Chemistry help (Manganese Dioxide)

Distillation methods and improvements.

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muckanic
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Re: Chemistry help (Manganese Dioxide)

Post by muckanic »

helmingstay wrote:Is the concern that there are minor amounts of contaminants that could potentially volatilize, or contaminants that could react in the pot? I'm a little confused.
I'm concerned about who's concerned here. :) I thought you originally raised the issue of fragrance volatility. The surfactants probably don't matter too much, except that they could potentially suppress various boiling points.
A quick search shows that any H2O2 you can buy is *not* pure. All sorts of weird things added to stabilize H202. And H2O2 in any concentration is pretty nasty stuff. And buying it from the drugstore at 3% by the quart sounds expensive, not to mention that it adds needless water that's going to be stripped out anyway.
Except that in the context of cleaning up vodka brews the wash would be alkalised anyway, so not much difference with the percarbonate approach. It's a while since I took a look, but I can't remember the peroxide stabilisers being particularly nasty. A bit of silver, or something like that? Actually, I don't want to know the answer, because I added a small amount to a drink recently in a fit of experimentation.
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Re: Chemistry help (Manganese Dioxide)

Post by pHneutral »

helmingstay wrote: Making oxygen via electrolysis? *Really* bad idea:
1) Extraordinary waste of electricity ( @ 65% efficiency, something like 10 kWh/Nm3? I ripped some specs from here - http://www.global-hydrogen-bus-platform ... ectrolysis" onclick="window.open(this.href);return false;" rel="nofollow)
2) Hydrogen is explosive. Oxygen only makes it more so...
3) Electricity + water can be dangerous for the inexperienced
4) Cost of electrodes?
5) Common electrolytes are dangerous chemicals: "The electrodes are placed in an ion-conducting electrolyte (usually an aqueous alkaline solution with 30 % potassium hydroxide KOH)."

I agree, KMnO4 seems pretty sketchy. Baking soda, on the other hand, is tried and true and, to my palette, tasty. Sodium percarbonate seems much closer to the "do no harm" end of things...
Mate, if you're taking off O2 from electrolysis, you, of course, run it through wash bottles to remove any contaminants. I didn't specifically mention that here, but if someone really wanted to try it, they should (I would hope) research it and find that out.

Yes its a waste of electricity. But it works, is simple and quiet, and you don't need tanks.

KOH is used by the kg by soap makers to no ill effect, and that gets put ON your body. You won't get KOH coming off a solution of it just by electrolysing water.

As far as the explosion hazard, you just need to do it with a divided cell. Vent the H2 to the air (its not much and won't go boom, as long as you think about venting.. and its lighter than air so it will float away).

The ethanol is a FAR more dangerous fire/explosion hazard than the tiny amount of H2 involved in this.

Anyhow, it is a boiler plate idea. Sodium percarbonate might be just the ticket. I dont know. We'd have to get a field report to find that out :) There are definitely easier ways to make O2 chemically, if people wanted to generate their own, than electrolysis. I just thought I'd put that idea out there.
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Re: Chemistry help (Manganese Dioxide)

Post by helmingstay »

muckanic wrote: I'm concerned about who's concerned here. :) I thought you originally raised the issue of fragrance volatility. The surfactants probably don't matter too much, except that they could potentially suppress various boiling points.
Sorry - I was trying to say, *assuming there are no fragrances*, blah blah blah.

Do surfactants and/or salts supress the boiling point of water more than ethanol? For salt, I would assume it's an entropic factor of concentrating the ions in the remaining water, with the ions having most of their interactions with the water and less the ethanol. I'd assume the per-gram effect of surfactants would be comparatively low, only one hydrophilic site per long, heavy molecule...
muckanic wrote: Except that in the context of cleaning up vodka brews the wash would be alkalised anyway, so not much difference with the percarbonate approach. It's a while since I took a look, but I can't remember the peroxide stabilisers being particularly nasty. A bit of silver, or something like that? Actually, I don't want to know the answer, because I added a small amount to a drink recently in a fit of experimentation.
Sorry again, i should point out that i consider re-distillation to be assumed after the addition of anything other than water, oak and other plants, carbon, oxygen... anything i'm missing here?

