Tobacco extraction using heated Ethanol

[Str8vision]

I noticed that the evaporation really slowed down after the first hour. I've eliminated 64% of the PGA so far with the fan at room temp but now the extract is full of solid looking particles that weren't there after the initial 75% reduction. I'm going to have to do another filtering at the end of this step.

Likely the ethanol had extracted, absorbed and held in solution a substance from the tobacco that isn't easily or completely soluble in PG. I don't normally transfer flavor from ethanol to PG so can't really help you very much, I leave my reduced extracts ethanol based. I wouldn't be in a big hurry to filter those particles out, they might actually be flavor. Just thinking out loud but once you've finished evaporating the ethanol off you might try warming the PG to around 120F and attempt to mix those particles in.

 

[Str8vision]

Those particles will dissolve once you shake the liquid. They are not to be discarded. They usually appear when you are nearing the limits of the evaporation process. I am not too enthusiastic about filtering a reduce solution since you invariably will lose some of the flavor molecules. But if Stra8 has done it successfully, there might be no harm in doing it.

I only filter reduced ethanol extracts, I've not filtered an extract after transferring the flavor into PG and driving off the ethanol. I'm afraid the solid particles kbriggs is seeing might actually be flavor carriers, if so filtering might be a bad idea but I don't really know. I rarely transfer flavor from ethanol to PG but when I have I don't remember seeing solid particles floating around so I'm at a loss. Could just be my poor eyesight or failing memory, advancing age diminishes both and if there's one thing I have way too much of, it's age...

 

[usr/]

I've only done about 7 pga extractions and during the process of reducing, ran into this coagulation a couple times. Just guessing but not sure, would this be the early stages of the extract becoming a concrete/absolute?

 

[Str8vision]

Hi all, i have been following this thread for about two weeks and have finally decided to join this community. Many thanks to the original poster Str8vision . I have tried your method and am getting pretty exciting results. Btw, when steeping the extract, is it enough to just let the extract itself sit, or should we mix it into PG/juice mix and then let it sit?

Some extracts require aging before their full flavor develops while others taste better freshly mixed, it really depends on the tobacco in play. As a general rule aging is beneficial and improves flavor. Extract itself will improve with age as will a mixed NET juice. When you first start extracting flavor from tobacco you'll likely mix most of your extracts into NETs and use them aged or not. As you develop a stockpile of well "aged" NETs, you'll have the luxury of being able to "wait" for optimum flavor. I have that luxury and so first age the extracts themselves. I then mix NETs using those aged extracts and allow the mixed NET to age before using it. The exception to this is heavily flavored pipe tobaccos (like Sutliff's "Molto Dolce"), they're often better freshly mixed. Truth is there is no right or wrong way to do it, if it tastes good, it's ready.

 

[kbriggs]

but it you touch the particles with a fork, or a glass bar, you should see them come apart.

They are just sticking to the fork and to the side of the jar. I put the lid on and shook the crap out of it but they didn't dissolve. I'm going to heat and shake one more time before filtering.

And BTW, since you are measuring by weight, an 80% reduction in weight does not necessarily translate into volume. Specific gravity of alcohol is less than other ingredients in your solution.

Yes, understood. I've been doing everything by weight, including calculating how much reduction has taken place. I left the fan on it overnight and eliminated 78% of the PGA by weight. I'll probably stop there. This is likely the first and last time I attempt to do a PGA to PG replacement. It's too much hassle with too little benefit. The test I did after the initial PGA reduction was perfectly fine, I didn't taste any alcohol. But I was curious to see how this would work. Now I know.

 

[kbriggs]

Likely the ethanol had extracted, absorbed and held in solution a substance from the tobacco that isn't easily or completely soluble in PG.

Here's what I'm seeing:

None of that was visible prior to the PGA to PG replacement stage.

