Sciencemadness Discussion Board

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

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blogfast25 - 2-8-2015 at 09:38

Dangle89:

The amounts (concentration) of NO<sub>x</sub> in non-catalytically treated exhaust gases is very small. Apart from the inherent problems of processing large amounts of hot gas, this is by no means a practical method of preparing nitric acid.

[Edited on 2-8-2015 by blogfast25]

aga - 2-8-2015 at 10:03

Quote: Originally posted by Dangle89  
I believe Aga said distillation is allowed :)

Distillation is fine.

Just not KNO3 (or any other nitrate salt) with H2SO4

aga - 2-8-2015 at 10:04

Quote: Originally posted by Dangle89  
I believe Aga said distillation is allowed :)

Distillation is fine.

Bashing it 5 times a second with a hammer is also fine.

Rubbing it rapidly between burnt bamboo stems is also good.

Just not KNO3 (or any other nitrate salt) with H2SO4

[Edited on 2-8-2015 by aga]

j_sum1 - 2-8-2015 at 15:07

Scrubbing the exhaust from a combustion engine was an idea I had too. And i had an old lawnmower engine that I could use. ("Had". It's gone now. It was beyond repair as it turns out -- at least with my skills.)

Other than the fact that I couldn't get the mower to work, I abandoned the idea for two reasons.
1) Oxidation of atmospheric N2 really only happens at high temperatures. I wasn't confident that the engine I had would get there -- particularly without a load on.
2) I could think of better things to do than spending several hours babysitting a noisy engine at high revs blowing bubbles in a bucket.
3) It seemed like a good way to get carboxyllic acid that I would then need to separate from the nitric acid. I figured CO2 would displace a lot if not all of the dissolved NOx.
4) I reasoned that nitrogen in the fuel was going to give a better yield than incidental reactions with N2 in the air.
5) I never was much good at counting.

J.

Little_Ghost_again - 3-8-2015 at 03:51

Ok I am back on this :D, I have a source for ammonia thats a bit wild lol but getting from ammonia to nitric acid without platinum is my sticking point. can it be done without the catalyst? my source for ammonia is maggots! Ive checked and double checked and they produce loads if you keep them 3-4 days in a bait box with sawdust and few vent holes (tiny ones) then clean them with clean sawdust and repeat for second load sawdust soaked in ammonia. I also found a paper on maggot treatment that also states they produce ammonia, ok its not huge amounts but I have 10 pints of them on the go and a fair bit of liquid to process. Next step is how can I get that to the monoxide?

Little_Ghost_again - 3-8-2015 at 05:22

Aga can we use a battery and copper wire? I cant remember all the rules. I used an aquarium test kit and sure enough the maggot liquid is off the scale for ammonia even diluted 20x :D. Still totally unsure how to get around the platinum but there must be a way :D

copper method

NWS - 3-8-2015 at 19:44

So I'm back after much ruminating and I have a theoretical reactor design with one or two kinks to be worked out yet.

step 1: acquire a copper cooling unit. I used the radiator from an old dehumidifier, however an old window AC would work.

step 2: obtain ammonia (for my purposes source doesn't matter, but for the competition one could boil down urine or some such)

step 3: strip the a aluminum fins off a short section in the middle of the unit. My thought process is leave just enough fins on to cool the reaction and prevent a copper melting runaway while leaving a section behind to fully cool the gasses to room temperature. (sorry if this is confusing, please ask for clarification if needed)

step 4: walk into fleet farm or a hardware store and pick up a small oxygen tank for around $5 USD

step 5: Set up a beaker and attach a rubber/vinyl/whatever hose from the beaker going to a T where the O2 and the NH3 can mix (make the O2 adjustable to optimize the reaction?). Then pipe this into the copper unit. Pipe the exhaust into water/H2O2/silica gel.

step 6: here is where the kinks come in. if you have anhydrous ammonia laying around in your shed this is pretty easy Pour NH3 in the flask, allow it to boil off. turn the oxygen on and then pre-heat the barred copper line to a red glow with a torch.
step 6b: obtain .880 ammonia either as is or through concentration. boil this off into the line. proceed as above. Be wary of water vapor forming HNO3 in the copper tubing and dissolving it.
step 6c: get dilute ammonia, boil off as above, and find a way to dry the ammonia vapor.

