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alternative to 190 proof alcohol

SkyHighLer

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I just finished distilling twice the combined distillations of the four 1.75mL bottles of vodka, and I got one full bottle at 92.0% (<195F faction,) and ~600mL in a second bottle at 90.0% (some of the <194F faction, and the 195-202F faction.) I also have about 350mL of 203/205-215F tails left over.

I'm going distill two more bottles three or four times using what I now know, and see if that gets it to >90%.


I took apart the bottom end of my replacement water distiller yesterday, it's better made than the first one I bought for $15 more, I think my original might have been a dirty Chinese knock off of the Chinese knock off of the MegaHome.
 
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troutman

Seed Whore
From troutman, one of the best pieces on anything I've ever read, smooth..... :biggrin:

Here's more info to help you and why high temps can hurt your purity. :tiphat:

The temperature of the vapour is the max high your still temps should be set.
For example: notice that 40% ethanol boils at just below 96°C
So higher temps are not required and mean less quality.
Alcohol_curve.jpg

From here:

https://homedistiller.org/theory/theory/strong
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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I just finished distilling twice the combined distillations of the four 1.75mL bottles of vodka, and I got one full bottle at 92.0% (<195F faction,) and ~600mL in a second bottle at 90.0% (some of the <194F faction, and the 195-202F faction.) I also have about 350mL of 203/205-215F tails left over.

I'm going distill two more bottles three or four times using what I now know, and see if that gets it to >90%.


I took apart the bottom end of my replacement water distiller yesterday, it's better made than the first one I bought for $15 more, I think my original might have been a dirty Chinese knock off of the Chinese knock off of the MegaHome.


You should be able to get the rest of the way using Dri Rite.
 

SkyHighLer

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You should be able to get the rest of the way using Dri Rite.

Would the CaSO4 in Drierite be better in this instance than 3A molecular sieves?


Speaking of which, from Bhogart, who carries 3A and 5A sieves,

"All our desiccant is manufactured in China. Thank you for your consideration.

Taymoor from Bhogart.com

On Fri, Aug 31, 2018 at 10:20 AM, xxxxxxxxxxxxx wrote:
Where are you sourcing your 3A molecular sieves? Can you say they're first quality, not from China or India? TIA!"


"Testing eBay Molecular Sieves by NurdRage,"

https://www.youtube.com/watch?v=MduzjhRHBFY


I just bought these inexpensive 3A molecular sieves with Amazon Prime, and will have them in two days to test out,

https://www.amazon.com/gp/product/B06Y2B4CPK/ref=oh_aui_detailpage_o00_s00?ie=UTF8&psc=1
 
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Gray Wolf

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Would the CaSO4 in Drierite be better in this instance than 3A molecular sieves?


Speaking of which, from Bhogart, who carries 3A and 5A sieves,

"All our desiccant is manufactured in China. Thank you for your consideration.

Taymoor from Bhogart.com

On Fri, Aug 31, 2018 at 10:20 AM, xxxxxxxxxxxxx wrote:
Where are you sourcing your 3A molecular sieves? Can you say they're first quality, not from China or India? TIA!"


"Testing eBay Molecular Sieves by NurdRage,"

https://www.youtube.com/watch?v=MduzjhRHBFY


I just bought these inexpensive 3A molecular sieves with Amazon Prime, and will have them in two days to test out,

https://www.amazon.com/gp/product/B06Y2B4CPK/ref=oh_aui_detailpage_o00_s00?ie=UTF8&psc=1


The suggestion came from Pharmer Joe, who thinks so.
 

Gray Wolf

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The suggestion came from Pharmer Joe, who thinks so.

Causa where ah was brung up, ah do know how to get to 190 proof in less steps, and that is a refluxing still. A refluxing still has a tall column packed with things like metal rings, ribbon, et al, which cool the boiling alcohol vapors as they lose heat passing in contact with the metallic packing in the column.

After the system reaches equilibrium, only the purest vapors are able to make it all the way to the top, where they are allowed to spill into a condenser to turn them back to a liquid.