Still, if it came from the drug store and it doesn't have a big red warning, then it surely won't kill you in small doses ;)

R.e. liquid H2O2 stabilizers, this interesting bit from http://www.h2o2.com/intro/faq.html" onclick="window.open(this.href);return false;" rel="nofollow -
"The types of stabilizers used in H2O2 vary between producers and product grades. Colloidal stannate and sodium pyrophosphate (present at 25 - 250 mg/L) are the traditional mainstays, although organophosphonates (e.g., Monsanto’s Dequest products) are increasingly common. Other additives may include nitrate (for pH adjustment and corrosion inhibition) and phosphoric acid (for pH adjustment). Certain end-uses -- which depend on the bleaching ability of H2O2 in alkali – utilize colloidal silicate to sequester metals and thereby minimize H2O2 decomposition. "
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Re: Chemistry help (Manganese Dioxide)

Post by helmingstay »

pHneutral wrote: KOH is used by the kg by soap makers to no ill effect, and that gets put ON your body. You won't get KOH coming off a solution of it just by electrolysing water.

As far as the explosion hazard, you just need to do it with a divided cell. Vent the H2 to the air (its not much and won't go boom, as long as you think about venting.. and its lighter than air so it will float away).

The ethanol is a FAR more dangerous fire/explosion hazard than the tiny amount of H2 involved in this.
The OH from the KOH is consumed in the reaction, so it's not present in soap. KOH itself can blind you in the, um, blink of an eye. I'd say that soap-making is more dangerous than moving ethanol fumes around inside an oxygen-free container, personally... :)

And don't forget that you're making twice as much H2 as O2!
pHneutral wrote:Sodium percarbonate might be just the ticket. I dont know. We'd have to get a field report to find that out :)
I'm on it :)
I'll try to do a small batch parallel, with and without, holding all else as equal as possible. If i can just get away from this screen...
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Re: Chemistry help (Manganese Dioxide)

Post by pHneutral »

The OH from the KOH is consumed in the reaction, so it's not present in soap. KOH itself can blind you in the, um, blink of an eye. I'd say that soap-making is more dangerous than moving ethanol fumes around inside an oxygen-free container, personally...
Well so can boiling hot oil that spatters on you, but people handle that pretty well when they are deep frying a turkey (usually). And all you have to do when handling KOH is wear some safety goggles and/or a spatter guard plus gloves, long sleeves, long pants.

All I am saying is that if you understand the nature of what you are working with, there are not likely to be any troubles. And there are an awful lot of people using KOH to make liquid soap out there, and they handle it ok.

I dislike the idea that dangerous things are less desirable to use for some things merely because there is a chance someone will make a stupid mistake and hurt themselves. I'd rather err on the side of personal responsibility, and give people the information they need to do things safely.. then.. when they don't.. its their own damn fault. :)
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Re: Chemistry help (Manganese Dioxide)

Post by helmingstay »

pHneutral wrote: Well so can boiling hot oil that spatters on you, but people handle that pretty well when they are deep frying a turkey (usually).
I generally agree...

But both knowledge *and* precautions are required. Over the years, I've had many friends that work in commercial kitchens who are extremely knowledgable of the dangers of hot oil from repeatedly burning themselves - high speed and lots of safety shortcuts.
pHneutral wrote: And all you have to do when handling KOH is wear some safety goggles and/or a spatter guard plus gloves, long sleeves, long pants.
And use common sense - move slowly, think about what you're doing, etc. This is the one most people miss...