Thoughts: Running Oxy through rubber/vinyl line poses a fairly large fire/explosion risk, especially near red hot copper. This is kink one, how to do this without risk of lighting the oxy/vinyl line on fire. The second problem would be how to dry ammonia gas. From the research I've done CaCl won't work as it forms a complex, neither will conc. H2SO4 due to acid base reactions, and MgSO4 will form MgOH.
Finally, I'd recommend a large bucket of water nearby in case of a meltdown and a fire extinguisher in case the oxy gets away on you.

Thoughts, comments, questions or concerns are welcome!

Dangle89 - 4-8-2015 at 04:44

Ah cool cool :D

Just though I would chuck it out there in case it was one of those things that are so simple it gets over looked by accident!

Did some more research on it and is definitely not simple! On an industrial scale it is possible but would not fit our desert island scenario!

On that, Just wondering why Pt was deemed out of bounds? Happy with the rule as it is expensive and wouldn't be a "cheap" method, which was one of the goals, But surely Pt could be obtained anywhere in the world OTC at a jeweler or bullion dealer (or maybe the Island has Pt nuggets in the river or buried pirate treasure :P)?

Aga, you would be surprised at how many things you can fix in mechanics by bashing them with a hammer 5 times a second :P

Little_Ghost_again - 5-8-2015 at 09:05

I am thinking electrolysis of water for oxygen and bubble that into it. first trial tomorrow, how do I titrate ammonia? smells pretty strong so maggots seem great at ammonia production and if you killed your mate on the desert island you would have loads of maggots after a couple of meals of course.

Praxichys - 5-8-2015 at 10:37

Quote: Originally posted by NWS  
The second problem would be how to dry ammonia gas. From the research I've done CaCl won't work as it forms a complex, neither will conc. H2SO4 due to acid base reactions, and MgSO4 will form MgOH.


You can dry NH3 with alkali and alkaline earth oxides and hydroxides. CaO works well, as does NaOH or KOH. First run it through a really cold and efficient condenser which will remove most the water, then use the chemical water trap. You may also be able to use molecular sieves or silica gel.

While CaCl2 does suffer from complexation with ammonia, it can still be used at the expense of ammonia yield. The complex itself is highly hygroscopic.

battoussai114 - 5-8-2015 at 15:07

Hey NWS, I have a similar setup waiting for me to get time to test it, maybe we could compare our results later on.
My setup is:
Ammonia being generated by reaction of ammonium chloride with NaOH in a glass container;
Connected to this container is a dry air inlet and the mixed stream then goes into copper tubing bought from local AC supplier;
A MOT pumps a huge amount of current into a section of the cooper pipe heating it, this part is problematic as the transformer and its wiring needs to be actively cooled as the copper pipe isn't particularly resistive. I'll either change to a tungsten resistance or get myself a propane torch (less likely due to limited budget);
The product gas stream then goes into a packed bed wet scrubber containing H2O2 solution (I'm expecting that most of the NO will be oxidized to NO2 and should then react to form nitric acid). Further in line I'll put another scrubber with water to keep any unreacted ammonia from leaving, and last I'll improvise some flow rate meter or just measure the volume of gas that will have left when its done.

Now, assuming full oxidation of NO to NO2 and that all NO2 would be captured in the first scrubber I can check how acidic the peroxide solution became and then use MnO2 to catalyze the decomposition of leftover peroxide into water, then boil the water/acid mixture down and see how much ammonium nitrate I got.
From the second scrubber I can see how much Ammonia was dissolved and given the amount of ammonia on the second scrubber + ammonia reacted to ammonium nitrate I can calculate the unreacted ammonia.

From the volume of inert gas (or from the flow rate of inert) I can calculate the selectivity of the reaction that is taking place and try varying the parameters of the reactor until I find the best yield of nitrogen oxides versus N2.

Overall that's what I plan on doing, if anyone could point mistakes on the experiment or in my proposed result analysis I'd appreciate it.