A thermocouple placed at the top of the column, will tell you the boiling point of the vapors coming through, thus what purity is coming through.

~95.6% EtOH is the azeotropic balance between ethanol and water at atmospheric pressure. To get higher purity requires a drying agent or a vacuum, which is why Everclear is only 95%/190 Proof.

There are ample online examples of refluxing stills primarily using copper, but attached is what I came up with as a throw down design using readily available stainless sanitary components and stainless steel ribbon, using commercial stainless steel pot scrubbers.

My design is a compound refluxing still, because it has two condensers at the top of the column. Instead of a tee at the top of the column, followed by an elbow and the water cooled condenser, the column has a cross and the overflow port to the elbow and first condenser has a valve on it, with the extra port on both designs plugged with a thermocouple.

The valve lets you block off the normal path to the condenser, so that the vapors reach another condenser at the top of the column, where you can control the flow at various purity levels by regulating the temperature and flow of the water through the condenser.


PS: Note that the example shown uses a boiler of less than one gallon capacity and is used in essential oil extraction in a laboratory. Do look at your local regulations with regard to operating a still and creating high purity ethanol without being licensed and paying taxes.
 

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SkyHighLer

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The suggestion came from Pharmer Joe, who thinks so.

I've searched and searched, indicating or non-indicating, and what mesh granules??

Also, can the molecular sieves or the Drierite be regenerated in a microwave oven?
 

troutman

Seed Whore
I've searched and searched, indicating or non-indicating, and what mesh granules??

Also, can the molecular sieves or the Drierite be regenerated in a microwave oven?

Molecular sieves and Drierite can be regenerated. But I wouldn't use a microwave oven.

Use a regular stove. Maybe even cook a pizza at the same time. :biggrin:

Drierite = Calcium sulfate.

It can be dehydrated at 163°C according to my one of my better chemistry books.

https://en.wikipedia.org/wiki/Calcium_sulfate

Molecular sieves 3A need about 250°C and 4A sieves need 280-300 °C for 2 hours to be regenerated. :tiphat:

https://en.wikipedia.org/wiki/Molecular_sieve#Regeneration
 

troutman

Seed Whore
I was just reading that molecular sieves 3A or 4A can both be used to dry ethanol.
That 4a works better than 3A. But 3A is used more often due to them requiring less
energy regenerate. 4A is recommended for solvents like hexane.

I found this drying solvent webpage:

Molecular sieve 0.3nm = 3A
Molecular sieve 0.4nm = 4A.

Solvents Drying and Drying Agents
 

SkyHighLer

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I tried substituting a cheap power controller for the Variac I use to lower the wattage of my water distiller. It works ok, dialing exact wattages isn't nearly as easy, but can be done.

To use a cheap ($55) countertop water distiller to distill alcohol I suggest you at least lower the wattage, this can be done simply by plugging the condenser fan in with it's own plug, and then feeding the base unit through either a Variac or solid state power controller like I mentioned above, the wattage is monitored with a power meter before the Variac or power controller.

What you need:

1) Water distiller

https://www.ebay.com/sch/i.html?_fr...+distiller.TRS0&_nkw=water+distiller&_sacat=0

2) An extra appliance cord (one comes with your distiller, you need a second one) to plug the condenser directly into the wall

https://www.amazon.com/Hosa-PWC-148...qid=1536000904&sr=8-8&keywords=appliance+cord

3) Power meter

https://www.amazon.com/s/ref=nb_sb_...prefix=kill+a+watt+,aps,195&crid=8U24L84O2VGH

4) Variac or solid state power controller

https://www.ebay.com/sch/i.html?_from=R40&_trksid=m570.l1313&_nkw=20a+variac&_sacat=0

or

https://www.amazon.com/gp/product/B00OZ5MBM6/ref=oh_aui_search_detailpage?ie=UTF8&psc=1

That solid state power controller is simple to wire with just an extension cord (see the picture below.)


