Tobacco extraction using heated Ethanol

[Str8vision]

That is the way I've been doing it lately with my heated PGA extractions. It made more sense to me do the reduction first since that leaves all kinds of gunk behind, sticking to the sides of the jar. I then run that through the coffee filter, freeze it for 48 hours, and then do a 2.5 micron filter inside the freezer.

Good to hear someone's already done it and isn't reporting diminished flavor. I was concerned that in addition to a higher percentage of "gunk" that the flavor might also be reduced. With 70% of the ethanol evaporated off the remaining ethanol should be seriously over saturated. When exposed to extreme cold temperatures further reducing the ethanol's ability to hold dissolved compounds in solution I wasn't exactly sure what might precipitate out. If it doesn't negatively impact flavor then (in theory) freeze filtering -after- reduction should yield a significantly cleaner extract and NET. However, losses to filtration should be higher since what you're losing is 4X concentrated.

On one of my early extractions I tried an experiment. I first did a 48 hour freeze filter (in the freezer 2um filter), and put the extract back in the freezer for another 48 hours and filtered again. Yep more gunk. I then did a third freeze filter that came out pretty clean. This can vary depending on the tobacco, but my conclusion is that 48 hours in the freezer is not long enough to get full fallout. I would guess that for the larger volumes you are working with even more time may be required.

I think the effectiveness of freeze filtering depends on a balance of two factors, time and temperature. When I used my household freezer (because it's handy) I found it required 72 hours to effectively clean a partially full half pint jar of extract. After my better half convinced me to stop using her household refrigerator/freezer for such nefarious purposes, I switched to using the industrial deep freeze out in my shop (-10F). The industrial freezer is significantly colder than my household freezer and I found it required just 36 hours to obtain the same results but again that was on a partially full half pint jar of extract which has been my normal batch size for the past few years. Being my first quart sized extractions I may have falsely assumed that larger quantities would need only a little extra time to reach the desired temperature and purge themselves of their ill gotten cargo. I won't really know even after I freeze filter the concentrated extract because I expect it to yield additional gunk simply because the remaining ethanol will be over saturated after being reduced by 70%.

Anybody ever tryed a hookah tobacco?
I am currently working on an extract of Al fakher Shisha apple flavored tobacco for a friend.
When I opened the box the tobacco was a gooey mess. My understanding is that the tobacco is soaked in molasses. Freeze filtering took over 14 hours.
I have a strong feeling this is going to be a coil killer. I am still in the reduction faze, and the extract smells very potent, so hopefully a low percentage mix will help offset the gunkyness.

Never have but am curious about the results you obtain, keep us in the loop. 14 hours? How much extract were you freeze filtering? With that much sugar involved (molasses) it'll be interesting to see how gunky the NET is but also how well the secondary flavorings present themselves in vape form.

 

[Boxster]

Good to hear someone's already done it and isn't reporting diminished flavor. I was concerned that in addition to a higher percentage of "gunk" that the flavor might also be reduced. With 70% of the ethanol evaporated off the remaining ethanol should be seriously over saturated. When exposed to extreme cold temperatures further reducing the ethanol's ability to hold dissolved compounds in solution I wasn't exactly sure what might precipitate out. If it doesn't negatively impact flavor then (in theory) freeze filtering -after- reduction should yield a significantly cleaner extract and NET. However, losses to filtration should be higher since what you're losing is 4X concentrated.




I think the effectiveness of freeze filtering depends on a balance of two factors, time and temperature. When I used my household freezer (because it's handy) I found it required 72 hours to effectively clean a partially full half pint jar of extract. After my better half convinced me to stop using her household refrigerator/freezer for such nefarious purposes, I switched to using the industrial deep freeze out in my shop (-10F). The industrial freezer is significantly colder than my household freezer and I found it required just 36 hours to obtain the same results but again that was on a partially full half pint jar of extract which has been my normal batch size for the past few years. Being my first quart sized extractions I may have falsely assumed that larger quantities would need only a little extra time to reach the desired temperature and purge themselves of their ill gotten cargo. I won't really know even after I freeze filter the concentrated extract because I expect it to yield additional gunk simply because the remaining ethanol will be over saturated after being reduced by 70%.