[Edited on 5-8-2015 by battoussai114]

j_sum1 - 5-8-2015 at 16:35

@battoussai114
The critical part is going to be the oxidation of NH3 to NOx. Ie, it doesn't happen without very high temperature, very high pressure and a platinum group catalyst. Even then, conversion to NO2 is low. Real world systems divert the NO produced back through the stream for further oxidation. (Not an easy thing to do at high T & P for a home chemist.) Now that is based on what I have read (and remembered). Feel free to do some more reading yourself and don't let my comments deter you from experimenting.
Then you have the problem of dissolving a hot gas stream in a liquid. Not ideal.
The other thing to consider is that ammonia is going to be a lot more soluble in your water/H2O2 mixture than your nitrogen oxides. In other words, you really don't want to have any NH3 left. In solution (or before) it will react with your nitric acid produced. Ammonium nitrate might not be a bad result but it is not your primary target.
https://en.wikipedia.org/wiki/Ostwald_process

battoussai114 - 5-8-2015 at 17:10

@J_Sum1,
Thanks, I've read a bit on the industrial ammonia to NOx conversion process, but since platinum group metals aren't very interesting in our situation I'm skipping these and going for things that are available to us. For instance someone here on the board tested cooper with results, although with low yields, and there are quite a few novel catalysts that could be tested, anything from cooper over various supports to maybe manganese nanoparticles... after all, catalysis is such diverse field.
I think the biggest point in the industrial use of platinum is how good it performs and, since there is going to be a huge investment in their production plant anyway, it's just easier to pay a lot for some rare metal that will definitely give good results albeit making the factory take longer to pay for itself instead of spending on R&D for something different.

For instance, I remember talking to a researcher of the university I study and he was commenting on how they presented to a local company a concept that would allow for higher efficiency for their soy dryers just to get turned down with the answer that in the case they needed higher soy drying rates they'd just buy another equipment.

Anyway, What I intend to do is first get the equipment to analyze the product stream of gas right, and then start working on different reactor parameters and various catalysts... And you have no idea how much I wish I could get a permit to use the gas chromatograph at the university....
Now, considering that ammonia is indeed more likely to dissolve in the peroxide solution, I'd better first scrub the gas with water and then put a H2O2 scrubber next.

Camroc37 - 5-8-2015 at 17:28

So if I drive to Lowe's and buy non-concentrated Nitric acid and distill it does that count

NWS - 7-8-2015 at 19:10

battoussai114 I had the same idea with the MOT, but I'm leaning towards a propane torch right now as I'd rather not add lethal amounts of electricity to the things that could possibly go wrong, btw a propane torch can be obtained at fleet farm for $10 + a $3 propane tank, and that's for a pretty nice simple one. The formula I've been using is:
16 NH3 + 21 O2 → 6HNO3 + NO + NO2 + 21 H2O
This means that an air stream with 56.7% Oxy and 42.3% NH3 will give around 70% nitric acid along with NOx. Now I know I'm not going to get that accurate with the gas streams, however I'd like to have excess oxy to oxidize the NO. And rather than bubble it through anything I was going to dissolve it in the water produced from the oxidation of ammonia by containing and cooling the output gasses.
Camrock, first, read the rules. second what Lowe's has nitric acid and where? I want in on this.

Edit: My source of ammonia is probably going to be heated cleaning ammonia ~15%, possibly with some NaOH added, depending on preliminary testing. My source for anhydrous ammonia switched to urea this year. :(
Edit2: I also stopped worrying about drying the ammonia after realizing the oxidation will produce water anyhow.
P.S. battoussai114 I doubt the Mot will be needed for very long as the oxidation is highly exothermic, the change in gibbs free energy for the reaction listed above is around 4800KJ, which if we calculate the change in temperature of the products we get
18.02 g/mole*21 mole * 4.181 J/g*K =1582(H2O)
30.01 g/mole*1 mole*0.995 KJ/Kg*K= 29.9(NO)
1 mole * 37.5 J/Mole*K=37.5
63.01 g/mole * 6 mole * 1.72 KJ/Kg *K= 650
1582+29.9+37.5+650=2.299 KJ/K
4800/2.299=2087 Kelvin
2087+21C (room temp) = 2098 degrees C (temp of products assuming full reaction)
now this temp feels wrong, and it's a bit late for math, so if someone can find any flaws in my math, please point it out. However if it is correct, then not only is continuous heating unnecessary, active cooling would be needed.

