Tobacco extraction using heated Ethanol

[Str8vision]

........Many people around the globe have informed me they don't have access to 190 proof, most can't even get 151. I do believe 151 would work just fine but haven't tried it myself. My curiosity is peaked so I'll use 151 proof PGA for my next extraction, we'll see what transpires....

I performed the experiment using 151 proof PGA for the extraction solvent. For the experiment I extracted C&D's "Old Joe Krantz". After the 12 hour hot extraction was complete I drew 30ml of extract off before sealing the jar and allowing the remainder to sit at room temperature for a month. The 30ml that was drawn off has been freeze filtered, reduced, and filtered. Initially I reported the extract smelled off, something like an over-processed hot PG based extraction, it still does. I mixed up 10ml of NET and shake-N-vape it tastes terrible. Generic musty tobacco flavor that doesn't resemble the Old Joe Krantz I'm familiar with. Tastes "murky" and lacks any well defined flavor notes, low or high. I'll let it age for a month before re-sampling but I have -serious- doubts about its chances.

I'm disappointed (and a bit surprised) but I'm also now curious. If the 25% water content in 151 proof PGA has this much negative impact on flavor, how much does the 5% that's present in the 190 proof I normally use have? Would flavor be noticeably better if 200 proof (pure ethanol) was used? I intend to find out but it'll be a few weeks before I can.

 

[kbriggs]

If the 25% water content in 151 proof PGA has this much negative impact on flavor, how much does the 5% that's present in the 190 proof I normally use have? Would flavor be noticeably better if 200 proof (pure ethanol) was used?

I was wondering the same thing. Are you planning on purchasing the 200 proof pga or making your own with those molecular sieves?

 

[brewbear]

I was wondering the same thing. Are you planning on purchasing the 200 proof pga or making your own with those molecular sieves?

I plan on using 151 and add the molecular seives. As it stands, I ordered the molecular sieves almost two weeks ago, received an email from them saying they're preparing to ship a week ago. Hopefully I will receive them this week. I guess if you're planning on using the molecular sieves, you need to order well in advance.

 

[Str8vision]

I was wondering the same thing. Are you planning on purchasing the 200 proof pga or making your own with those molecular sieves?

The cost of 200 proof (with shipping) is just too high, think I'll use 3A sieves to convert 190 proof PGA.

EDIT: What I hope to find is that the 5% water content in 190 proof has little or no adverse effect on flavor.

 

[kbriggs]

I guess if you're planning on using the molecular sieves, you need to order well in advance.

I've seen them on Amazon Prime so I'd just go there.

 

[brewbear]

I've seen them on Amazon Prime so I'd just go there.

I just ordered from the source, as it were, Sorbent media.....figured it would be faster but I guess I am wrong.

 

[jonnydoe]

Does somebody knows where to buy these cigarettes or tobacco ?

MAGIC 0 and MAGIC 2 – 22nd Century Group, Inc.

SPECTRUM Government Research Cigarettes – 22nd Century Group, Inc.

Its about low nicotine cigarettes. Perhaps they have also low tsna content. But i can not find more information.
My english is not good enough. I have problems to find any shops. On the website they have written that they only sell to RTI. Who is RTI ?

 

[brewbear]

I guess ordering the molecular sieves from Amazon will be faster. My order was placed on Oct 5th. I just got the notification it was sent. Even FT ships faster!

 

[kbriggs]

I guess ordering the molecular sieves from Amazon will be faster.

Mine came today from Amazon. It's in pellet form rather than beads but is labeled as "3A":
https://www.amazon.com/gp/product/B071W5ZZ7Z

I also picked up this hydrometer and graduated cylinder:
https://www.amazon.com/gp/product/B007VFBG1O
https://www.amazon.com/gp/product/B00FGDFBAK

I have about a half liter of 190 Proof "Mohawk" PGA on hand so I tested it and after adjusting for temperature using the included chart, it indicated about 191 proof so that's good enough.

So now the question is, how much of these sieves do I dump into a half liter of 190 proof to bring it up to 200? And for how long, 24 hours?

 

[Str8vision]

.....So now the question is, how much of these sieves do I dump into a half liter of 190 proof to bring it up to 200? And for how long, 24 hours?

500ml (half liter) of 190 proof should contain no more than 25ml of water (5%). If I remember right, fully activated sieves can absorb/hold 22% of their weight so I'd likely use 5 or 6 ounces of the sieves which is roughly 1/3 of the bag you ordered. I believe the sieves need to be activated before use. Spread out in a single layer on a baking (cookie) sheet, it seems like at 450F it takes a few hours. Once cooled add to the PGA. Remember to stir/swirl the alcohol every now and then. I'm not sure how long it takes but I'd likely give it the better part of a day before testing. I'm just guessing. Let us know what you end up doing and how it turns out.

 

[kbriggs]

sieves can absorb/hold 22% of their weight

I found that 22% number right after posting so I calculated 227g needed for 1 liter of 95% alcohol. So I went with 150g (5.3 ounces, about 1 cup) for the half bottle. I did not think to pre-dry the pellets, though. I'll do that if I don't get a good result by tomorrow. They do kick up quite a cloud in there so I'll definitely be filtering this.

