Sciencemadness Discussion Board - Arkoma attempts 95% azeotropic EtOH

Arkoma attempts 95% azeotropic EtOH

arkoma - 13-4-2016 at 20:40

13 APRIL 2016 Attempt at 95% Azeotropic Ethnanol

I have attached actual photos of my lab notebook.

Summary:

Well, I started with 56% EtOH and H₂O solution. Figured this would be as straight forward as the initial distillation of my low percentage EtOH wash. First off, I way overloaded my 1 litre RBF. 819ml. STOOPID. My heat source is a fry daddy with no thermostat. This caused several SERIOUS bumping incidents, including one that blew my thermometer adapter out of my distillation head and sprayed boiling EtOH everywhere. Thank goodness there was no source of ignition, and I did have a fire extinguisher within arms reach. By trying to "hurry" at the end of an 2 hours I ended up with 100ml of 87% EtOH per my hydrometer. I could have burnt my house down.

Conclusions:

I need a water bath instead of a temperature unregulated oil bath for a distillation of EtOH at high percentages. Or perhaps a triac control or maybe a damned real thermostatically controlled hotplate. THIS STUFF BUMPS LIKE YOU WOULD NOT BELIEVE, noobs and youngsters take note.

What I listened to "While Doing The Dirty" LOL;

Belinda Carlisle-Heaven is a place on Earth
Marilyn Manson-Tainted Love
Katy Perry-Wide Awake
Pet Shop Boys-East End Boys
Cranberries-Linger
Disturbed-Down With the Sickness
Duran Duran-Rio
Easton Corbin-A Little More Country Than That
Patti Smyth-I Am the Warrior
Lady Gaga-Poker Face
Madonna-Music
Pistol Annies-Hell On Heels
Metallica-The Memory Remains
Brooks & Dunn w/Reba-Cowgirls Don't Cry
Carrie Underwood-Blown Away
Blondie-Heart Of Glass
Sugarland-All I Want To Do
Jamey Johnson-In Color
Slayer-Seasons In the Abyss
Travis Tritt-Modern Day Bonnie and Clyde
Megadeth-A Tout Le Monde
Jethro Tull-Locomotive Breath

Now, on to "Bad Habits in the Lab"--DRINKING--Just noticed I "lost" an hour in my notes *sigh*

crystal grower - 13-4-2016 at 20:51

Yay Arkoma, Im glad nothing happened to you

, by the way, you're real mad scientist!

arkoma - 13-4-2016 at 20:56

This is gonna be harder than I thought. Think I might need to distill over oven dried gypsum. Getting to 60, 70% is no sweat, 95% is a challenge

j_sum1 - 13-4-2016 at 21:00

That is quite a playlist you got going there.

arkoma - 13-4-2016 at 21:12

I have "Eclectic" taste. Put vlc on random and let it go. Have HUNDREDS oif music videos.

Magpie - 13-4-2016 at 21:27

If you are distilling just pure water and alcohol (no mash particles), AND you have added boiling stones (I use porous pottery shards) you should not have bumping problems. Bumping problems are often caused by solids settling on the bottom of the pot and causing localized overheating.

JJay - 13-4-2016 at 21:50

I have done this dozens of times with no boiling stones or anything of the sort. A boiling water bath is definitely the way to go. I'm not sure why you would insulate your Vigreux.

violet sin - 13-4-2016 at 22:27

First off, just have say... Was a little dissapointed to see you were making 95% not drinking(trying) 95%. Lol.

Secondly, nice work keeping that noggin fed and trying new things. If you get some of the kinks worked out, you may find aga pulling down your driveway one day

boiling chips are nice, just for peets sake be smarter than i was... Put it in first, not after its warmed up.. steam clean your flesh over the flask neck and end up wearing god knows what some time(think it was copper chloride for me). Keep up the good work man!

Here is something dirt cheap that could help:
http://www.ebay.com/itm/50-110-C-Heat-Cool-Temp-Thermostat-T...

$3.19 free s/h, can switch 10A appliance so may be a winner!