[Edited on 8-8-2015 by NWS]

[Edited on 8-8-2015 by NWS]

gatosgr - 10-8-2015 at 23:49

how did you get to this?

18.02 g/mole*21 mole * 4.181 J/g*K =1582(H2O)
30.01 g/mole*1 mole*0.995 KJ/Kg*K= 29.9(NO)
1 mole * 37.5 J/Mole*K=37.5
63.01 g/mole * 6 mole * 1.72 KJ/Kg *K= 650
1582+29.9+37.5+650=2.299 KJ/K
4800/2.299=2087 Kelvin
2087+21C (room temp) = 2098 degrees C (temp of products assuming full reaction)

Dangle89 - 11-8-2015 at 03:06

Hello again :)

Found this (making Nitrates from dirt):

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

Not sure why the guy tastes it but hey! Personally I wouldn't stick anything I've made in the backyard lab in my mouth and anything made of poo would be no exception! Whatever floats your boat though :P

Does anyone knows how to make another acid from OTC compounds? I believe all strong acids of any concentration were out of bounds for this challenge weren't they?

If you could make say H2SO4 or HCl from OTC materials, mix it with nitrates made from poop dirt would that be a winner?

Not sure if this is a good / stupid idea and have done next to no research on any of this proposed process but saw the video while looking at other stuff and thought I would put it out there as I remembered someone talking bout chicken poop early on in this thread :D

Hope this is of some use!

Dan

gatosgr - 11-8-2015 at 22:21

how about ammonium nitrate from ice cold packs?
if h2so4 is allowed then it's a piece of cake to make HNO3
that guy codylab has made HNO3 in many ways check out his videos

[Edited on 12-8-2015 by gatosgr]

Dangle89 - 12-8-2015 at 01:46

Quote: Originally posted by gatosgr  
how about ammonium nitrate from ice cold packs?
if h2so4 is allowed then it's a piece of cake to make HNO3
that guy codylab has made HNO3 in many ways check out his videos

[Edited on 12-8-2015 by gatosgr]


Na mate.

Bought Nitrates are a no no. As is H2SO4.

The situation is pretty much what you could find in a supermarket in the year 2050 where anything of any scientific value is regulated so far up the bum that you might have to sign your life away to buy 5g of NaCl.

Or what you can find on a desert island now :P

aga - 12-8-2015 at 04:21

Quote: Originally posted by gatosgr  
if h2so4 is allowed then it's a piece of cake to make HNO3

Exactly. That's why it's not allowed.

If it was easy, it wouldn't be a Challenge would it ?

gatosgr - 12-8-2015 at 06:54

One easy way that requires no chemicals at all is with high voltage from the sky, it's 100V/m the higher you go when it's about to rain. It would take a lot of time to make amounts of HNO3 but still...

Big Boss - 12-8-2015 at 13:51

I'll try and figure something out...
That money is as good as mine! muahahaha

[Edited on 13-8-2015 by Big Boss]

aga - 12-8-2015 at 14:19

It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]

battoussai114 - 12-8-2015 at 18:07

Fun fact, a single MOT is not enought to strike a decent plasma arc... but it certainly is enough to get a tungsten electrode really really hot, like incandescent hot, and then the insulation on the secondary melt... One of these days I'll drop by the scrap yard and get more wire and another transformer to put in parallel with the first one.
And yes, all these days and this is the only thing worth or report I done in this matter.

Quote: Originally posted by aga  
It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]

No idea... I didn't even read all these pages.

Dangle89 - 12-8-2015 at 20:57

Quote: Originally posted by aga  
It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]


I think it was now 350euros wasn't it?

Started at 250 but pretty sure it increased to 350!

With the Australian dollar the way it is that is around $1,000,000 :D Hahaha Na :P Is a LOT of moneys though :)

Quote: Originally posted by aga  
Amazing finds WGTR and j_sum1

A Nitric Acid Competition, and a Bug Exterminator discovered !

The sheer innovation and imagination you guys are demonstrating is what this is all about.

For those that don't know, bugs tend Not to eat things that kill them, much like us, and most living things.

