Tobacco extraction using heated Ethanol

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Str8vision

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I freeze filtered the reduced/concentrated extracts of Louisiana Red and Acid Blondie. Even though both had been freeze filtered before being reduced both still yielded a lot of wax and gunk. I tried to get a pic of the waxy film stuck to the bottom of the containers but the relative humidity here is currently 99% and the moment the -22F containers were exposed to the warm, moist ambient air they frosted over. I had to allow the frosted containers to warm before taking the pics but once warmed much of the solid waxy buildup had turned liquid. The liquid you see inside the container isn't extract, it's semi-transparent liquefied waxy muck. The red glaze stuck to the bottom of the container appears to be oil. From ~60ml of reduced L. Red I caught around ~3ml of gunk. I consider that significant.

DSCF0197.JPG


The Blondie filter (left) caught quite a bit of "normal" muck in addition to the waxy buildup that was stuck in the jar. The L. Red filter (right) caught very little muck beyond the waxy buildup that was stuck in the jar. Neither extract contained observable amounts of the unusual transparent gel I encountered when filtering the Acid Opulence extract last week. Bottom line; while it does cost more extract (due to being concentrated), freeze filtering extracts after they've been reduced removes far more undesirable gunk that would otherwise end up mixed in your NET.

DSCF0198.JPG


EDIT: For the past week I've been vaping the Acid Opulence that was "winterized" (after reduction) two weeks ago even though it hasn't been filtered through anything but a coffee filter. I'm seeing a 30% improvement in wick/coil performance even before final (1 micron) filtering has taken place. So far the performance gain appears to be quite "significant", I'm impressed. Next I'll evaluate its performance after 1 micron filtration to see what (if any) additional gains are achieved. So far not a trace of oil has coalesced from the extract which is rather surprising.
 
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kbriggs

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Forgive me if this has been mentioned but I'm wondering if anyone might suggest a good online source of 1 micron filter paper and what diameter you've found best?

Amazon has various sizes but the price seems to vary wildly depending on which listing you select. I bought some Ahlstrom brand there early in the year, 2.5 micron, 18.5 cm diameter, which is a good size for placing in wide-mouth jelly jars without needing a funnel underneath it.
 

gt_1955

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@Str8vision ... I wonder if there's any value in skipping the first freeze filtering phase and going straight to the reduction phase, then freeze filtering? We may not lose as much concentrate as filtering losses?

So Hot extract > Coffee filter > reduce > freeze filter instead of
Hot extract > Coffee filter > freeze filter > reduce > freeze filter

I'd try it, but I'm all out of 190 PGA :(
 

Str8vision

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Forgive me if this has been mentioned but I'm wondering if anyone might suggest a good online source of 1 micron filter paper and what diameter you've found best?

1 micron filters are crazy expensive at $1 - $2 each in pkgs of 100. I bought mine on sale years ago for $0.25 each (pkg of 100) but if I were buying filters today I'd go for the 1.5 micron filter paper instead, it's -a lot- cheaper. I have a filter holder which allows me to use 5.5cm diameter filters (very small) but anyone using a funnel would need a much larger diameter such as 11cm+. You can pleat fold a filter disk for use in a funnel, looks something like a cone shaped coffee filter when done. Here's a link to 11cm diameter 1.5 micron filters https://www.amazon.com/gp/product/B006OP29PE/ref=ox_sc_act_title_1?ie=UTF8&psc=1&smid=ATVPDKIKX0DER Other sizes are available but as the diameter increases so does the price.
 
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Str8vision

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@Str8vision ... I wonder if there's any value in skipping the first freeze filtering phase and going straight to the reduction phase, then freeze filtering? We may not lose as much concentrate as filtering losses?

So Hot extract > Coffee filter > reduce > freeze filter instead of
Hot extract > Coffee filter > freeze filter > reduce > freeze filter

I'd try it, but I'm all out of 190 PGA :(

Yes, there would be little benefit from freeze filtering immediately after the extraction process was complete If you intended to freeze filter after reduction. It only needs to be done once.
 

kbriggs

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I conducted an experiment last week where I heated a single jar of Billy Budd + PGA, ran that through a coffee filter and then split the result into two separate jars. On one jar I did an evaporation/freeze and on the other I reversed the order and did a freeze/evaporation. Each one got a 2.5 micron filter after the freeze and coffee filter after the evaporation. I then mixed each one at 7% and got a dramatic difference:

BillyBudd.jpg


The picture is post-mixing in a 70/30 VG/PG blend. The lighter one on the left was evaporated before the freeze and the darker one on the right had the freeze before the evaporation. It's only been a few days and they need more steeping but the lighter one so far is milder but more pleasant tasting than the darker one.
 

Str8vision

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I wasn't expecting there to be any difference.