Another note,.. put a glass globe over you light bulb. Looks like it takes one, with 3 or so set screws on the rim. Be a shame to have temp shock give you an ignition source if it were to spray from your glassware just right. I live by Murphy's law daily(technically it's my law, but i take no responsibility for the pizza franchise). Think ahead of the curve

woelen - 13-4-2016 at 22:54

Indeed, that was a good lesson learned and happily nothing worse happened than the loss of some ethanol. This could indeed have resulted in a huge fire!

You need a long column and need to apply minimal heat so that the ethanol just boils over. In that way, you should be capable of getting 85 to 90%. You will need patience though. If you hurry and have a lot of liquid distill over in short time, then a lot of water distills over as well.

Getting to 95% azeotrope will indeed be hard. I think that a chemical drying agent like CaSO4 or CaCl2, combined with distilling, is the best for getting water out. Having all these solid materials, however, introduces other problems like caking. Especially CaSO4 will lead to a very hard to remove cake of solid.

Corrosive Joeseph - 13-4-2016 at 23:23

Quote: Originally posted by woelen

Indeed, that was a good lesson learned and happily nothing worse happened than the loss of some ethanol. This could indeed have resulted in a huge fire!

You need a long column and need to apply minimal heat so that the ethanol just boils over. In that way, you should be capable of getting 85 to 90%. You will need patience though. If you hurry and have a lot of liquid distill over in short time, then a lot of water distills over as well.

Getting to 95% azeotrope will indeed be hard. I think that a chemical drying agent like CaSO4 or CaCl2, combined with distilling, is the best for getting water out. Having all these solid materials, however, introduces other problems like caking. Especially CaSO4 will lead to a very hard to remove cake of solid.

How long is a long column............?

This is VERY similar to my latest project. I am using a water bath (an old deep fryer with no thermostat running water), a 1l RBF and a 300mm length homemade column of 30mm stainless tube filled with stainless steel scrubbers. I also have a 400mm length of the same tube which is about to be tried next. I have just taken delivery of an 'alcoholmeter' and will report back with my findings.

My starting material is distillate from the mash in the 'beer stripper' and measured 58% EtOH

95% is also my target figure..............

I will be watching this thread with great interest.............

CJ

aga - 13-4-2016 at 23:48

It just so happens that i'm also distilling booze, although i want 100% EtOH.

woelen's suggestion of gentle heating does seem to help.

Insulating the vigreux might be counter-productive, although i'm not sure exactly why (something to do with the reflux equilibrium).

After two initial runs from a 1L bottle of 37.5% vodka, the distillate was distilled again to get around 350ml of constant-boiling 78C ethanol.

Next up is dehydration using tripotassium phosphate if i can sucessfully make it properly. CaO doesn't seem to work very well for me.

woelen - 13-4-2016 at 23:50

A column of 30 to 40 cm should be OK. I myself have a vigreux and this works quite well, but you need to heat, so that the top of the column is just reached and the column must be wrapped in isolating foil or linen or something like that, especially if there is variable air-flow in the room where you perform the distillation. Otherwise the behavior is erratic, at one moment the distillation goes too fast, at other moment nothing distills over. I can see in my colum that the top of the vapor column moves up and down with wind around the column varying in speed and direction.

JJay - 14-4-2016 at 00:41

I usually do three runs using an uninsulated 30 cm Vigreux with a boiling water bath and then finish dehydrating with 3A molecular sieves. This doesn't completely eliminate ketone denaturants (for that I could probably reflux with sodium hydroxide but I'm not drinking the stuff), but the resulting anhydrous ethanol works ok for most purposes.

[Edited on 14-4-2016 by JJay]

CuReUS - 14-4-2016 at 00:56

I may be paranoid,but a naked incandescent bulb so near a distillation setup for ethanol sounds like a recipe for disaster,does it not ?

aga - 14-4-2016 at 05:09

Paranoid.

I use an open flame spirit burner for ethanol, acetone etc.

That said, the shed is pretty much expendable.