Finding something they Will eat, yet kills them, is the entire Bug Poison Industry's secret.

Prize fund increases to 350 euros.

Edit:

Anyone Stressing Plants by shouting 'Harvester' or 'Sheep' at them in order to increase their nitrate levels will be disqualified.

[Edited on 23-2-2015 by aga]


Here you go :)

[Edited on 13-8-2015 by Dangle89]

Dangle89 - 13-8-2015 at 00:16

I have an actual fully thought through idea that I think is within the rules!

Aga can you please say "Yes" or "No" to the chemicals used?

1. Make the Poop dirt nitrates from the video I linked to a couple of posts ago. It uses: composted poop, Na2CO3(can be bought as supermarket washing powder - Bicarb would probably(?) be OK too) and H2O.

2. Mix NaClO (supermarket bleach) with Acetic Acid (vinegar) and bubble the Cl2 gas through H2O to produce HCl acid.

3. Add homemade crap nitrates to homemade HCl

4. Distil the HNO3(hopefully) from the salts :)

Is this possible and within the rules?

I don't really have the time to do this but if someone wants to use the idea to win the 350 euro I will only charge them a small fee :P Hehehe Jokes :)

If anyone wants to try this method go for it :) I would just be happy to contribute something to the backyard scientific community :D

Hope this idea is an OK one!

Dangle


[Edited on 13-8-2015 by Dangle89]

gatosgr - 13-8-2015 at 00:53

Well I think I have a process within the rules as well, instead of making HCL supermarkets sell batteries which contain H2SO4 and you can even use an old battery if you don't wanna spend the $$ there are cars everywhere and batteries are the least controlled item anywhere. The nitrates can be made using this video from dirt: https://www.youtube.com/watch?v=VaGykqoNhJk

H2SO4 + 2 NaNO3 --> Na2SO4 + 2 HNO3

gatosgr - 13-8-2015 at 01:37

Another cheap and easy source for acids are drain cleaners , they are usually 23% HCL or you can find some with H2SO4. Every supermarket has them.

About making the nitrates you can extract them from plants but given ~50mg NO3- /g of plant material you need ~840g of plant material in order to make 100ml 30% HNO3. The soil method is pretty old and involves feces or urine as the source of nitrates, urine alone can be made into nitrate but the quantity needed depends on the concentration of nitrates or urea, extracting nitrates from ham or milk is possible but you need lots of it.

Between these method I prefer the plants, the fermentation of manure soil e.t.c. can take up to a year.

[Edited on 13-8-2015 by gatosgr]

gatosgr - 15-8-2015 at 01:54

Are drain cleaners allowed or should we bubble chlorine gas through water to make HCL? Electrolysis and such... although drain cleaners are very common everywhere.

[Edited on 15-8-2015 by gatosgr]

aga - 15-8-2015 at 08:08

Why not just Buy some conc HNO3 ?

That'd be really interesting, educational, informative and Fun. Not.

Re-read at least the first page for a Clue as to what this is about.

gatosgr - 15-8-2015 at 08:29

Yeah I read it and it says whatever you can find in a typical supermarket.. but anyways bubbling some Cl2 through water is not that hard.

blogfast25 - 15-8-2015 at 08:57

Quote: Originally posted by gatosgr  
Are drain cleaners allowed or should we bubble chlorine gas through water to make HCL [sic]? Electrolysis and such... although drain cleaners are very common everywhere.

[Edited on 15-8-2015 by gatosgr]


How, pray tell, are you going to make HCl by bubbling chlorine through water, huh?

aga - 15-8-2015 at 09:00

Magic Water is also not allowed as it is made from Unicorn Extract.

gatosgr - 15-8-2015 at 10:36

Quote: Originally posted by blogfast25  
Quote: Originally posted by gatosgr  
Are drain cleaners allowed or should we bubble chlorine gas through water to make HCL [sic]? Electrolysis and such... although drain cleaners are very common everywhere.

[Edited on 15-8-2015 by gatosgr]


How, pray tell, are you going to make HCl by bubbling chlorine through water, huh?


with unicorn extract from dangle

aga - 15-8-2015 at 11:34

It is not clear if you get blogfast25's obvious point : bubbling Cl2 through water just dissolves a bit of chlorine in the water, it does not make HCl.

