Sciencemadness Discussion Board

Druken Aga Challenge (DAC) #3 - Closed (but open to discussion)

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blogfast25 - 30-10-2015 at 18:15

@agari: using anything already nitrated as raw material is against the competition's rules as well as spirit.

Wake up and smell aga's fart.

Quote: Originally posted by aga  
Ooooh !

Sulphuric acid and a Nitrate Salt !

I fart in your general direction.

Agari - 30-10-2015 at 19:29

Quote: Originally posted by j_sum1  
Ok. But it still does not qualify as a novel route. Convenient? yes. Novel? no.
Prohibited within the terms of the competition? you'll need to ask aga that. But I would read into his above comment that something a bit more adventurous is required. After all, it is a hefty prize pool and I think you have to earn it.


Updated the procedure, I didn't "refine" it yet,but the chemicals it calls for should be readily available.

Agari - 30-10-2015 at 19:32

Quote: Originally posted by blogfast25  
@agari: using anything already nitrated as raw material is against the competition's rules as well as spirit.

Wake up and smell aga's fart.

Quote: Originally posted by aga  
Ooooh !

Sulphuric acid and a Nitrate Salt !

I fart in your general direction.


My procedure actually specifies how to make the nitrate salt.

Sidenote:Is it just me or is Aga's promise of over 309 American dollars very fishy and we are being trolled?

MolecularWorld - 30-10-2015 at 19:35

It looks like you copied most of your ideas (and the copper sulfate picture) from NurdRage. Have you actually tried any of this? I'm sure original photos, perhaps even videos, will be required to claim the prize.

[Edited on 31-10-2015 by MolecularWorld]

As for the amount of the prize:
Quote: Originally posted by aga  


Prize fund Increased to 500 Euros.


[Edited on 31-10-2015 by MolecularWorld]

blogfast25 - 30-10-2015 at 19:40

Quote: Originally posted by Agari  


My procedure actually specifies how to make the nitrate salt.

Sidenote:Is it just me or is Aga's promise of over 309 American dollars very fishy and we are being trolled?


Are you just obtuse or is it you who that's trolling?

Quote: Originally posted by Agari  
Materials:
1 Instand cold pack (Either 86g of calcium ammonium nitrate or just 70g of ammonium nitrate), but not urea.
75g of potassium chloride bought at a grocery store.


Shop bought CAN. That's a NITRATE, idiot.

So is nitrate found in composted materials.

The money's real but you're unlikely to get a dime of it. Or start documenting your procedure as required in the opening post.


[Edited on 31-10-2015 by blogfast25]

deltaH - 31-10-2015 at 02:39

Okay, time for another potential hypothetical idea open for anyone to try...

Earlier jsum1 tried the destructive oxidation of urea using calcium hypochlorite and lime. It seems to fail because of the formation of explosive nitrogen chlorides, but it did succeed at destructively oxidising urea, so I am thinking of a non-chloride version.

One version is to scrounge out some manganese dioxide from a couple of new torch cells, filter and wash the dark powder and dry it. Then mix it with whatever the most concentrated sulfuric acid you can get and add urea. Then attach a condenser and distill off [hopefully] nitric acid and be left with manganese sulfate hydrate in the flask which can be recycled back as ingredients using electrolysis and carbon electrodes.

The hypothetical reaction is:

8MnO2(s) + (NH2)2CO+ 8H2SO4(l) + heat => 2HNO3(g) + CO2(g) + 8[Mn(SO4).(1.125)H2O](s)

WARNING: This is a novel untried hypothetical reaction! It should be trialed in very small amounts initially to ascertain if it's safe to carry out!

aga - 31-10-2015 at 02:43

Now that's much more like it !

How clean/concentrated would the H2SO4 need to be ?