Chemist_Cup_Noodles - 14-4-2016 at 05:33

Also if you don't have any boiling chips, just add some glycerin to your alcohol and water. I did it the other day just sort of chucking science at the wall, and I must say I'm very happy with the result. It has almost triple the BP of water, and quadruple that of EtOH. This stuff will make the liquid a lot more viscous and thick and hopefully it won't bump as much. It will also allow the temperature of the solution to be a little higher while boiling. By this means I've gotten some very vigourous but very tame boiling that nicely hovers ~85^oC so the alcohol boils out truly quite fast. And because it bumps very gently if at all with the addition of the glycerin, I don't even need a vigreux column. It actually sort of bubbles like the swamps of Dagobah.
I too use a hot oil bath, and I do this outside with absolutely no possible sources of ignition. But I like to keep my oil bath around ~120-130^oC. At this temperature I still get a fantastic drip rate coming out of my condenser. And after all is said and distilled I just swirl around my glycerin and most of the remaining EtOH escapes, and then I burn off any last little traces. 10/10 would recommend.

arkoma - 14-4-2016 at 06:47

@violet sin 95% can be rather toxic

@JJay no denaturants as this was a simple sugar "wash" made with turbo yeasts

I had a bunch of bent pennies in the bottom of the flask. I'll try actual porcelain chips as the name of the game is nucleation sites, right?

@aga, I can't explain the science behind it, but Mr. Vogel in his wonderful Org Chem book says to keep a fractioning column insulated or even in some cases heated. I can use Trisodium Phosphate to dry EtOH? I have a box of it as it is still OTC here.

And yeah, I need to do two things:

1) Do this earlier in the day so I ain't as "buzzed" on Tasty Malt Beverages

2) cover and move that damn light.

JJay - 14-4-2016 at 11:47

I am of the opinion that insulation isn't really necessary with liquids boiling under 100 C. What really matters is the reflux ratio; insulation tends to lower it, and higher reflux ratio leads to purer product. Of course, you may need to insulate if your product can't make it through the column. Here are Vogel's words on the subject:

In practice, it is usual to employ a fractionating column to reduce the
number of distillations necessary for reasonably complete separation of
the two liquids. A fractionating column is designed to provide a continuous
series of partial condensations of the vapour and partial vaporisations
of the condensate and its effect is, indeed, similar to a number of
separate distillations. The effect of partial condensation will be evident
from Fig. /, 4, 2. If the temperature of the vapour is lowered, it will partly
condense giving a hquid richer in B and leaving the vapour richer in A.
The vapour passing up the column will accordingly contain more of A than
did the vapour which left the boiling liquid. Similarly the hquid returning
to the flask will contain relatively more of the less volatile component B.
A fractionating column consists essentially of a long vertical tube
through which the vapour passes upward and is partially condensed;
the condensate flows down the column and is returned eventually to the
flask. Inside the column the returning hquid is brought into intimate
contact with the ascending vapour and a heat interchange occurs whereby
the vapour is enriched with the more volatile component A at the expense
of the hquid in an attempt to reach equihbrium. The conditions necessary
for a good separation are :—(i) there should be a comparatively large
amount of hquid continually returning through the column ; (ii) thorough
mixing of hquid and vapour ; and (iii) a large active surface of contact
between liquid and vapour. Excessive cooling should be avoided ; this
difficulty is particularly apparent with liquids of high boiling point and
may be overcome by suitably insulating or lagging the outer surface of
the column or, if possible, by surrounding it with a vacuum jacket or an
electrically heated jacket. Various types of laboratory fractionating
columns are described in Sections II, 15-11,18

[Edited on 14-4-2016 by JJay]

arkoma - 14-4-2016 at 12:14

As soon as I get my "Safety Protocol" a bit more in hand, I'm going to re-attack this. I might try it with and without the foil. I've got Vogel's Third in eBook. My older brother had a damned HARD BACK of it once. Got stolen, dangit.

I think the biggest thing I need to realize is that I need to slow way down on my input of heat. The last piece of my "Bunn-O-Matic" that I haven't utilized yet is this thermostatic control. I'm seeing it repurposed to rein in the FryDaddy

JJay - 14-4-2016 at 12:40

A boiling water bath is the perfect temperature for this application - hot enough to boil ethanol but just not quite hot enough to boil a flask of water. You can use a higher-tech solution, but it's going to be awfully hard to find one that works better than boiling water.