 

[Str8vision]

When we extract flavor from tobacco using ethanol (or any other solvent) it leeches not only flavor but oils, waxes, resins, plant matter and other compounds. Many of these compounds are dissolved and absorbed in the ethanol some are not. The solubility of certain compounds and ethanol's ability to hold them in solution can be altered by temperature, "freeze filtering" reduces ethanol's ability to hold certain compounds in solution, in sub-zero temperatures -many- compounds will precipitate out of solution and settle to the bottom of the container. Freeze filtering simply removes excess compounds, but not all of them. When we reduce an ethanol extract we concentrate not only flavor but all other compounds that were still locked up in solution. The ethanol will evaporate but these other compounds do not and are left behind in the reduced extract. Once the remaining ethanol is saturated it simply can't hold any more and excess amounts of these compounds fall out of solution. Over time (~five days after reduction) these excess oils, waxes and resin will have coalesced together and are visible. Filtration removes "suspended" particles at and above the filter's retention rating but not dissolved and absorbed compounds. These dissolved compounds are what makes NET "gunky". This is why even though our cleaner ethanol based NETs out perform those extracted using PG/VG as the solvent, they're still harder on wicks and coils than a synthetic juice. It's not just tobacco, any naturally extracted organic flavoring will be problematic for the same reason.

 

[Str8vision]

Here's what I'm seeing:

None of that was visible prior to the PGA to PG replacement stage.

The scum toward the top of the container looks like the oil/wax that will develop after reducing an ethanol extract and letting it sit for five days undisturbed. It'll coat the sides of the container just like that. Those large chunks towards the bottom of your container, I have no idea, haven't seen that before. I'd follow Exchaner's advise and try to mix it in, it could be flavor.

 

[kbriggs]

I'd follow Exchaner's advise and try to mix it in, it could be flavor.

I already started (yet another) 2.5 micron filtering so it's too late for that. But I still have the 7% PGA mix from yesterday to compare it against so I'll know pretty soon how this affects the flavor.

 

[kbriggs]

But I still have the 7% PGA mix from yesterday to compare it against so I'll know pretty soon how this affects the flavor.

So I mixed this final result at 9% (to compensate for not getting all the PGA out) and compared it to the 7% PGA mix yesterday and they taste pretty much the same. If there's any flavor loss from that last filter, it's probably minor.

 

[Str8vision]

I've got multiple extractions in the works. The first batch involves four different pipe tobaccos and the amount of ethanol I used for these extractions has increased. I used enough to just cover the tobacco then added 25% more (rather than the normal 10 - 15%). I processed these for 100 hours at 125F and am now allowing them to soak at room temperature for 30 days. Each day I turn the containers upside-down and then back up-right several times to circulate the solvent and tobacco inside. After 30 days I'll separate the solvent from tobacco, freeze filter the extracts, reduce them by 80% and allow the reduced extracts to set undisturbed for a week before final filtering at 1 micron.

The second batch I'm (currently) extracting involves one cigar and one pipe tobacco. For these I've used -a lot- of ethanol, enough to just cover the tobacco and then added about 60% more. I plan to process these for 12 hours at between 175 and 190F allowing the ethanol to lightly boil or "simmer". I've made sure the lids on the canning jars are loose enough to allow excess pressure to vent, just like when canning food. Six hours into these extractions I've lost around 30% of the solvent from each container and expect to lose upwards of 70% by the time 12 hours has rolled around. I plan to allow these extractions to rest at room temperature for one week (7 days) before separating the solvent from tobacco and freeze filtering them. The amount of reduction will depend on how much solvent remains after hot processing is complete, I believe I'll have accomplished some of the necessary reduction -beforehand- during the flavor extraction. This batch could easily flop due to the level of heat involved but I was ~curious~ what effects boiling ethanol might have on flavor. My first reportable observation is the PG contained in the pipe tobacco (as a humectant) has increased the ethanol's boiling point slightly above that of the cigar extraction. The cigar is still simmering nicely at 175F while the pipe tobacco has slowly dropped off to low simmer, about half the vigor of the cigar...

 

[Exchaner]

reduce them by 80% and allow the reduced extracts to set undisturbed for a week before final filtering at 1 micron.