No taking the distiller apart or anything. You just adjust the power to a 1-2 drip per second rate, note the wattage for the next time, and taste the output until it's water or near so.


To go further you need to open the base of the distiller, and add a thermocouple for temperature readings and/or controller input.
 

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SkyHighLer

Got me a stone bad Mana
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I haven't messed with the 3A molecular sieves yet.

I just finished distilling the remaining tails from the six 1.75mL bottles of cheap vodka.

The result so far:

One full 1.75mL bottle of 92.0% ABV
One nearly full 1.75mL bottle of 91.0% ABV
160mL of 90.5% ABV (from the tails)

Total ~3.6L of ~91% ABV from 10.5L of 40% ABV (40% of 10.5L is 4.2L)

Cost me $70 including tax for the six bottles, Everclear is stronger and less expensive.


I'm going to take what I learned and apply it to distilling two more 1.75mL bottles, then I'll try the sieves to get some to 95% ABV or better.


Bottom line, the cheap countertop distillers with the wattage under control can be used to distill alcohol, but you need to distill several times.


If you're thinking you'll just get a reflux still, remember they are more of a hassle as they use water cooling.


Interesting discovery, the discard 'water' remaining after every distillation was slightly cloudy. I'm too cheap to try another brand of vodka. :biggrin:
 

troutman

Seed Whore
Bottom line, the cheap countertop distillers with the wattage under control can be used to distill alcohol, but you need to distill several times.

The Bottom Line;

is if everything is not properly sealed with a drying tube you'll never get
better than 95% even if you use molecular sieves or other drying agents.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
5g of 200 proof 100% food grade kosher ethanol
299

NON-denatured

"UTILITY GRADE 200-PROOF (NOT-CERTIFIED-ORGANIC) GRAIN ALCOHOL - 5 GALLON
IN STOCK
Excluding Federal Excise Tax: $125.00

Alchemical Solutions' 200-proof neutral non-organic, Utility Grade Grain alcohol is made from non-organically-certified grain (in other words, it is not certified organic, it is pure alcohol WITHOUT organic paperwork trace-ability).

We maintain the utmost level of quality and attention to detail, while at the same time adhering to environmentally sound practices.

Tested by an independent lab to insure that they meet United States Pharmacopeia (USP) standards, not all pure alcohol is pharmaceutical grade - only 190 proof and 200 proof pure ethanol which meets or exceeds the stringent standards of the USP.

Five gallon purchases ship in a single food-grade, high-density polyethylene container suitable for shipping high-proof alcohol."

https://organicalcohol.com/utility-grade-alcohol-200-proof-5-gallon/

"Federal Excise Tax Rate Update The Organic Alcohol Company has reached the limit of alcohol that can be sold at the reduced Excise Tax rate of $2.70 per proof gallon in 2018. Under the Craft Beverage Modernization and Tax Reform Act of 2017 passed by Congress on last December 22nd, the new rate of $13.34 per proof gallon must now be collected for all sales until the end of 2018. (Before 2018, the rate on distilled spirits was $13.50 since 1991.) The rate of $2.70 will become effective again on January 1st, 2019. '$13.34 per proof gallon' translates into $26.68 per gallon for 200-proof alcohol, and into $25.35 per gallon for 190-proof alcohol - this is the current basis for the excise taxes collected on nation-wide sales of high-proof alcohol that are remitted directly to the US Department of the Treasury Alcohol and Tobacco Tax and Trade Bureau (TTB). For more official details, see https://www.ttb.gov/alcohol/craft-beverage-modernization-and-tax-reform.shtml"

https://organicalcohol.com/#
 

h.h.

Active member
Veteran
Is there a distinction between, methanol, ethanol, or isopropyl alcohols, when it comes to extractions?
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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Is there a distinction between, methanol, ethanol, or isopropyl alcohols, when it comes to extractions?

Yes, they are different polarities and extract differently. Iso is least polar and Methanol most polar.

Ethanol is GRAS and the other two are not.
 

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