I've been thinking about using thermostatic controls too, but I'd want one that is good to 300 C.

aga - 14-4-2016 at 13:20

Column insulation must certainly depend on ambient temerature.

I have no idea where Vogel lived, cold or hot.

Here the ambient temps are relatively high (24+) at least during the day.

In my current ambient temperatures i think that a water bath would be an excellent choice for EtOH distillation, the column needing no insulation.

Reading your post AFTER doing 5 EtOH disty runs today makes me feel like an idiot.

Nothing new there then !

aga - 14-4-2016 at 13:22

Quote: Originally posted by arkoma

I need to slow way down on my input of heat

Gentle boil dude, just like, yeah, simmer.

arkoma - 14-4-2016 at 18:40

OK. I dug out the "Bunn-O-Matic" thermostatic control and wired it to an outlet. Anyone that notices the duct tape, know that I AM a Red Green devotee. The temp control isn't very "fine", BUT I can keep the temp within' MUCH more acceptable limits. Hovering around 93 C is way better than the wide open temp of around 202 C.

This evenings notes and "playlist" I'm thinkin' the playlist is kinda like solving a blockchain hash--"Proof of Work" LOL--plus y'all get a peek into the mind of an eccentric middle-aged Neck^*

^*Y'all do get the pun, dontcha'?

Sparklehorse - 15-4-2016 at 09:25

Arkoma, love your posts and sense of humor. Also great taste in music. Posting playlists should be a forum requirement

I just did about the same thing, starting from vodka, distilled in 1L RBF with a vigeraux, but I was using a mantle/stirrer. Looking at the column, I could see the difference between the water condensation and the ethanol condensation and sort of a break about half way up the column where the water condensation stopped and ethanol was more pronounced. As the distillation approached completion, the water condensation slowly worked its way up until it was all the way in the still head. I was thinking that as long as I didn't have any water condensation in or near the head, that the ethanol coming over should be pretty close to azeotropic. The water would for many droplets while the Ethanol hardly formed any. After the first run I redistilled the distillate, dried over 3A sieves, and then filtered through diatomaceous earth to get rid of the particulate from the sieves. I was shooting for 100% anhydrous but I don't really have a good way to check the moisture content besides checking the density.

JJay - 15-4-2016 at 09:42

I'm not really sure where to post playlists. I am in a KMFDM mood today:

KMFDM - Krank (Official Music Video)
KMFDM - Megalomaniac [HD]
KMFDM - A Drug Against War ‌‌ - Bohemia Afterdark
KMFDM - Amnesia (Official Music Video)
Juke Joint Jezebel - KMFDM
KMFDM - Bitches
KMFDM - Stray Bullet
KMFDM - Looking For Strange(Super Strange mix).
KMFDM - D.I.Y
KMFDM - Free Your Hate
KMFDM - Virus - (Ghost In The Shell)
Eisenfunk - Pong
KMFDM - Power
KMFDM - Anarchy
KMFDM - I Am What I Am
KMFDM - Godlike
KMFDM - Money
KMFDM "I Heart Not" (Official Video)
KMFDM - Professional Killer
KMFDM - Bait And Switch.
PSYCLON NINE "parasitic" -official-
KMFDM - Risen
KMFDM - Light.
KMFDM - Today
KMFDM - Blackball
KMFDM - Waste

aga - 15-4-2016 at 10:41

Quote: Originally posted by arkoma

^*Y'all do get the pun, dontcha'?

A Star Redneck.

Er, yeah, ahem, we just didn't like to say er, anything, ahem.

I now got about 450ml near-azeo EtOH.

Also some tripot phos in the oven in a now-broken glass bowl

Was OK until i cranked the heat to 220 C.

macckone - 15-4-2016 at 12:55

Use a copper reflux colum like everyone else. Three foot with intercooler will give nice reflux ratios 3 or 4 :1. The length and diameter are very dependent on heat input. You can get over 80% in a single run from mash and azeotropic on a second run after diluting to 50%. Discard the heads and tails. Primary contaminant is acetyal which gives a butter flavor. You can distill water out of vinegar a setup like this with 10:1 reflux ratios. But SS is better for corrossion resistance as acetic acid will corrode copper.