Never have but am curious about the results you obtain, keep us in the loop. 14 hours? How much extract were you freeze filtering? With that much sugar involved (molasses) it'll be interesting to see how gunky the NET is but also how well the secondary flavorings present themselves in vape form.

My freezer's lowest temperature is -5F so I guess that could be a factor.

yes, 14 hours to filter ~6 oz of extract.
In hindsight, I should have only filtered 3oz at a time, because the filter clogged up pretty fast and the cold extract was very thick.

 

[kbriggs]

Good to hear someone's already done it and isn't reporting diminished flavor.

I can't say that for sure because I haven't done an A/B test. What I need to do is split a batch into two jars, heat them together and put one through freeze filtering first and the other through reduction first.

I've had some other issues with flavor that you may be able to help me with. I've had several batches that have given me an off-putting chemical taste. Hard to describe exactly but it's almost like someone added window cleaner to it. I was wondering if I was tasting the PGA but other batches with the same amount of reduction (70 to 80%) and mix ratio (7%) have been fine. For example, my first batch of Billy Budd came out great right after shake and vape. But the second batch (months later) had the chemical taste and it lasted for weeks. I just now tested it again after 6 weeks and I think that chemical taste is pretty much gone but it's not as flavorful as I remember that first batch to be (I've since vaped all of that first batch so I can't do a direct comparison).

I'm wondering if I "cooked" some of these at too high a temperature and messed up the flavor, is that possible? I have the cheapest model CrockPot and typically I leave the lid on crooked on the lowest "warm" setting to bring the temp down. I use a temperature gun to check on it and it would fluctuate up near 165. Not sure how accurate a reading that was giving me, though, because it varied depending on where I aimed it. But one night I started the 12-hour heat cycle and left the lid on tight and when I got up in the morning every bit of that PGA had boiled right out of those jelly jars. Those two-piece jar lids were on fairly snug, too. Since then I bought one of those inline dimmer switches and calibrated it so it stays under 160 with the lid fully on. The two batches I made since then (Louisiana Red and Brown Irish X) came out fine with no chemical taste.

 

[Str8vision]

I've not really noticed a chemical taste from any tobacco extraction even those intentionally over or under cooked. Like you I doubt alcohol is the culprit, otherwise all of your extracts would taste off. However, alcohol does impart a flavor even at just 7%. Normally, once I've mixed a NET I let it to sit open air in a canning jar for a few days allowing most of the alcohol to evaporate off before bottling and aging it further. I cover/tent the jar with a coffee filter held in place by a rubber band, this keeps dust and other possible contaminants out. I don't do this because of any perceived flavor alcohol may impart (tastes fine to me), but because the alcohol content might cause the flavor to age differently especially over very long periods of time (years).

I have noted a difference in flavor intensity from one batch to another using the same tobacco blend even when a temperature controller was used for each of the extractions. Experienced the same phenomenon back when I used hot PG/VG as the extraction solvent. Billy bud was the first blend I noticed such a problem with, Drew Estates Acid Blondie is a more recent one. The Blondie produced inconsistent results, one extraction was perfect the next tasted like perfume. The temperature of my hot water bath is electronically controlled to within 2 degrees of the target temperature so I don't think it's related to fluctuating temperature but it could possibly be due to elevated temperatures in general. I know for a fact that too much heat can ruin an extract, I've done it. On the other hand none of my long term room temperature extractions have ever suffered such a problem, all have turned out very consistent. Even so most of my extractions are heat assisted mainly for expediency, especially when sampling new tobaccos. For extracting tobaccos I know I like I prefer an extended room temperature soak, no heat at all. That's why I'm currently experimenting with long term room temperature ethanol soaks, works best for PG/VG based extractions so I don't see why it wouldn't for ethanol based.