[Edited on 15-8-2015 by aga]

aga - 15-8-2015 at 11:50

Quote: Originally posted by Dangle89  
Aga can you please say "Yes" or "No" to the chemicals used?

1. Make the Poop dirt nitrates from the video I linked to a couple of posts ago. It uses: composted poop, Na2CO3(can be bought as supermarket washing powder - Bicarb would probably(?) be OK too) and H2O.

Poop Yes, Bleach, dunno, wavering to No as it's hard to make yourself, yet is widely available, so Yes ?

OK. Yes to 5~8% Bleach, unless there's somebody out there who actually cannot get any Bleach.

Quote: Originally posted by Dangle89  
2. Mix NaClO (supermarket bleach) with Acetic Acid (vinegar) and bubble the Cl2 gas through H2O to produce HCl acid.

Vinegar yes (easy to make anyway), Bleach as above.

Quote: Originally posted by Dangle89  
3. Add homemade crap nitrates to homemade HCl

Sounding like a Plan.
Not sure it'll work, one way to find out for sure.

Quote: Originally posted by Dangle89  
4. Distil the HNO3(hopefully) from the salts :)

Distillation is allowed.

gdflp - 15-8-2015 at 12:11

Quote: Originally posted by aga  

Bleach, dunno, wavering to No as it's hard to make yourself, yet is widely available, so Yes ?

OK. Yes to 5~8% Bleach, unless there's somebody out there who actually cannot get any Bleach.

It's not terribly difficult to make, electrolysis of a sodium chloride solution in a well designed cell yields sodium hypochlorite solutions.

aga - 15-8-2015 at 12:16

OTC bleach is OK then.

I've never built a chlorate cell.

Is it worth the bother ?

[Edited on 15-8-2015 by aga]

Little_Ghost_again - 16-8-2015 at 14:15

Quote: Originally posted by aga  
OTC bleach is OK then.

I've never built a chlorate cell.

Is it worth the bother ?

[Edited on 15-8-2015 by aga]


sure even if its just for shits and giggles! But seriously some can only get 3% bleach so might be useful? Its a tinkering project so I guess they are always worth a go.

Big Boss - 17-8-2015 at 03:34

I have managed to make nitrates via bacterial oxidation of ammonia, tested a few tiny crystals with H2SO4 and little copper wire strands, it evolved NO2.

gatosgr - 17-8-2015 at 05:17

Where will you get ammonia from?

[Edited on 17-8-2015 by gatosgr]

Big Boss - 17-8-2015 at 05:59

Where won't I get ammonia from is the better question, you can buy it at practically every hardware store, you could make it from piss and urease which I have done and it's in most constant cold packs nowadays.

[Edited on 17-8-2015 by Big Boss]

gatosgr - 17-8-2015 at 23:28

Ammonia is out of the rules. You can use piss but again there's no need to make ammonia you can make nitrates with it.

[Edited on 18-8-2015 by gatosgr]

Little_Ghost_again - 18-8-2015 at 08:07

Quote: Originally posted by gatosgr  
Ammonia is out of the rules. You can use piss but again there's no need to make ammonia you can make nitrates with it.

[Edited on 18-8-2015 by gatosgr]


Like other insects the fly goes through three phases to reach adulthood: egg, larva, pupa and then adult.

One of the most fascinating aspects of these creatures is the ammonia which is produced by fly larvae, a natural secretion used by the creatures to kill bacteria.

Read more: http://www.mediaclubsouthafrica.com/tech/2770-maggots-070212...


this is from http://www.mediaclubsouthafrica.com/tech/2770-maggots-070212

however any google on maggots and secretions should provide reliable reference to the fact that maggots produce rather alot of ammonia. Or ask a fisherman :D

So ammonia must be in the rules if gained by desert island routes, like your shipmate died and is now maggot infested :D

aga - 18-8-2015 at 08:20

Maggots are OK.

What do we Want ? Freedom for Maggots !
When do we want it ? Now !

Big Boss - 18-8-2015 at 10:00

Quote: Originally posted by gatosgr  
Ammonia is out of the rules. You can use piss but again there's no need to make ammonia you can make nitrates with it.