JJay - 15-4-2016 at 17:06

I've used water-detecting paste that they sell at automotive stores to check for water in ethanol before (it's typically used for checking to see if you have coolant in your oil or water in your gasoline, etc.). Usually I just check the density (that's what ACS and USP suggest).

http://www.distill.com/specs/UK.html

I think you could add a small amount of anhydrous copper (II) chloride and look for a blue/green color to detect water, but I have not tried this... that might be a fun way to spend my Friday night.

Corrosive Joeseph - 22-4-2016 at 05:14

My 300mm stainless tube column packed with a scrubber returned 91% EtOH in one run from my 'moonshine' starting material...........

Testing my 400mm tube soon. More to come....................

arkoma - 22-4-2016 at 06:51

I'm actually NOT drinking it. (Dumbass alert) and after checking my Vogel's (D'uh!!!)(facepalm) CaO, which I have.

XeonTheMGPony - 22-4-2016 at 09:07

*Edit: Clarified statement

Step one: Throw the radio out, it has no place in a lab! Especially when dealing with flammables

Step Two: Hit self very hard with solid object for even thinking of consuming a mind altering substance when working with flammables and setting foot into a lab *(Alcohol consumption + Lab = Darwin award)

Step three: Make a shield around the column but do not directly insulate

Step four: Ditch the oil do as others stated and used distilled water bath (We need very precise temp control here)

Step five: Start with low heat, allow every thing to saturate befor bringing the heat up, the slower you go the higher the purity you get!

All distillations are the same I find, precise temp control and taking your time, and ensuring a clean well lit lab with no distractions and a clear head = high purity results!

Only insulate your fractional column if you simply can not get the head temp to the target with slight increase in the heat source, but if this is required drop the heat source down, let the column balance then insulate a fraction, allow to balance and see where you end up befor increasing the heat source again.

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

[Edited on 22-4-2016 by XeonTheMGPony]

arkoma - 22-4-2016 at 09:14

Quote: Originally posted by XeonTheMGPony

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only $200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad.

*EDIT* And yes, my notes narrate a "comedy of errors". As in, "Don't do it this way". I'm 52 years old and live alone in a detached home. I also know I can screw up.

I hope though that any younger/reckless/new to the hobby members read carefully and therefore don't have as cavalier an attitude.

[Edited on 4-22-2016 by arkoma]

aga - 22-4-2016 at 09:16

Quote: Originally posted by arkoma

CaO, which I have.

Let us know how that works out.

I tried it with oven-dried CaO and didn't get much drying of the EtOH at all.

JJay - 22-4-2016 at 09:19

Molecular sieves work great for removing the last of the water. They are a little pricey, but you can reuse them.

XeonTheMGPony - 22-4-2016 at 09:20

Quote: Originally posted by arkoma

Quote: Originally posted by XeonTheMGPony

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only $200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad.

I used to use huge volumes as a solvent and for fuel so I had a 56gallon feed still! and the reflux was made out of 3" diameter copper with a thermostatically controlled condenser lol.

and it came out at 90% in large volume. But for you doing small batch work I'd make 1L once you get it all set up right and store it some where cool and dry, to get it right in small scale is a royal pain in the rear, well worth making more then you need as you'll regret not doing so.

But the critical point is there is no rushing it, the slower you go with your temp, the finer the finished product, part of that temp control is having a good tight gradient on your column

arkoma - 22-4-2016 at 09:22

Quote: Originally posted by aga

I tried it with oven-dried CaO and didn't get much drying of the EtOH at all.

I plan to take an Oxy-Acetylene torch to it to dry it. Heating to incandescence oughta do the trick. Vogel says DISTILL over CaO.

aga - 22-4-2016 at 10:17

Who is this Vogel dude ?

Bet it's PHDchemist in disguise

Just kidding.

If it's in Vogel's 3rd, it will probably work if done correctly !