Would used battery acid work ?

deltaH - 31-10-2015 at 03:39

Purity isn't too much of an issue as you're expected to distill off the nitric acid as it forms, so if the sulfuric acid is too weak, the first portion of the distillate may be mostly water and so this would be discarded until the good stuff comes over. Long story short, battery acid should be fine :D

I've done a reaction between urea and two equivalents of 40wt% sulfuric acid that after much boiling down results in a sudden vigorous effervescence (CO2) that forms a crystalline product upon cooling to RT. I hypothesised this to be the double acid salt (NH4)HSO4.[(NH2)3C]HSO4.2H2SO4, but that reaction only kicks in at quite high temperature and when most of the water has been driven off, so I expect the urea to be oxidised by the MnO2 much before that (hopefully).

When I first thought up this idea, I was thinking of reacting *that* acid salt with MnO2, but then thought that it would be simpler to do it with urea straight. However, that is a variation that might be tried, especially if you want to pre-concentrate dilute sulfuric acid.

Anyway, the urea version should do something, we can refine it further after we know what happens.

[Edited on 31-10-2015 by deltaH]

deltaH - 31-10-2015 at 03:50

BTW, the nice thing about MnO2 is that it's a known catalyst for ammonia oxidation (as per the article I attached a long time ago on this thread), so it seems like a good oxidant to use in a wet chemical approach. Strong sulfuric acid would greatly increases its oxidation strength so that I would reasonably expect NOx or HNO3 to distill off at high temperature.

Furthermore, the acidic conditions ensure that ammonium nitrate is not formed, but nitric acid. Also manganese sulfate is very hygroscopic, so it ought to mop up some of the water formed by the reaction.

[Edited on 31-10-2015 by deltaH]

j_sum1 - 31-10-2015 at 03:50

Interesting. I like the idea of urea as a source as it is so easy to get. H2SO4, not so easy round here. HCl and oxalic are readily available though. Not sure that helps. Still, if we are after a new route, it is food for thought.

The African Process

deltaH - 31-10-2015 at 04:25

Just remember, you only need to get a little the first time, because you can easily electrolyse manganese(II) sulfate solutions back to manganese dioxide and sulfuric acid!!!

In a recycling process, the overall ingredients are just urea, heat, water and electricity making carbon dioxide, hydrogen and nitric acid.

The African Process.JPG - 34kB

[Edited on 31-10-2015 by deltaH]

j_sum1 - 31-10-2015 at 04:39

Genius.
I lovr the way the carbon violates the law of conservation of mass. :D

deltaH - 31-10-2015 at 04:44

Oops, forgot to include that :mad: I'll correct the graphic thanks!

... now with fewer carbon credits :D:D:D

The African Process.JPG - 38kB

[Edited on 31-10-2015 by deltaH]

Pourbaix diagrams... again!

deltaH - 31-10-2015 at 05:20

Okay, thought I'd check out some pourbaix diagrams to see if this is feasible.

MnO2 at a pH of -1 (10M H+ conc.) has an oxidation potential of about +1.3V.

For nitric acid extrapolated at the same pH, it's around +1.2V, so it ought to proceed with strong heating, just-just.

Manganese pourbaix:
http://www.sciencemadness.org/talk/files.php?pid=425582&...

Nitrogen pourbaix:
https://upload.wikimedia.org/wikipedia/commons/c/c9/Pourbaix...

[Edited on 31-10-2015 by deltaH]

arkoma - 31-10-2015 at 05:52

Quote: Originally posted by Agari  


Sidenote:Is it just me or is Aga's promise of over 309 American dollars very fishy and we are being trolled?


He's good for EVERY bit of it, trust me I know from personal experience his generosity. And in case ya didna know AMMONIUM NITRATE IS a nitrate fertlizer. Not just for shake and bake. Every slice of bread you eat depends on it.

*edit* misspelled ammonium

[Edited on 10-31-2015 by arkoma]

aga - 31-10-2015 at 08:55

It's $550 US at today's exchange rates, and yes, it's Real.

Forget any notion of 'fair' or 'organised' - it is what it says in the title - a Drunken Challenge, so the Rules are not enforceable, and could change.