Another problem is that many people lose the ability to taste certain flavors after indulging in them, their taste buds become somewhat desensitized. Vanilla is -my- Achilles heal but several other flavors fade after I've vaped them for awhile, the creamy cigar note in Billy Bud is one of them. Latakia is another, it starts out extremely smoky and dark but after a day or two subsides considerably. The flavor is still there but my ability to taste it has subsided. This is why I extract and mix so many distinctly different flavors of tobacco, variety and daily rotation is the only cure that works for me.

 

[kbriggs]

On the other hand none of my long term room temperature extractions have ever suffered such a problem, all have turned out very consistent. Even so most of my extractions are heat assisted mainly for expediency, especially when sampling new tobaccos. For extracting tobaccos I know I like I prefer an extended room temperature soak, no heat at all.

I initially tried some 30-day room temperature PG extractions (including an ACID Blondie cigar) and they all came out terrible. But now I'm trying a couple of 90-day room temp PGA extractions with Billy Budd and Mississippi Mud, (from the same batches that gave me a chemical taste via heated PGA extraction). The first of those won't be ready until late January so I won't know until then.

 

[Str8vision]

I initially tried some 30-day room temperature PG extractions (including an ACID Blondie cigar) and they all came out terrible. But now I'm trying a couple of 90-day room temp PGA extractions with Billy Budd and Mississippi Mud, (from the same batches that gave me a chemical taste via heated PGA extraction). The first of those won't be ready until late January so I won't know until then.

Yes, 30 days for a cold soak just isn't enough time and that's my opinion no matter what solvent is used. My initial impression of room temp ethanol soaks is they require even more time than does PG/VG based extractions. My Voodoo Queen wasn't quite ready at the 90 day mark but the Billy Bud tasted great. Doesn't surprise me because Voodoo Queen (like most VaPers and Virginia heavy tobaccos) is a bit more difficult to extract and NET made with it requires aging before reaching full maturity. It will be interesting to see if your Billy Bud and Mississippi Mud turn out OK considering the heat assisted extractions of the same tobaccos tasted off. Both blends are made by Cornell & Diehl, their tobaccos do have a unique signature casing note.

 

[Str8vision]

A ~70% reduction of the five extracts is complete. 60ml of the reduced (concentrated) Acid Opulence extract has been returned to the freezer to see what benefits (if any) freeze filtering a concentrated extract might offer. If there are no negative impacts associated with freezing a concentrated extract I have other ideas in mind. The remaining extracts will sit at room temperature undisturbed for two weeks allowing time for the oils to coalesce before running them through a 1 micron glass filter. I intend to keep 30mls from each of these extracts out for use but the rest will be bottled in glass containers and stored in the freezer next to my liquid nic. This is my first experiment with long term cold storage of tobacco extracts, I'm hoping the extreme cold temperature slows oxidation to a crawl like it does for liquid nic.

Here's a question for the group; Should I leave the extracts ethanol based or should I transfer the flavor over to a PG or VG base for long term cold storage? I'm concerned ethanol might be too reactive even at -10F and end up being a poor base for long term storage. What are your thoughts?

This is the final leg in my journey, if cold storage proves successful I can extract large quantities of my favorite tobaccos and store the reduced extracts long term simply pulling a 30ml bottle from the freezer as needed.

 

[happy valley]

Here's a question for the group; Should I leave the extracts ethanol based or should I transfer the flavor over to a PG or VG base for long term cold storage? I'm concerned ethanol might be too reactive even at -10F and end up being a poor base for long term storage. What are your thoughts?

I'll have a go but answer with a question: are not the flavorants we commonly purchase from suppliers PG based?

This is the final leg in my journey.........................

Hmmm, sure about that? Methinks an active and inquisitive mind will always have nuance and refinements to explore.

 

[gt_1955]

...

