperatures that will not damage or degrade
the flavor contained in the solvent.

My vacuum source for this experiment was an old air (pneumatic), powered vacuum pump driven by compressed air. I
didn't use my electric HVAC pump because the extracted water vapor would be flowing directly through the pump
before being discharged into the ambient air. The 12vdc pump I use for filtering doesn't provide a high enough
vacuum, tops out at around 20". A Faucet Aspirator Vacuum Pump might be ideal for this process, I may opt to get one
for future use.

The first problem encountered was my heated magnetic stirrer wouldn't keep the temperature of the
extract above 130F. I performed this operation in my shop building where the air compressor is located, it's not
heated and was a cool 38F. I improvised by using an electric hot plate and pan of water, placing the pint canning jar I
use for a vacuum chamber in the pan of hot water. Once up to temperature I applied vacuum. At ~26" of vacuum I
began opening and closing the needle valve I use to introduce/cycle fresh air into the chamber. The extract never
"boiled" but a light caramel colored foam developed on the surface of the extract with small bubbles appearing while
others popped. I would occasionally swirl the extract to "stir" it. After about 30 minutes I was finished, the amount of
clear liquid around the discharge port of the vacuum pump was surprising, a small puddle. The aroma of tobacco filled
the entire shop, brought back fond memories. Ended up with 81ml of extract so the process removed about 31ml of
water, not all of it but better than I expected. It was a lot of fun, I enjoy tinkering around with extracts. Will report
back on this extract's flavor after it has aged a bit.

Extracting flavor from tobacco - doesn't require - vacuum pumps, other expensive equipment or complex procedures.
Simply soaking tobacco in PG, VG or PGA and gravity filtering it provides a wonderfully satisfying extract that is full of
flavor. There are threads in this sub-forum detailing procedures for both hot and cold extraction methods. I choose to experiment
with various solvents, methods and levels of filtration simply because I enjoy doing so and am always
seeking perfection/improvement, it has become a fun hobby.

 

[Dave_in_OK]

Str8vision did you see the post "iSi nitrous whipper for flavor infusions"

Do you think that would be a good way to extract?

 

[Str8vision]

Str8vision did you see the post "iSi nitrous whipper for flavor infusions"

Do you think that would be a good way to extract?

First of all I'd like to say that using Nitrous oxide is no laughing matter........

Actually, I'm a bit skeptical about the effectiveness of using N2O to infuse flavor from leaf tobacco into a solvent but who knows? Looks like a interesting experiment to me...... Somewhat reminiscent of the supercritical CO2 process I witnessed, minus the heat and extreme pressure (4600psi). Food or medical grade N2O is non-toxic and if I remember correctly readily mixes with alcohol and oil. If a single infusion pass was insufficient, perhaps several passes would work?

 

[asmcriminal]

Str8vision did you see the post "iSi nitrous whipper for flavor infusions"

Do you think that would be a good way to extract?

I am not sure if that was just directed to Str8vision or to everyone. My take on it, it makes no sense. You put NO2 in to the container to pressurize it. When you add pressure to a system, the molecules in the container "SQUEEZE" tighter together. This is how diamonds are made synthetically, putting carbon under high pressures. The claim in the comment of the video says, "When the gas is suddenly released from the siphon, the sudden pressure drop causes gas to come out of solution in the liquid and solids as bubbles. As these bubbles rapidly swell in size they rupture the microstructure of the solid ingredients, releasing aromatic molecules into the surrounding liquid. The result is a remarkably flavorful infusion in mere minutes."

When you release the pressure it will "SHRINK" not swell.(As these bubbles rapidly swell in size.) If you want the molecules to "swell" you need a vacuum, the opposite of pressure. I am sure we all seen marshmallows under vacuum.

On second thought, i re watched it, did more research on it. At best this thing is just a mixer. It pushes the NO2 gas in to the liquid. It takes up space, once the NO2 is released. It creates space for a fraction of a second. Once the space is removed, the molecules crash together making a mixture.

I still believe your best bet is low heat with stiring to mix things.

 

[Dave_in_OK]

First I welcome all input! I'm looking at this as a possible way to force the solvent into and out of the tobacco giving us the best flavor the tobacco can. Now today is the first day I've even considered this process but If I can get my hands on the equipment I'm willing to give it a try. When I saw that I thought of the difference between a drip coffee pot and an espresso machine. just my

 

[asmcriminal]

The problem with heat is that if it gets to hot it can destroy the molecule if it's too hot. Ethanol has a lower boiling point than water. at 78 degree's C. This is your best bet to maximize the concentration. You can use lower boiling piont solvents, but... I wouldn't recommend them, only to an experienced chemist. If you're dead serious about extraction with ethanol. your best bet is a soxhlet extraction. It will pull out every bit of the tobacco flavoring and concentrate it. Here is what it looks like. The actual start of the extraction is at 1:20seconds. He's extracting oil from peppers.





People also use those to extract oils from all types of things. If i was doing something like what you want to do without any real equipment. I'd get some ethanol(alcohol) not EVERCLEAR, it contains water. You can buy alcohol online, it might be expensive. Get yourself a thermometer. I'd grind up the leaves, use a small container, maybe a 1 cup pyrex measuring cup. Put some ground up leaves in the cup, maybe about 1/4 of and add alcohol to about 1/2 cup. try to get the temperature to about 40 degree's C. and work with that. How long to heat it? I have no idea. I have done organic matter and it takes about 3-4hrs.

If you want, you can raise the temperature, to the boiling point of ethanol, and it will just evaporate off. Once all the ethanol is gone, you have pure tobacco oil. But this is a waste of ethanol obviously. There is equipment that can collect it. Ideally, I'd use a vacuum distillation. Looks like this.


Just to be clear, I never extracted oil from tobacco leaves, I am a chemist, I have done other types of extractions.