(the 'correctly' part tends to trip me up a lot ...)

macckone - 24-4-2016 at 09:57

You can't oven dry CaO. You need extremely high heat and low carbon dioxide.

zed - 24-4-2016 at 15:40

Well, 95% I can buy at my corner liquor store. Not terribly expensive either.

But, Absolute is a very handy reagent, and harder to come by. Molecular sieves, you say? You have done this?

Lately?

macckone - 24-4-2016 at 19:25

I will stick with my epsom salts and potassium carbonate. You need 3A molecular sieves.

aga - 24-4-2016 at 22:48

Quote: Originally posted by macckone

You can't oven dry CaO. You need extremely high heat and low carbon dioxide

I put mine in an oven at ~ 220 C insead of the furnace.

This may easily explain why it didn't work.

[Edited on 25-4-2016 by aga]

Eddygp - 25-4-2016 at 01:25

I would have added some dry (anhydrous) MgSO4 to the alcohol while distilling, as woelen suggested (CaSO4 is more of a hassle, MgSO4 can be easily removed!).
And yes, careful heating ensures efficiency; anti-bumping granules might be interesting if you really are having those problems - remember, safety is key, especially with hot flammable liquids!

JJay - 25-4-2016 at 01:54

I'm distilling some right now from 70% through a 30 cm Vigreux on a water bath. It's pretty slow going (approx 100 mL per hour) and might require another distillation to reach 95%.

Edit: From 950 mL of 70% v/v denatured ethanol, approximately 720 mL of distillate dripped over until nothing more came through the Vigreux. I haven't checked, but I already know that the concentration is pretty close to 95%; I could distill it a couple more times, but I'm just going to dehydrate it.

[Edited on 26-4-2016 by JJay]

arkoma - 25-4-2016 at 11:05

oh, this is "pricy" alcohol for sure. Not the point.

JJay - 25-4-2016 at 19:44

Oh, right, if anyone wants to pay $100/L for anhydrous ethanol, hit me up

[Edited on 26-4-2016 by JJay]

XeonTheMGPony - 26-4-2016 at 03:59

Quote: Originally posted by arkoma

oh, this is "pricy" alcohol for sure. Not the point.

Pure near anhydrous Alcohol is very pricey! Lots of time, energy, material work goes into it on the lab scale.

That is why I do all my high investment synths in larger then needed batches, so when I need it all the work has all ready been don.

Velzee - 26-4-2016 at 06:19

Where'd you get that pin, arkoma?

EDIT: Nevermind.

[Edited on 4/26/2016 by Velzee]

Chemist_Cup_Noodles - 26-4-2016 at 06:38

Hm, dehydrating your alcohols from what I've seen doesn't have to be too pricey. IIRC, you can use magnesium shavings and molecular seives. You might can get magnesium bits for free from a local machinist if you dig around hard enough. And molecular seives can be reusable if you dry them right. So this seems like a good way to go if you can wait a long time.

I found a pretty long JOC Article on drying your solvents that should be of good use: http://ccc.chem.pitt.edu/wipf/Web/Solvent_Drying.pdf

arkoma - 26-4-2016 at 08:16

@chemist_cup_noodles thanx for the paper KOH was never even on my radar.

JJay - 26-4-2016 at 09:33

I wonder how hard it would be to remove ketone denaturants with sodium bisulfite.

I probably shouldn't....

Chemist_Cup_Noodles - 26-4-2016 at 10:21

Quote: Originally posted by JJay

I wonder how hard it would be to remove ketone denaturants with sodium bisulfite.

I probably shouldn't....

If you think you'd feel inclined to test the fruits of your labor personally, maybe you shouldn't. But I'd still it for science (heh). I think it would be a neat experiment to carry out, and quite a fun and interesting process. Kinda like a puzzle. Because in theory denaturants are meant to make the alcohol unfit for consumption, even after distillation or chemical means, but that is certainly untrue. Where there is a will there is a way. So go for it.

JJay - 26-4-2016 at 20:47

I don't think that's a good idea, really... for one thing, it would be likely to leave some sulfur dioxide in the ethanol after distillation (which would require further distillation from, for example, sodium carbonate).