Here's a question for the group; Should I leave the extracts ethanol based or should I transfer the flavor over to a PG or VG base for long term cold storage? I'm concerned ethanol might be too reactive even at -10F and end up being a poor base for long term storage. What are your thoughts?

This is the final leg in my journey, if cold storage proves successful I can extract large quantities of my favorite tobaccos and store the reduced extracts long term simply pulling a 30ml bottle from the freezer as needed.

My thoughts, and this is from gut feel with no scientific reasoning, are to transfer to VG or even PG for loooong term cold storage (VG, because it stores better according to Kurt).

 

[gt_1955]

As an afterthought (and because I was mixing a hybrid juice [steeped tobacco + concentrates]), I feel the double cold filtering as explained by Str8vision above will be about the best we can achieve at home.

 

[Str8vision]

As an afterthought (and because I was mixing a hybrid juice [steeped tobacco + concentrates]), I feel the double cold filtering as explained by Str8vision above will be about the best we can achieve at home.

I've tried many different solvents and methods but in all honesty when it comes to NETs I believe a "winterized" ethanol based extract is as good as it's going to get for flavor and enhanced performance. I may push the industrial freezer down to -30F to see if that further improves the effectiveness of the freeze filtering process but that's just another tweak, nothing new.

 

[aceswired]

As an afterthought (and because I was mixing a hybrid juice [steeped tobacco + concentrates]), I feel the double cold filtering as explained by Str8vision above will be about the best we can achieve at home.

I still feel like distillation would be the ultimate, if we could do it in a way that the flavor is carried. Would be clean and concentrated, with careful fractionalization. Maybe that's not realistic at the hobby level though.

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[Str8vision]

I still feel like distillation would be the ultimate, if we could do it in a way that the flavor is carried. Would be clean and concentrated, with careful fractionalization. Maybe that's not realistic at the hobby level though.

Did you ever try any of the old "aromatics" line of NETs Ahlusion used to sell (2012 - 2013) like Blue grass Burley, Devil Dog etc.? They quit selling NETs a few years back but the old aromatics were made from steam distilled tobacco extracts and were cleaner than PG based soaks. For a few hundred dollars investment steam distillation is within the realm/possibility of DIY. Steam distillation produces an essential oil but I have no idea if it needs to be purified, refined, treated or filtered before use.

If you've ever tried HHV's NETs they're made from essential oils extracted with Supercritical CO2. Cleanest NETs I've found. Unfortunately, I don't think Supercritical CO2 extraction is within the DIY realm. As with the essential oils from steam distillation I have no idea if they're purified, refined, treated or filtered before use but suspect they are.

 

[Boxster]

Did you ever try any of the old "aromatics" line of NETs Ahlusion used to sell (2012 - 2013) like Blue grass Burley, Devil Dog etc.? They quit selling NETs a few years back but the old aromatics were made from steam distilled tobacco extracts and were cleaner than PG based soaks. For a few hundred dollars investment steam distillation is within the realm/possibility of DIY. Steam distillation produces an essential oil but I have no idea if it needs to be purified, refined, treated or filtered before use.

If you've ever tried HHV's NETs they're made from essential oils extracted with Supercritical CO2. Cleanest NETs I've found. Unfortunately, I don't think Supercritical CO2 extraction is within the DIY realm. As with the essential oils from steam distillation I have no idea if they're purified, refined, treated or filtered before use but suspect they are.

For only $3200.00 you can get a table top supercritical fluid extractor (SFE)

Extractors - Ocolabs

 

[Boxster]

A ~70% reduction of the five extracts is complete. 60ml of the reduced (concentrated) Acid Opulence extract has been returned to the freezer to see what benefits (if any) freeze filtering a concentrated extract might offer. If there are no negative impacts associated with freezing a concentrated extract I have other ideas in mind. The remaining extracts will sit at room temperature undisturbed for two weeks allowing time for the oils to coalesce before running them through a 1 micron glass filter. I intend to keep 30mls from each of these extracts out for use but the rest will be bottled in glass containers and stored in the freezer next to my liquid nic. This is my first experiment with long term cold storage of tobacco extracts, I'm hoping the extreme cold temperature slows oxidation to a crawl like it does for liquid nic.