Basically i'll pay out if someone comes up with something more interesting than just
"Hey ! New Idea ! Distill a Nitrate Salt with Concentrated Sulphuric acid !"

Someone better come up with something soon or i'll have to post the process the lizard aliens use and win it myself so we can get on with DAC#7 - AntiGravity.

Agari - 31-10-2015 at 11:08

Quote: Originally posted by aga  
It's $550 US at today's exchange rates, and yes, it's Real.

Forget any notion of 'fair' or 'organised' - it is what it says in the title - a Drunken Challenge, so the Rules are not enforceable, and could change.

Basically i'll pay out if someone comes up with something more interesting than just
"Hey ! New Idea ! Distill a Nitrate Salt with Concentrated Sulphuric acid !"

Someone better come up with something soon or i'll have to post the process the lizard aliens use and win it myself so we can get on with DAC#7 - AntiGravity.

Will nitrates found/produced in compost violate the rules?

arkoma - 31-10-2015 at 11:21

I realize its 11 pages long, but why don'tcha READ the THREAD?

MolecularWorld - 31-10-2015 at 11:54

@arkoma : I see 21 pages. Still readable within a reasonable amount of time.

Quote: Originally posted by Agari  

Will nitrates found/produced in compost violate the rules?


I can't speak for aga, but I'd imagine you'd have to start with fresh compostables or manure (or a non-nitrate compound extracted from fresh compost/manure), and provide a complete procedure (with photos!) for turning it into and extracting nitrates; then provide a complete procedure for turning the nitrate into nitric acid using only common household items (with more evidence you actually tried it), to have a shot at the prize.

[Edited on 31-10-2015 by MolecularWorld]

aga - 31-10-2015 at 12:00

Something like that.

A quick google, cut-n-paste to this thread will not win anything.

aga - 5-11-2015 at 11:37

OK.

I'm getting bored with this whole thing.

How hard is it to break out of the 'distill a nitrate with conc sulphuric acid' mindset ?

So many times that has been suggested, clearly by people with zero understanding (or reading abilities).

Recently deltaH broke the 'dissolve in Nitric' mould for Gold dissolution, using salt, vinegar and bleach.

Perhaps the prize fund for this DAC was too small to attract serious interest.

If no actual useful and qualifying process is posted within 6 months i'll post my own submission, win, and be able to move on to something else much more exciting.

MolecularWorld - 5-11-2015 at 11:45

6 months? Mine should be ready before then. And it shouldn't require input of nitrates or sulfuric acid.

aga - 5-11-2015 at 11:59

Cool !

I look forward to seeing your process.

MolecularWorld - 5-11-2015 at 12:06

Quote: Originally posted by aga  
Cool !

I look forward to seeing your process.


No details yet; I'm not yet certain that it'll work, and I don't want anyone to get a jump on me if it does. I will say that I found everything I [think I] need at a single Walmart, including materials -and- apparatus (mason jars... LOTS of mason jars!). Whether it works or not, I should have something useful posted before the New Year.

aga - 5-11-2015 at 12:31

Sounds Good !

We can call it the Single-Wallmart MolecularWorld process - if it works ...

Jstuyfzand - 25-8-2016 at 10:42

So..... we are well past 6 months later.....

PHILOU Zrealone - 25-8-2016 at 12:26

There is this idea from Laboratory of Liptakov to use Pb and NH4NO3 to produce NxOy and further HNO3; I have proposed from PbO for recycling.
HNO3 from Pb or PbO and NH4NO3 thermolysis

And this from Nux vomica to use NaNO3 and H3BO3 to dry distilate HNO3
HNO3 from NaNO3 and H3BO3 (boric acid)

Neme - 25-8-2016 at 12:59

Blue vitriol (I can get that in shop, pool section) + potassium nitrate (from fertilizer) + KAl(SO4)2 (also available in shops here, many sources). And heat it afterwards. I think i read this route in chemistry magazine in article about discovering HNO3.