For another, removing denaturants is almost certainly illegal.

XeonTheMGPony - 27-4-2016 at 04:45

Quote: Originally posted by JJay

I don't think that's a good idea, really... for one thing, it would be likely to leave some sulfur dioxide in the ethanol after distillation (which would require further distillation from, for example, sodium carbonate).

For another, removing denaturants is almost certainly illegal.

So is some of the stuff you do in home chemistry and the entire energetics board in some countries

It is the intent that determines if it is illegal IMO, and that is how our legal system mostly works too (Canada) SO if he where doing it to sell then yes, but just purifying a reagent for usage at home no.

It wouldn't be worth the cost for any one of concern to hassle him.

JJay - 27-4-2016 at 05:11

Eh, I follow the law. Technically, when distilling denatured ethanol without a license, you have to be recovering it from some other process, which is why I wiped my *ss with it before distillation (I left out that part), but I'm in the clear here.

Chemist_Cup_Noodles - 27-4-2016 at 06:12

Quote: Originally posted by XeonTheMGPony

Quote: Originally posted by JJay

Well but why would you get "busted" for doing this? As long as you're not buying gallons and gallons of denatured alcohol or trying to sell your de-denatured product, I don't see where any issues should arise. If you're worried about neighbors seeing you doing experiments and calling the police, I wouldn't be. I live in the suburbs and I've done some experiments in my back yard (I lack a fume hood and I don't want to burn my house down), and no one has ever said anything other than just being curious about my "lab equipment". So as long as it doesn't look like you're running a huge meth operation, I really wouldn't worry about following the law perfectly. But worst case scenario, for some random reason if the police found out that you removed denaturant from just a small amount of alcohol, they give you a ticket and a small fine for doing it without a license.

The Volatile Chemist - 30-4-2016 at 09:32

I do stuff in the backyard. One house adjoining ours is unoccupied, one is a close friend of the family who couldn't be suspicious of me, and the other two *I'm* suspicious of, so I don't worry too much. I've also told friends of my lab, and had to deal with guidance counselors on the subject, so I'm slightly experienced in dealing with such...

Refinery - 8-5-2016 at 05:20

Last year I used to distill 92-95% EtOH with 2" stainless steel wool packed active reflux still so it is doable, but it could require extensive steps with small scale glassware. The odorous and tasteous properties of the product will improve significantly if it is to be processed with activated carbon and sodium carbonate at 50% dilution after first concentrative distillation and redistilled.

[Edited on 8-5-2016 by Refinery]

Corrosive Joeseph - 31-5-2016 at 22:36

Quote: Originally posted by Refinery

Last year I used to distill 92-95% EtOH with 2" stainless steel wool packed active reflux still so it is doable, but it could require extensive steps with small scale glassware. The odorous and tasteous properties of the product will improve significantly if it is to be processed with activated carbon and sodium carbonate at 50% dilution after first concentrative distillation and redistilled.

[Edited on 8-5-2016 by Refinery]

Could you explain your process a little please................?

Corrosive Joeseph - 1-6-2016 at 23:18

Sorry for the double post, l can't edit....................

As l promosed l would report back with results so here goes....................

58% ran through the 300mm length 30mm dia stainless steel tube column stuffed with half a scrubber yielded 91%

58% ran through a 500mm length 32mm dia stainless steel tube column stuffed with a full scrubber yielded 91%

91% ran through the 500mm column once again yielded about 93.5%.....................

Comments and criticisms welcome please =)

CJ

[Edited on 2-6-2016 by Corrosive Joeseph]

careysub - 2-6-2016 at 11:48

Wouldn't the fact that KOH is soluble in ethanol be a problem?

arkoma - 25-6-2016 at 13:43

UPDATE.

Having made a few slight procedural changes, I have reached 92% via distillation. I used about 10 feet of 10ga copper wire cut into short pieces and bent in curlicues. These I used to pack a claisen adapter. Hit an old dinner plate with a hammer and voila, boiling chips. Also swapped out the oil bath for a water bath.

The packed claisen works much better than my 300mm Vigreux. I see an "old school" fractionating column on my shopping list.........