Interesting result, the drastic color change is a bit disturbing. That's what I expected/feared when I first tried post reduction winterization. I've only winterized three extracts after reduction; Acid Blondie, Louisiana Red and Acid Opulence. I didn't notice a significant color change from any of them. All three were cold extracted in ethanol for 4 months duration, I haven't tried it on a hot processed extract yet and don't know if the extraction method might influence the results. I have a large batch of cold processed Billy Bud approaching the six month mark, I'll do a side by side freeze filtering comparison on it after it reaches the six month mark.
 

happy valley

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Good day all, it's a quiet Sunday afternoon and thought I'd chime in with a few mid-winter reflections. First I want to mention how I've come to enjoy the pace of this concise, unhurried corner of the vaping world, populated by patient, thoughtful folk who understand process and that good things come to those who wait........and wait we do.

Also I'd like to offer a sincere thanks to the originator of this thread, the months, years of observations, condensed, clearly articulated and shared that went into it and the many helpful contributors here who have markedly flattened the learning curve of NET alchemy for a noob like myself (and given my age that might qualify as an act of humane kindness ;-) It is a reference I find myself returning to time and again.

So, right now I have more than a dozen long term, cold process 190 PGA tobaccos working. They have about 6 weeks on them and I plan on leaving them for at least that long again.

In the near term, I've been using the heat processed 190 PGA method and am presently testing the following tobacco extracts:

Gawith & Hoggarth Brown Flake-
A favorite in the pipe, this is good but light, Virginia predominate. This might be a better candidate for a lengthy cold process. We shall see.

Gawith & Hoggarth Brown Irish X Rope-
Dark and strong, earthy, easy to overdo, good for me at 5%, a real winner, I love it but one would have to like this style of tobacco to begin with.

Gawith & Hoggarth Coniston Cut Plug - this is a real sleeper, comprised of 75% dark fired leaf and a hint of that traditional Lakeland style flavoring, this is smooth but original, might be my favorite thus far.

Rattray's Red Rapparee - A bit of Virginia with Orientals, Black Cavendish and a goodly amount of Latakia, this is one I've always enjoyed in the pipe but as a NET it's not quite as I hoped, too busy and a bit murky tasting, perhaps a cold process would fare better?

McClelland 5100 Red Cake - another Virginia dominate that was a steady rotation in the pipe but far too tame as a NET for my taste. Figuring out the subtle Virginia thing is very much a work in progress.


As addendum, I decided to treat myself for the holidays to a NET sampler from Black Note, ostensibly a quality outfit from CA that certainly does a nice job of marketing and packaging, pricey (in the $1@ml range) but they had a half price sale w/shipping for Christmas. A 4 pack of Virginia, Burley, Cavendish and Kentucky flue cured. They are nice, very clean but mild, frankly and not meant as a slight, these 4 all taste about the same. Honestly, from my fledgling trials thus far, and with the help of the good folk here, I am confident I can do better and for a whole lot less. Cheers!
 

Str8vision

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I have a large batch of cold processed Billy Bud approaching the six month mark, I'll do a side by side freeze filtering comparison on it after it reaches the six month mark.

After a six month cold soak of C&D's "Billy Bud" I separated the tobacco from solvent. I subjected the extract to -20F for 72 hours before running it through a coffee filter, a relatively normal freeze filtering process. After freeze filtering was complete I reduced the extract by 65% and from the reduced extract I mixed a 4 ml sample of NET using 10% extract. I then subjected the remainder of reduced extract to -20F for another 72 hours and filtered it through a coffee filter performing a "post reduction" freeze filtering process. It removed around 60% as much gunk as the initial freeze filtering did. I mixed a 4 ml sample of NET using 10% of the post reduction freeze filtered extract.

Billy Bud compare.png


On the left is the "normal" freeze filtered extract, on the right the "post reduction" freeze filtered extract. Neither have been filtered through anything but a coffee filter. Taste wise I can't really tell any difference between them.

Post reduction freeze filtering does produce a cleaner better performing extract/NET but at the cost of higher filtering losses since what you lose to the filters is highly concentrated. I intend to modify my extraction procedures to include it.

As a side note I would add that for C&D's "Billy Bud" a 12 hour hot extraction yields results almost as good as this 6 month cold soak, there's just not enough difference in flavor to justify such a long wait.

EDIT: Read post #1001 below for an update.
 
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happy valley

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The bottle on the right looks really clean.
12 hour hot extraction yields results almost as good as this 6 month cold soak, there's just not enough difference in flavor to justify such a long wait.

Interesting......... quite a revelation considering the time involved.

Is the 65% reduction +/- what you usually shoot for?
 

kbriggs

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As a side note I would add that for C&D's "Billy Bud" a 12 hour hot extraction yields results almost as good as this 6 month cold soak, there's just not enough difference in flavor to justify such a long wait.

Yeah, I recently finished a 90-day room temp PGA extraction of Billy Budd and so far it's not much different than my heated 12-hour version. If anything it seems a little milder so I'm going to stick with the shorter heated method.
 
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Str8vision

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Yeah, I recently finished a 90-day room temp PGA extraction of Billy Budd and so far it's not much different than my heated 12-hour version. If anything it seems a little milder so I'm going to stick with the shorter heated method.

Same with Sutliff's "Voodoo Queen", not much of a flavor difference between a 12 hour hot extraction and 6 month cold soak. L red was better cold as were the cigars so I guess it depends on what tobacco is in play.

EDIT: Read post #1001 below for an update.
 
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