I recall from a few posts back that you do not filter the extractions after reduction. Is this part of your experiment?

 

[kbriggs]

So after trying several heated PGA extractions, I've had mixed results so far. First up was with an old Cream Dominican cigar from a batch I had left over from my cigar smoking days. I did a 12-hour crock pot heat followed by a 2 day freeze with a 2.5 micron filtering. Reduced that by 75% using oven heat. Mixed that at 7% (with 28% PG, 65% VG). The initial shake and vape was pretty good as it tasted like a cigar. But then 1 week later the cigar taste was fading and an odd taste was surfacing. I was wondering if that was the alcohol. Then I just tried it again after another week and it's absolutely horrible, tastes like Windex or some industrial cleaner.

Immediately after making the first mix I took the rest of that extract and attempted a PG replacement of the PGA. I got 78% of it replaced and mixed it up at 9%. I'm getting similar results as above but it's taking longer to go bad. I also did a 5-day PGA extraction (same batch of cigars) with no heat. 10 days after mixing I feel it going the way of the others.

I've got some room temperature PG extractions going for those same cigars. The first one will turn 4 weeks old this coming Tuesday so I'll be filtering and mixing that for comparison. I have another batch that I'm going to process after 6 weeks.

Anyway, I also bought some pipe tobacco (Nightcap, Billy Budd, and Voodoo Queen) and did a 12 hour heated PGA extraction of those with a 48 hour freeze, filter, and 80% reduction using a small fan (took about 6 hours). That reduction caused all kinds of solid particles to appear even worse that what I showed earlier with the cigar. It really caked onto those jars, especially for the Nightcap which was difficult to clean. Much less for the Voodoo Queen. The Billy Budd was somewhere in between. Anyway, mixed those up at 5% and they were much stronger than the cigar batches. Nightcap had a dense smokey flavor. Voodoo Queen was milder with a slightly sweet taste and less smokey. Billy Budd was somewhere in between. After 2 weeks, they all taste about the same as before and Billy Budd is definitely my favorite among the three as it has more of a woody cigar taste than the others. I'm not (yet) getting any of that alcohol taste that ruined those cigar batches. I'm wonder if that's just because these are much stronger tobaccos and it's being masked. Time will tell. I also started room temperature PG extractions for these same tobaccos and will test them when they reach 4 weeks old.

 

[Exchaner]

But then 1 week later the cigar taste was fading and an odd taste was surfacing.

I wonder if that odd taste had anything to do with the type of tobacco. Sometimes Virginia type tobaccos develop a funky taste over time.

As to those particles that appear during reduction, they usually go away after a vigorous shake as discussed earlier. The sticky material clinging to glass is actually waxes/resins, oils and also some flavor. They are responsible for clogging your coils, and therefore best if they are discarded.

 

[kbriggs]

I wonder if that odd taste had anything to do with the type of tobacco.

Could be. I'll know better next week if the 4-week PG maceration comes out any better. And I also have PG maceration going of an ACID Blondie cigar to compare those against.

As to those particles that appear during reduction, they usually go away after a vigorous shake as discussed earlier.

On the first PGA/Cigar batch, I filtered those after the reduction and didn't see them again in the final bottle. But I did not filter the PGA/Pipe tobacco batches and those are sticking to the plastic bottles that I put the final extract in (which were shaken hard). Not seeing them in the actual ejuice mix, though.

 

[Str8vision]

I recall from a few posts back that you do not filter the extractions after reduction. Is this part of your experiment?

After reducing the extract I normally wait a few days for the oils to coalesce before performing the final filtering, that way the filter helps catch the tenaciously sticky oil.

 

[Str8vision]

But then 1 week later the cigar taste was fading and an odd taste was surfacing. I was wondering if that was the alcohol. Then I just tried it again after another week and it's absolutely horrible, tastes like Windex or some industrial cleaner.