 

[kbriggs]

So my molecular sieve experiment was mostly successful with a huge cautionary note about putting ethanol soaked pellets in a hot oven. So I let my half liter of 190 (tested at 191) proof PGA soak with 150 g of the pellets for 24 hours with occasional stirring. The pellet dust kept the mixture cloudy the whole time. I poured it out through a coffee filter but it didn't catch much. So I poured again through 2.5 micron paper and that got most, but definitely not all of it. And that took 2 hours.

While that was filtering I washed the pellets with 3 water rinses to remove the alcohol (or so I thought) and then spread them out on a cookie sheet. I put that in the oven at 350 F and set the timer for 60 minutes. Well about 5 minutes into it I hear a loud bang and the over door comes flying open. I look inside and there's a nice alcohol fire floating just above the pellets, which went out pretty quickly. But otherwise, no damage done. I left the oven door cracked for awhile before it closing it. After an hour I took them out and weighed them after a cool down period. It came to 155 g, so 5 g over the initial weight. Close enough for now.

As for the PGA, I measured it at 197 proof, so it went up 6 proof from 191. Not bad I guess. Pre-drying the pellets, using more of them and for a longer period may have brought it up near 200. I've got tobacco on order so won't be able to extract anything until next week.

 

[Str8vision]

I poured again through 2.5 micron paper and that got most, but definitely not all of it.

I wonder what level of particle retention will be required to remove all the dust, 1 micron? 0.5? Watching the video it's apparent the dust will settle to the bottom if given enough time, the ethanol appeared to be crystal clear.

Pre-drying the pellets, using more of them and for a longer period may have brought it up near 200.

Activating the sieves before use might have helped, could be they were partially burdened with moisture. Seems like 24 hours should have been more than enough time. Nothing wrong with using extra sieves, the guy in the video did just that. Guess if I calculate 10 ounces of sieves are required, I'll use 15.

 

[brewbear]

Guess if I calculate 10 ounces of sieves are required, I'll use 15.

It seem in this case "the more, the merrier!"
If it took 24 hours, more or less, for 500 ml of 191 to reach 197 proof, I'm in a world of hurt! All I can get is 151 but I do have a whole pound of sieves! I'm going to start with 750 ml of 151.....but I have to wait another week or so

 

[kbriggs]

I wonder what level of particle retention will be required to remove all the dust, 1 micron? 0.5? Watching the video it's apparent the dust will settle to the bottom if given enough time, the ethanol appeared to be crystal clear.

It was still fairly cloudy after sitting overnight for 9 hours. But after I was done and was doing a water rinse, the water was less and less cloudy after each rinse so I think I could have just cleaned them all beforehand and then dried them, and probably would have had much less dust putting them in the PGA. So I'll probably do that on the next bottle.

 

[kbriggs]

If it took 24 hours, more or less, for 500 ml of 191 to reach 197 proof, I'm in a world of hurt!

I didn't test before 24 hours so who knows if I really needed that much time. I might have just needed more sieves, I only used about one-third of the bag.

 

[Str8vision]

......I washed the pellets with 3 water rinses to remove the alcohol (or so I thought) and then spread them out on a cookie sheet. I put that in the oven at 350 F and set the timer for 60 minutes. Well about 5 minutes into it I hear a loud bang and the over door comes flying open. I look inside and there's a nice alcohol fire floating just above the pellets, which went out pretty quickly. But otherwise, no damage done. I left the oven door cracked for awhile before it closing it......

Your post likely saved me from experiencing a similar outcome, thanks for the heads-up, knowledge is power. I initially plan to rinse the sieves off in distilled water but I'll fan dry them before baking.

I'll bake mine at 450F for two hours. The sieves I plan to buy recommend 450F to 550F for activation/re-activation. I'll definitely leave the oven door cracked open for the first ten minutes or so while closely monitoring them. I'll store the sieves in a quart canning jar for an air/moisture tight seal. As the sieves cool they'll likely pull a vacuum inside the jar. That's the "plan" at least.

 

[Str8vision]

It seem in this case "the more, the merrier!"
If it took 24 hours, more or less, for 500 ml of 191 to reach 197 proof, I'm in a world of hurt! All I can get is 151 but I do have a whole pound of sieves! I'm going to start with 750 ml of 151.....but I have to wait another week or so

I'm curious just how much ethanol you'll end up with, I'm "guessing" around 500ml. Converting 750ml of 151 proof PGA to 200 proof using 1 pound of 3a sieves will require at least two passes. A pound of fully activated sieves can only absorb/hold a maximum of 3.5 ounces of water (~105ml), whereas 750ml of 151 proof PGA contains around 187ml of water. You definitely want to fully activate (bake) the sieves before using them so they're at their peak efficiency. The first pass could boost you to near 175 proof (~88% ethanol), the second pass might get you the rest of the way or at least "close enough". I look forward to hearing how it goes!

 

[kbriggs]

I initially plan to rinse the sieves off in distilled water

So I decided to do that with the 365 g of yet-to-be-used sieves which I put in a mayonnaise jar. So I just poured distilled water right into the jar near full and man it got hot. Too hot to hold the jar. My laser temperature gun read 142 F. I was not expecting a thermal reaction like that. I assume tap water would have done the same? I don't have any more virgin sieves to test. When I added 150 g to my PGA the other day I didn't notice any temperature increase. But I did that slowly through a funnel which kept getting jammed.

 

[Str8vision]

A 70F rise in water temperature but no such reaction when added to PGA? Interesting. Did you notice any reaction when you rinsed the 150g of sieves in water after they were exposed to the PGA the other day?