When in doubt, consult google:
http://www.google.com/search?q=%22turke ... ccident%22" onclick="window.open(this.href);return false;" rel="nofollow
Yup. It happens more than none... Results 1 - 10 of about 172 for "turkey frying accident"

I think of this forum as a "informational reference book" for the future. It's our responsibility here to clearly name dangerous compounds and activities as such, and leave readers with the responsibility of appropriate preparation. KOH *is* dangerous, and the damage it causes can be permanent. Statistically, frying a turkey has a non-zero risk of catastrophe; driving a car has a much higher risk of catastrophe (especially if you're a male under 25 in a red sports car...).

I'm *not* saying folks shouldn't fry turkeys or make soap, or drive.

I *am* saying we should be clear of the risk. Is a small risk of death worse than a large risk of loosing a finger? That's up for the operator to decide...

As far as i can tell, the most probable and most serious risk of distillation is legal. Are there modern examples of still explosions or catastrophic fires at the home-brew scale (i'm not considering industrial-scale operations here)?
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Re: Chemistry help (Manganese Dioxide)

Post by muckanic »

pHneutral wrote:Mate, if you're taking off O2 from electrolysis, you, of course, run it through wash bottles to remove any contaminants. I didn't specifically mention that here, but if someone really wanted to try it, they should (I would hope) research it and find that out.

KOH is used by the kg by soap makers to no ill effect, and that gets put ON your body. You won't get KOH coming off a solution of it just by electrolysing water.
KOH isn't necessarily required. The anolyte needs to be polar enough to provide good conductivity, alkaline to balance the OH- that is consumed in the reaction, and not to contain anything that will oxidise in preference to the water. The latter requirement also applies to the anode, so some sort of noble metal would normally be employed. I would have thought that you could get away with a less caustic anolyte, possibly in addition to some sort of salt to improve conductivity. I also can't think of too many noxious gasses that might be generated in the anode compartment and which might require trapping. Just in case, it would probably be an idea to avoid Cl- salts in the anolyte.
As far as the explosion hazard, you just need to do it with a divided cell. Vent the H2 to the air (its not much and won't go boom, as long as you think about venting.. and its lighter than air so it will float away).

The ethanol is a FAR more dangerous fire/explosion hazard than the tiny amount of H2 involved in this.
The simple response is to ensure that something besides the H+ gets reduced in the cathode compartment. Eg, use a cathode with a high hydrogen over-voltage (like Pb), in conjunction with something like Cu salts in the catholyte.
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Re: Chemistry help (Manganese Dioxide)

Post by muckanic »

helmingstay wrote:Do surfactants and/or salts supress the boiling point of water more than ethanol? For salt, I would assume it's an entropic factor of concentrating the ions in the remaining water, with the ions having most of their interactions with the water and less the ethanol. I'd assume the per-gram effect of surfactants would be comparatively low, only one hydrophilic site per long, heavy molecule...
We had a thread a while back on the use of salt to improve water-alcohol separation, and there were a surprising number of naysayers. My view was that it should work because salt is more soluble in water than alcohol. Re surfactants, what I was trying to say yesterday in a garbled fashion was that they might grab onto the organics and raise their boiling point. But of course that doesn't make much difference if the water boiling point is raised by a similar amount. So it comes down to a question of which substance has the greater affinity and I don't know the answer for sure, except to flag that this is a potential downside of retail oxy-bleach treatment. OTOH, it could be an upside. :)
R.e. liquid H2O2 stabilizers, this interesting bit from http://www.h2o2.com/intro/faq.html" onclick="window.open(this.href);return false;" rel="nofollow -
"The types of stabilizers used in H2O2 vary between producers and product grades. Colloidal stannate and sodium pyrophosphate (present at 25 - 250 mg/L) are the traditional mainstays, although organophosphonates (e.g., Monsanto’s Dequest products) are increasingly common. Other additives may include nitrate (for pH adjustment and corrosion inhibition) and phosphoric acid (for pH adjustment). Certain end-uses -- which depend on the bleaching ability of H2O2 in alkali – utilize colloidal silicate to sequester metals and thereby minimize H2O2 decomposition. "
I should have bothered to look up peroxide stabilisers yesterday, because silver is the complete opposite. The practical issue is whether relatively small amounts of stabiliser are better or worse for distilling than relatively large amounts of surfactants, fragrances and possibly other stuff in retail oxy-bleach? Dunno for sure, except that fragrance would definitely be one to avoid if possible.
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Re: Chemistry help (Manganese Dioxide)