Cryolite. - 25-8-2016 at 15:21

Guys, the rules for this competition explicitly state no direct use of nitrate ion....

And either way, aga left sciencemadness about a month ago, so even if you managed a working route to nitric acid I strongly doubt you will get any of that prize money.

Velzee - 25-8-2016 at 16:09

Who won?

j_sum1 - 25-8-2016 at 16:57

Who won?

There was no clear winner. No one actually achieved the desired goal.
That said, there were a few ideas out there of some merit which could potentially have got there eventually.
What mostly happened is that it came down to a matter of time investment, engineering and motivation. No one constructed a functioning unit that actually met the brief.

wg48 IIRC put together a Birkland Eade reactor of sorts. But his was several engineering steps away from producing any product. At last report (and there is a nice video somewhere here) he was having difficulty organising a stable spark in the presence of airflow.

I put together a unit to combust soy beans that had been soaked in Cu(II) and permanganate solutions as a catalyst. For this effort I was given some prize money. I had significant issues with airflow and so had nothing that I could test for nitrates. I came up with a conceptual design that I think will work better but life took over and I never got to work on it. I still have the beans but it is not likely at this stage that I will be able to do the construction that I intended. If I am realistic I'd give myself a 30% chance of making (very dilute) nitric acid with my intended setup.


What was really good about this competition is the number of different ideas that were floated and discussed. It was a good introduction for me to a non-trivial problem and I learned a lot through it.

Velzee - 25-8-2016 at 17:19

I believe it's time for new one!

j_sum1 - 25-8-2016 at 17:25

A new competition?
Yeah. Great idea.
Getting participation is the key thing. The one I ran had just one formal entry. The copper carnival that was run before that had I think six or eight entries. There have been others.

Let me recommend looking up the few competitions that we have had and see what worked. Then run with it. I don't think the prize needs to be huge for people to have fun taking on the challenge.

PHILOU Zrealone - 28-8-2016 at 08:39

Quote: Originally posted by PHILOU Zrealone  
There is this idea from Laboratory of Liptakov to use Pb and NH4NO3 to produce NxOy and further HNO3; I have proposed from PbO for recycling.
HNO3 from Pb or PbO and NH4NO3 thermolysis

And this from Nux vomica to use NaNO3 and H3BO3 to dry distilate HNO3
HNO3 from NaNO3 and H3BO3 (boric acid)


Nux vomica has made a test and it works!
Illustrated test for HNO3 from H3BO3 and NaNO3

I have done the maths for improvements and proposed recycling of boric acid from borax:
Maths for H3BO3/NaNO3 process to HNO3

Also possible increase of HNO3 concentration was proposed from dehydrated H3BO3 (easily accessed B2O3)
concentrated HNO3 or N2O5 from diluted HNO3/B2O3 or NaNO3/B2O3

[Edited on 28-8-2016 by PHILOU Zrealone]

arkoma - 31-8-2016 at 21:17

Quote: Originally posted by Cryolite.  
Guys, the rules for this competition explicitly state no direct use of nitrate ion....

And either way, aga left sciencemadness about a month ago, so even if you managed a working route to nitric acid I strongly doubt you will get any of that prize money.


aga ain't gone. And his money so to speak, was always good. He might be pithy at times but he has been pretty daggum generous over the last few years. If DAC 3 was actually completed I imagine he would probably be HAPPY to award the prize.

Cryolite. - 31-8-2016 at 23:03

Quote: Originally posted by arkoma  
Quote: Originally posted by Cryolite.  
Guys, the rules for this competition explicitly state no direct use of nitrate ion....

And either way, aga left sciencemadness about a month ago, so even if you managed a working route to nitric acid I strongly doubt you will get any of that prize money.


aga ain't gone. And his money so to speak, was always good. He might be pithy at times but he has been pretty daggum generous over the last few years. If DAC 3 was actually completed I imagine he would probably be HAPPY to award the prize.


When I posted that, aga hadnt logged on in about a month and a half. However, the day after he started posting again. Talk about bad timing;)

aga - 7-10-2016 at 13:58

Time's Up.