[Edited on 18-8-2015 by gatosgr]

Original post says I can buy anything found in a supermarket, I'm going to assume that means OTC as well.
Where did aga say ammonia is out? Also I'm not utilising aqueous ammonia but ammonium salts

Little_Ghost_again - 18-8-2015 at 10:19

Quote: Originally posted by Big Boss  
Quote: Originally posted by gatosgr  
Ammonia is out of the rules. You can use piss but again there's no need to make ammonia you can make nitrates with it.

[Edited on 18-8-2015 by gatosgr]

Original post says I can buy anything found in a supermarket, I'm going to assume that means OTC as well.
Where did aga say ammonia is out? Also I'm not utilising aqueous ammonia but ammonium salts


OTC means different things in different countries, some countries you can buy conc nitric acid OTC, so the supermarket I took to mean an average type supermarket with common under the sink or bathroom stuff.
NOT root killer ect ect ect. SHIP WRECK with a local corner shop that sells beer and a few other things is what I think aga had in mind :D

aga - 18-8-2015 at 11:02

LG2 has it just about right Big Boss.

I'll not pay a a single cent to someone who just makes HNO3 simply out of an OTC nitrate salt and conc H2SO4.

This a Drunken aga Challenge : the Rules are not 100% fixed and frozen.

If i think that a Solution is boring and just following the same old well-trodden ground, then it won't win.

If you managed to fire an ex-Hampster wrapped in Clover into the air with a fart-powered gas cannon, and it magically hit a Hot Copper funnel and magically made HNO3, then that would probably Win, even if the underlying reaction were a Nitrate salt and Sulphuric acid somehow getting themselves distilled somehow.

Buy/purify/distill = Nitrate Salt & H2SO4 will not win.

What will win is a New pathway to Nitric Acid.

Surprising that nobody has any Funghi growing ...

Little_Ghost_again - 18-8-2015 at 12:08

Quote: Originally posted by aga  
LG2 has it just about right Big Boss.

I'll not pay a a single cent to someone who just makes HNO3 simply out of an OTC nitrate salt and conc H2SO4.

This a Drunken aga Challenge : the Rules are not 100% fixed and frozen.

If i think that a Solution is boring and just following the same old well-trodden ground, then it won't win.

If you managed to fire an ex-Hampster wrapped in Clover into the air with a fart-powered gas cannon, and it magically hit a Hot Copper funnel and magically made HNO3, then that would probably Win, even if the underlying reaction were a Nitrate salt and Sulphuric acid somehow getting themselves distilled somehow.

Buy/purify/distill = Nitrate Salt & H2SO4 will not win.

What will win is a New pathway to Nitric Acid.

Surprising that nobody has any Funghi growing ...



SHhhhhhhhhh
;)

Shetland pony takes a while but..........

Texium - 18-8-2015 at 13:41

Quote: Originally posted by aga  
OTC bleach is OK then.
How is OTC bleach alright but OTC ammonia isn't? They are about the same availability wise, and can be purchased from the same stores.

gdflp - 18-8-2015 at 13:45

Quote: Originally posted by zts16  
Quote: Originally posted by aga  
OTC bleach is OK then.
How is OTC bleach alright but OTC ammonia isn't? They are about the same availability wise, and can be purchased from the same stores.

Because of this.
Quote: Originally posted by gdflp  
Quote: Originally posted by aga  

Bleach, dunno, wavering to No as it's hard to make yourself, yet is widely available, so Yes ?

OK. Yes to 5~8% Bleach, unless there's somebody out there who actually cannot get any Bleach.

It's not terribly difficult to make, electrolysis of a sodium chloride solution in a well designed cell yields sodium hypochlorite solutions.

Big Boss - 18-8-2015 at 16:39

Ammonia can be made extremely easily, much easier than NaClO. I have made it as a proof of concept, I will not however be making it on the scale that is required to make 100ml of nitric acid. Also aga please check your supermarket for Ammonia bleach. It is fairly common.

Little_Ghost_again - 18-8-2015 at 18:05

Ok pics to follow tomorrow on progress so far, but I need a little help with something...................................