Post by helmingstay »

muckanic wrote: We had a thread a while back on the use of salt to improve water-alcohol separation, and there were a surprising number of naysayers. My view was that it should work because salt is more soluble in water than alcohol. Re surfactants, what I was trying to say yesterday in a garbled fashion was that they might grab onto the organics and raise their boiling point.
Ahhhh, yes, I see.

So, I a small batch "experimental" run of some really smelly stuff. I can't make detailed comparisons until i do the "control" run of the other half of the really smelly stuff, but I can make some initial observations.

Set-up:
I tested pH with 2-12 paper. The initial pH of the low wines was about 7, initial ABV ~ 55%, initial volume ~1gallon, stainless pot, copper vapor-path, electric stove, 1500-2000 watts? My elevation is ~5000 feet, so water boils at ~202degF here. A small analog thermometer sat in the lid of the pot, extending into the fluid at the beginning of the run, just vapor probably about half-way through.

I added 2 Tablespoons "one-step" cleaner (manufactered by LOGIC, commonly sold in homebrew stores... I've been trying to track down the exact ingredients with no luck).
It had very low solubility in room-temp low wines. Maybe 50% solubility at 130degF.
At this point, pH was high, 10 or 11 maybe? I stirred then, and closed up the pot.

pH of distillate was 7.

pH of the slop/left-overs was very high, 12+. It had an almost perfumy smell. All the one-step was dissolved. No signs of damage to the kettle. There were a few crystals that had deposited that dissolved in hot water.

The thermometer followed the curve i'm used to seeing - i didn't see a noticeable water boiling point depression from this run, but i can't read more than +/-2degF.
muckanic wrote: The practical issue is whether relatively small amounts of stabiliser are better or worse for distilling than relatively large amounts of surfactants, fragrances and possibly other stuff in retail oxy-bleach?
I'm leaning towards the use of oxo brite for my general brewing/cleaning needs due to clearly labeled ingredients - Sodium percarbonate and sodium carbonate. It's decently priced, too. I'm still unsure how it's performance compares to one-step. Product link here: http://www.ecos.com/pages/oxo.html" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Chemistry help (Manganese Dioxide)

Post by muckanic »

helmingstay wrote:So, I a small batch "experimental" run of some really smelly stuff. I can't make detailed comparisons until i do the "control" run of the other half of the really smelly stuff, but I can make some initial observations.
The problem is that you may wind up demonstrating nothing more than that Na2CO3 is good stuff for cleaning up vodka, which is already established. The essential issue to be tested is whether oxidation, either controlled or uncontrolled, does more good than harm (as in formation of extra aldehydes and loss of yield, maybe some lipid rancidity that sneaks across).
I'm leaning towards the use of oxo brite for my general brewing/cleaning needs due to clearly labeled ingredients - Sodium percarbonate and sodium carbonate. It's decently priced, too. I'm still unsure how it's performance compares to one-step. Product link here: http://www.ecos.com/pages/oxo.html" onclick="window.open(this.href);return false;" rel="nofollow
As a combo cleaner/sanitiser, I find unscented retail oxy-bleach beats liquid household bleach hands-down (no smelly fumes, rinses easier, sanitisation capability doesn't degrade as fast and possibly works better under alkaline conditions, surfactant improves cleaning capability). For the sake of balance, however, some folks don't seem to accept that peroxide actually functions as a sanitiser, and others think the surfactants in iodophor aren't a problem with no-rinse approaches. PS: if your oxo stuff foams, then it contains surfactants, regardless of what the ingredients label might say.
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Re: Chemistry help (Manganese Dioxide)

Post by mjstorm »

I am from Ukraine. My English not so good (Russian, however too) But I gradually read your forum from last year. And it to me
Very to be pleasant. I am engaged many years in alcohol distillation.
I have experience. About chemical clearing of alcohol I can tell
The following: it is not necessary to be afraid of it. I and other people use It many years without harmful consequences are successful.
For translate I used the computer program, and if you
The text understand, I can give you our recipe
Chemical clearing of alcohol.
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Re: Chemistry help (Manganese Dioxide)

Post by HookLine »

Hi mjstorm

Welcome, and thanks for your comments. Have you got some links to stuff we can look at?