No $ here for anyone anymore.

What i found was a reference which was posted on some unknown, vague, slightly crazy website back in 2008.

http://www.sciencemadness.org/talk/viewthread.php?tid=10511

Basically you electrolyse a peat bog with a plant-pot and get nitric acid.

Next Challenge coming soon to a screen near you.

zwt - 7-10-2016 at 15:08

I must also be "druk". I would have sworn an off-topic post by aga to my Amazon thread led me here, but it's gone! Anyway...
Quote: Originally posted by aga  
The Ideal is to make a useful quantity of Nitric Acid in a way that we all could make it, and be shown/described in a way that others could copy.
I read the thread you just linked, but I can't find the part where they demonstrate how they successfully made their own nitrate-containing peat bog from commonly available items. Did I miss it, or am I the only one here who doesn't own a peat bog?
I also must have missed the part where they actually made and photographed some nitric acid.

In theory, a niter bed could produce nitrates from urine/urea, which could then be electrolyzed, and while that thread hints at a similar concept, nobody has posted a detailed procedure that they themselves have used to produce nitrates, in this way, anywhere on this website, and that's not even considering the second step of making the nitric acid through electrolysis.

It seems that, like this thread, that one has some ideas that might work, but no evidence anyone here has actually done it. Those old articles often leave out important information - electrolysis of nitrates in a divided cell also gives side products, this is what woelen has said on the topic:
Quote: Originally posted by woelen  
This is not a practical method of making nitric acid.


[Edited on 7-10-2016 by zwt]

j_sum1 - 7-10-2016 at 18:32

I have to say that the official closure of this competition has been some time coming. I assumed that it had defacto closed around the time aga took his hiatus. My aspirations for this competition went into permanent recession at the time i shifted house and, because of a different location, have had to graduate from junk-yard chemistry to something a bit more professional-looking. My furnace ideas are just not going to be practical here. I have some permanganate and copper sulfate-soaked soy beans if anyone wants them. (Secret santa anyone? :))


Anyway, a huge thanks to aga for organising this competition. There have been a number of different ideas floated and discussed and it has been very educational. It promoted me from someone with little knowledge of HNO3 (Conc NA was the one acid that scared me) to someone comfortable to work with it and aware of its properties and uses.

Interesting also that, from the start, opinions were divided on the practicality of this exercise. There were experienced and knowledgeable chemists who were a bit dismissive (or even derisive) of the idea stating that it was not going to be doable within the constraints. And there were the newbies with ambitious and imaginative ideas. I think that the verdict has to be that OTC nitric acid from non-nitrate sources is theoretically possible, but in practice, awkward, problematic and time-consuming -- to the level that every other possible source is more convenient. If push came to shove (and we are talking post-apocalyptic conditions here) I am confident that I could make my own hydrochloric, sulfuric and nitric acids from garden sulfur, salt, batteries, pee, heat, electricity and time. That is a good thing to know but It does not mean I will be doing it any time soon.


Anyway, big thanks to aga. This exercise has been very valuable and I hope that the thread continues to attract readership and comments into the future.

J.

j_sum1 - 7-10-2016 at 18:33

I gotta ask, aga. Were you aware of the peat bog electrolysis method when you proposed this competition?

aga - 7-10-2016 at 23:45

No, i didn't know about that before proposing the challange.

Whilst looking for a possible solution i stumbled across that SM thread purely by luck.

When i read it i laughed long and hard.

I mean, where else could a possible answer be !

Texium - 8-10-2016 at 06:52

So you're ending the competition now because you feel like it's already been solved by that thread?
Bit anticlimactic if you ask me.

aga - 8-10-2016 at 09:00

I feel it's too long since it started to leave it open any longer.

Tidying up basically, so maybe a new, more do-able Challenge can begin.

A couple of years should have been enough for anyone to reach a climax ;)

[Edited on 8-10-2016 by aga]

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