Here's a question for the group; Should I leave the extracts ethanol based or should I transfer the flavor over to a PG or VG base for long term cold storage? I'm concerned ethanol might be too reactive even at -10F and end up being a poor base for long term storage. What are your thoughts?

This is the final leg in my journey, if cold storage proves successful I can extract large quantities of my favorite tobaccos and store the reduced extracts long term simply pulling a 30ml bottle from the freezer as needed.

I've been storing my nets diluted in PG in amber glass bottles at cool room temperature for two years and have not noticed any degradation.
I have some HHV & Quicknic juices 60/40 in glass bottles in the fridge that are about 3 years old. I don't vape them very often because they are high nicotine juices. Fresh out of the fridge they taste like the day I bought them, in fact I usually have to let them steep a few days before vaping them.

 

[Str8vision]

For only $3200.00 you can get a table top supercritical fluid extractor (SFE)

Extractors - Ocolabs

A smart man would buy two at that price just so he'd have a spare on hand.

A couple of years ago I watched a video where a guy (in his garage) used a modified S.S. Scuba tank, a series of H.P. valves, H.P. flexible S.S. braided hoses, Large tank of CO2, flexible wrap-around heating pads and a PID temperature controller to achieve Supercritical extraction of flower petals. He'd fill the scuba tank with flower petals then hooked it up and applied full pressure from the large CO2 tank (~2800 psi). Then he closed the valves, disconnected the hoses and heated the CO2 filled Scuba tank to a certain temperature (seems like it was 150F or so). Once heated the CO2 pressure inside the tank was driven -considerably- higher (seems like it was 4600 psi) in order to reach the desired Supercritical extraction pressure. It worked and he ended up with what looked like ~5ml of essential oil from the flower petals at the end... Interesting but looked a bit dangerous to me.

 

[mongo74]

Being a sci-fi buff, I wouldn't be comfortable with something near my person that's super-criticle.

 

[gt_1955]

... Interesting but looked a bit dangerous to me.

Ha ha ha ... just a bit

 

[Str8vision]

A ~70% reduction of the five extracts is complete. 60ml of the reduced (concentrated) Acid Opulence extract has been returned to the freezer to see what benefits (if any) freeze filtering a concentrated extract might offer.

I set the freezer one notch colder and achieved -22F. I allowed the reduced/concentrated Opulence extract to sit at -22F for six days, not purposely, I was just busy with other things. While filtering it I noticed a clear gelatinous goo (approximately ~3ml worth) that after hundreds of extractions I've -never- encountered before. Also, stuck tight to the bottom of the container was a thin film of semi-clear waxy material much like paraffin, I'd say 1 to 2ml worth. Neither of these anomalies bore any resemblance to the runny tan/brown muck freeze filtering usually produces. I got very little (virtually none) of the muck I was actually expecting. The transparent gelatinous goo was trapped by the filter and discarded, the waxy film in the bottom of the jar required hot soapy water for removal. Very interesting indeed. After this round of freeze filtering I mixed 5ml of NET to sample and "shake-n-vape" it tasted perfect, couldn't perceive any loss of flavor. Nothing resembling oil dropped out of solution while in the freezer so I'll let the extract sit at room temperature for a week or two before the final 1 micron filtration. This experiment raises many interesting questions, certainly more than it answered.

One thing I've come to realize is that Ethanol is the solvent of choice for flavor extraction. Not only due to the range of flavor it extracts or the fact ethanol based extracts can be concentrated (or the flavor transferred), but also because of all the undesirable muck that freeze filtering successfully removes. Ethanol is the only non-toxic solvent that can be freeze filtered, with PG/VG based extracts all that muck ends up in the mixed NET to be vaped.

 

[aceswired]

Nights here are in the -20 and -30 this time of year. Supercold freezing would be pretty easy. ...

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