Cheers
Hook
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Be discreet.
And have fun.
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Re: Chemistry help (Manganese Dioxide)

Post by mjstorm »

The chemical method of clearing is based on interaction between molecules alcohol and a brought reactant.
Are as a result formed new substances of which it is possible to get rid repeated distillation.
As a result of numerous researches in spirit industrial production
Have decided to make clearing by such substances:
Soda NaOH
Soda Na2CO3
Kalii permanganas KMnO4
If you suppose use of these chemical substances I can continue the story.
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Re: Chemistry help (Manganese Dioxide)

Post by HookLine »

Soda NaOH =sodium hydroxide
Soda Na2CO3 = sodium carbonate
Kalii permanganas KMnO4 = potassium permanganate (Condy's crystals)

Please continue.
Be safe.
Be discreet.
And have fun.
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Re: Chemistry help (Manganese Dioxide)

Post by mjstorm »

I have attentively read notes about chemical clearing of alcohol on your site
and at a forum. Many correct statements about use of soda and other substances.
But I have not found in one note of the whole system of clearing of alcohol.
I do not wish to repeat the information which you have. I actively pressed button "Search", but can have not seen.
If there is such information, give links please..
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Re: Chemistry help (Manganese Dioxide)

Post by HookLine »

You are correct. This forum has no information on a whole system of chemical clearing or cleaning of alcohol. We only use Na2CO3 or NaHCO3.

Explain your system. This is new information for us.
Be safe.
Be discreet.
And have fun.
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Re: Chemistry help (Manganese Dioxide)

Post by mjstorm »

Excuse, that so long was silent.
At our people it is a lot of holidays and after Easter. In a week
аfter Easter recollect the died relatives and friends, in three days - parents,
and then - on May, 1-2-3st the international Day of workers, these days have fun and spend picnics.
It is natural, that after these days very difficult to get fingers on the keyboard.
I will begin gradually.

Spirit which turns out after distillation we name crude spirit or spirit-raw. It has approximately 60 %-70 % of pure spirit. (Pure spirit-96,4 of %)
This product of distillation also should be processed chemical substances.
The first.
It is necessary to define acidity of crude spirit. It can be made with the help pH-metre or a litmus paper.
If acidity is less 5 processing by soda is necessary Na2CO3. Soda dilute with the distilled water and a solution add in spirit, supervising pH.
The product received thus will have рН 6,5.
After that it can be processed KMnO4.
to be continued
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Re: Chemistry help (Manganese Dioxide)

Post by athiril »

Sorry to dig up an old thread but..

helmingstay wrote:
muckanic wrote:I suspect finding purish H2O2 would be easier than finding pure percarbonate. With any luck, liquid peroxide stabilisers wouldn't muck too much up.
I checked a package of Oxo Brite (http://www.ecos.com/pages/oxo.html" onclick="window.open(this.href);return false;" rel="nofollow) this morning, and there are 2 ingredients listed: Sodium Percarbonate and Sodium Carbonate. Is the concern that there are minor amounts of contaminants that could potentially volatilize, or contaminants that could react in the pot? I'm a little confused.

A quick search shows that any H2O2 you can buy is *not* pure. All sorts of weird things added to stabilize H202. And H2O2 in any concentration is pretty nasty stuff. And buying it from the drugstore at 3% by the quart sounds expensive, not to mention that it adds needless water that's going to be stripped out anyway.
muckanic wrote: None of this constitutes endorsement of the whole notion that chemical oxidation reduces congeners. :o
Fair enough :)
Anyone qualified to comment?