I have approx 450ml of the 92%, and am planning to distill it over CaO. If I can beat the azeotrope by even one or two percentage points the whole Ark-La-Tex will hear my whoops of triumph.

aga - 25-6-2016 at 14:13

Using some kind of reflux column is much Smarter than not doing.

A stripping run, collecting everything up to around 88 C never hurts, followed by a temperature-specific run where you Only collect everything at 78~79 C, provided that the thermometer is calibrated.

That was todays' fun !

If it had to be gehtto'd and azeo++ on the second run, i'd use the Thumper idea and part-fill the thumper with oven dried tripotassium phosphate.

Since my first attempt at tri-pot-phos i have not been able to successfully make it again.

I am pretty sure the 'pure' KOH i bought from some dodgy geezer in a Turkish kasbah is actually KOH/KCl mixed, which seems to screw it up.

My original batch of KOH was from a much more reputable source, but got used up in the first tri-pot-phos experiments.

Some A3 molecular sieves arrived yesterday.

How to dry and test them for 'activity' ?

Well, stick them in the oven at 250 C for 3 hours and see what happens.

Result : They get hot.

After being allowed to cool for 10 minutes, they were warm, but easy to handle, so a couple of spatulas were held in the expendable left GLOVED hand and a squirt of water was put on them from the wash bottle (found that test embedded in some discourse on how to dry sieves).

They immediately got too hot to be safe, and were thrown with great speed into the void.

This apparently signifies that :-

a) these molecular sieves are indeed 'activated' by 3 hours at 250 C

b) i have less molecular sieves now

arkoma - 25-6-2016 at 14:30

92% was achieved on the third run.

My starting "substrate" this time around was wine made from Ar-Kin-Saw blackberries and Montrachet yeast. My Chinese thermometers ain't that accurate, so first run I kept everything up til about 90c. That yielded 50% EtOH. Second run I did by VOLUME, 500ml in the flask, discarded the first 30ml, and kept the next 200ml. There were a lot of "second runs", but not as many as it took to gather up an appreciable qty of 50% (I am limited as my biggest RBF is 1000ml). Second run was averaging about 80% EtOH. Slow careful fractionating through my packed claisen on the third run got me to 92%. My Chinese thermometer sat rock steady at 82c (like I said, not real accurate).

edit--spelling
Not "ghettoing". I can BUY 95% Everclear for WAYYYYY less time and money. But where is the fun in that?

[Edited on 6-25-2016 by arkoma]

aga - 25-6-2016 at 14:47

Calibrate your thermometers maybe ?

Glass of water with lots of ice, thermometer should read 0 C.
Whatever the reading is, y1 = 0, x1 = the thermometer reading.

Boil some water, thermometer should read 100 C.
Whatever the reading is, y2 = 100, x2 = the thermometer reading.

Mathematically, if y is the actual temperature and x is what the thermometer says, then :
$$y = mx + c$$
If you do the algebra, it works out that
$$m = \frac {y2 - y1}{x2-x1}$$
In this case y2=100 and y1=0 so we can simplify it to :
$$m = \frac {100}{x2-x1}$$
$$c = 100 -mx_2$$
Once you know the 'm' and 'c' values for that particular thermometer, you can easily work out the accurate exact temperature based on what it reads by feeding the x (thermometer reading) back into the equation :
$$y = mx + c$$
... y being the actual exact temperature, no matter how 'wrong' the thermometer reading seems.

Any thermometer, especially a digital thermometer for a few bucks off ebay still needs calibrating in this way if you want it to be accurate.

[Edited on 25-6-2016 by aga]

hyfalcon - 25-6-2016 at 18:04

Don't forget to allow for altitude differences. 300 ft above sea level will make a big difference when compared to 7500ft.

macckone - 25-6-2016 at 18:25

At 7500 the azeotrope has about 96% alcohol.

The Volatile Chemist - 26-6-2016 at 18:59

Huh, so starting a lab at a certain, different than average altitude could let you produce better than standard azetrope...

Why waste such fine wine? What happened to using cane sugar and tomato paste?