I've not had that experience with PG or ethanol based extractions. At one time I thought my hot PG extractions were losing flavor after a few days but it turned out I was losing the ability to taste specific flavors after a few days of vaping them. One of the reasons I switch flavors (tobaccos) daily. The Acid Blondie cigar is a good example, after vaping it two days straight I lose the ability to taste the "Acid" flavor completely. If I alternate it every other day with a different tobacco everything's fine. Vanilla is one of my favorite secondary flavorings but I lose the ability to taste it after just a couple of hours...

 

[kbriggs]

So I filtered and tested my first 4-week ambient PG maceration today. This used a cigar from that same batch of old ones I mentioned earlier in my PGA extractions. And I'm getting that same bad taste, just milder. So obviously it's not coming from any alcohol since there was none here. These are just old dry cigars not well suited for extraction. I won't know until next month what a better cigar (ACID Blondie) should taste like when that batch becomes ready. I just ordered 6 whole leaf samples (0.25 lb each) from leafonly.com so I'll have plenty more material to work with soon.

 

[Str8vision]

The second batch I'm (currently) extracting involves one cigar and one pipe tobacco. For these I've used -a lot- of ethanol, enough to just cover the tobacco and then added about 60% more. I plan to process these for 12 hours at between 175 and 190F allowing the ethanol to lightly boil or "simmer". I've made sure the lids on the canning jars are loose enough to allow excess pressure to vent, just like when canning food. Six hours into these extractions I've lost around 30% of the solvent from each container and expect to lose upwards of 70% by the time 12 hours has rolled around. I plan to allow these extractions to rest at room temperature for one week (7 days) before separating the solvent from tobacco and freeze filtering them. The amount of reduction will depend on how much solvent remains after hot processing is complete, I believe I'll have accomplished some of the necessary reduction -beforehand- during the flavor extraction. This batch could easily flop due to the level of heat involved but I was ~curious~ what effects boiling ethanol might have on flavor. My first reportable observation is the PG contained in the pipe tobacco (as a humectant) has increased the ethanol's boiling point slightly above that of the cigar extraction. The cigar is still simmering nicely at 175F while the pipe tobacco has slowly dropped off to low simmer, about half the vigor of the cigar...

This experiment proved very difficult to control and required considerable attention. The temperature controller I use did its job perfectly but as these two extractions simmered the boiling point of ethanol constantly changed in one of them (the pipe tobacco). I boiled off 80% of the ethanol 10 hours into the process so halted the extraction at that point. The Nightcap turned out quite good -very robust- although the Latakia flavor component seems more pronounced than usual which isn't desirable for my taste. Unfortunately the Acid Blondie cigar lost its "acid" flavor, I believe the high process temperature "cooked" it off. I don't see great promise in highly elevated extraction temperatures when using ethanol as the solvent, a PITA to process/control and as we've discussed before higher temperatures can indeed harm and or alter flavor.

Thanks to a question asked by Kbriggs in a different thread I've started another experiment. Two pipe tobaccos (Voodoo Queen and Billy Bud) will be extracted at room temperature for 30+ days. It's been a year or two since I played around with room temperature extractions using ethanol as the solvent and if memory serves me correctly 10 days was the longest cold soak I was able to perform due to the excessive gunk ethanol would pull from the tobacco. Extractions processed beyond 10 days developed a murky plant like chlorophyll taste and were hard on wicks and coils. I wasn't able to achieve the full range or depth of flavor I desired from a 10 day room temperature ethanol soak -but- that was back before the advent of "freeze filtering". I'd be interested to see what kind of flavor a 30+ day room temperature ethanol extraction can yield and I'll be depending on freeze filtering to remove the undesirables elements that'll be leeched from the tobacco during the process. I'll start pulling in-process samples at the 30 day mark and at 2 week intervals thereafter.

 

[Aurora Indica]

Hi guys. Great to see this thread growing and still active. Since last I posted, i have produced around 3 litres of ethanol extract from my pipe tobacco collection. I was wondering, at around 6-10% ethanol extract for flavour, whats your preferred PG/VG ratio ?

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