IF that is a problem, dissolve it in water, boil/dry it back down to a salt.

Or get food grade bicarb soda, heating it will decompose it into sodium carbonate. I recommend bicarb soda over carbnate though, carbonate produces carbon monoxide (tasteless, clear, odourless) upon reaction with ketones and aldehydes which is soluble in ethanol.




andre.silent wrote:Hi,

I am not good enough in organic chemistry to give any scientific explantion but I remember that aldehydes are considered to be reduction agents while alcohols are not (therefore aldehydes must get oxidised easier than alcohols).

You need to post a source for this, since adlehydes are the oxidised product of alcohols, higher oxidised states become harder to oxidise than lower oxidised states since they're higher in oxidation already, unless there is some other favourable condition.

KMnNO4 reacts with alkenes in an alkaline solution to form glycols, and aldhehydes are favourable in oxidation to ketones, as they are easier to oxidise.


Apparently silver oxide will also only oxidise aldehydes.


The few non-detailed sources I can find suggest Aldehydes are easier to oxidise than Alcohols.

Hope this of some research/experimental value.
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Re: Chemistry help (Manganese Dioxide)

Post by mjstorm »

Those interested in many new moonshiners. I've been this way.
But after a comparative tasting beverages that have been processed in chemistry and without it - refused to chemistry.
The odor worse. Even with a good distillation of a long column with good separation.
I do not want to replace the well-known to unknown impurities.
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Re: Chemistry help (Manganese Dioxide)

Post by athiril »

NaOH on its own will make aldehydes and ketones undergo aldol reactions into aldols.

It'll also make esters (like ethyl acetate) under go hydrolysis back to their alcohols + sodium acetate.


So I see KMnO4 as kind of useless, unless it has a preferred order of reactions among the alcohols.

IIRC it does react with secondary alcohols (to ketones) first before primary alcohols.. which means you can use it with NaOH to knock out fusels (Secondary only though, not tertiary) out of tails if you save them for re-distillation later

What would be important to know though, is if it had a reaction order for primary alcohols based on molecular weight. I've asked about this order elsewhere to see if I can get an answer. If the preferred reaction was to oxidise heavier molecular weight alcohols first, it would also help with primary alcohol fusels.. and anything above ethanol.
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Re: Chemistry help (Manganese Dioxide)

Post by athiril »

I just thought that if anyone wans to play around with this, then ascorbic acid would be a good way to neutralise excess NaOH and KMnO4, as it's also a powerful anti-oxidant, though you should not end up with excess oxidiser, but it'll take out lower products formed that have oxidising power but cant oxidise alcohol.
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Re: Chemistry help (Manganese Dioxide)

Post by docdave »

Guys,

I have quite a bit of experience in a lab setting and all this talk of using MNO2 and KMnO4 kind of scares me a bit. Both of these substances are powerful oxidants and can accelerate a 'safe' chemical reaction like making ethanol into an extremely dangerous event. One of my colleagues managed to blow up a lab with MnO2. Lots of off the cuff talk on this thread and lots of questionable safety here. Fermentation is a natural event and we should treat it as such. Turbos produce lots more ethanol product but I don't everyone using turbos because the results are bad. I take advice from the master distillers here and they just don't advocate using all these extra chemicals. The big guys do but they have trained chemists closely monitoring the situation with the necessary monitoring equipment in place. I am trying to keep everything as natural as possible because I'm trying to avoid the shortcuts the big guys need for profits and focus more on a quality product. Also, do you need really need to be making a potential bomb in your garage. Try explaining that one to your insurance man when your house is leveled!

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Re: Chemistry help (Manganese Dioxide)

Post by Husker »

I agree with DD here. Talk of chemical processes such as this HAVE NO PLACE in a home distillation forum.

athiril, please abstain from trolling up dead topics, just to hear yourself spout. Topics die for many reasons. This one was dead.

H.
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