I have nitrates from poo!! shetland pony poo and other animals, since this started I have been picking up the poo and plonking it into a heap, it tests positive for nitrates nitrites and ammonia using aquarium water test kit.
I have a cement mixer to make life easier but bucket and/or bath and plank of wood to stir would do as well, I just chose the mixer for speed. so I now have poo to process with water and then filter into old bath tub. Let it settle and decant off liquid (nitrates). My problem then becomes what is allowed within the rules to get from nitrates to nitric acid? I also have maggot ammonia (50ml).
I will post the pics tomorrow.

j_sum1 - 18-8-2015 at 21:03

Mmmm maggot ammonia! Sounds tasty.

Little_Ghost_again - 19-8-2015 at 07:42

seriously maggots make great ammonia! and loads of it! vermiculite is tops for collecting it (maggots crawl around in it) I found sawdust started to convert the ammonia to nitrite and something else. :D

aga - 19-8-2015 at 08:56

Mmmm. Nitrites.

Romain - 29-8-2015 at 07:15

A youtube user (Cody'sLab) has had success with making nitric acid via a Birkeland-Eyde reactor: https://www.youtube.com/watch?v=ep23ds4cZs4. It sounds like an easy option, particularly if you have solar panels to generate electricity (because electricity ends up costing a lot if your reactor runs 24/7).

aga - 29-8-2015 at 13:30

Voltage rule applies.

Big Zaps of kilovolts = already done (many decades ago) = not allowed.

How much you pay for your 'lectric doesn't really make any difference.

Perhaps people wanting HNO3 could look to Other routes, and not just those that Google serves up readily ?

It was not always like this.

There was a Time, not so long a go in a Galaxy not so far away where people Discovered things not by using the Internet or computers.

Shocking, i know - the Internet did not exist way back then, a full 35 years ago.

People back then Did Actual Stuff, which was called Experimentation.

Amazingly, despite the woeful lack of Internet or Computers, they discovered things, like the way the Universe works, such as Electricity, Magnetism, the structure of DNA and Quantum Mechanics.

Whether this challenge is do-able or not, it'd be great to see people Doing things, as even a failed attempt to produce HNO3 by a NEW route may well Discover something New that could be of great value to Science.

Prize fund Increased to 500 Euros.

Little_Ghost_again - 29-8-2015 at 15:03

I am waiting for the rain to stop at some point during daylight hours so I can post what i have so far. Its a great challenge and harder than it first seems!

gdflp - 29-8-2015 at 16:22

Is an aspirator or vacuum pump allowed? I have an idea and, while a vacuum is not technically needed, mechanical losses will otherwise be too high for the process to be feasible.

aga - 30-8-2015 at 01:08

There's a vac pump in my lab, so that would be 'standard labware', so Yes.

In McGuyver World, some degree of vacuum could temporarily be rigged up with two containers of water and a hose, or with a hand-cranked pump too.

kecskesajt - 30-8-2015 at 02:54

Vacuum pump is too easy. I made by a buncher funnel(aviable in normal stores)a vitamine bottle,and a 100 ml syrenge.

KesterDraconis - 1-9-2015 at 06:31

Would it be ok in this challenge to get nitrates from a cave? I happen to go spelunking often, it would be pretty easy to get it there (since a lot of caves in my area have it present in them).

aga - 1-9-2015 at 08:24

You can go collecting whatever you like.

What's the plan with the nitrates ?
Distill with conc sulphuric acid .... :o

[Edited on 1-9-2015 by aga]

Little_Ghost_again - 2-9-2015 at 01:29

Quote: Originally posted by aga  
You can go collecting whatever you like.

What's the plan with the nitrates ?
Distill with conc sulphuric acid .... :o

[Edited on 1-9-2015 by aga]


According to the original rules if you made sulfuric acid via everyday chemicals or whatever then surely there is nothing wrong with that?
i know the electric methods etc and some of the 'new' ideas are great but they do kinda limit who could replicate them.
So quick clarification.............
Is it as per the second post of this thread or is it now a 'new' as yet undiscovered way to make nitric acid? I have my nitrates taken care of and now I was going to go a very very OTC way about getting sulphuric acid from scratch, rather than buy something that contains it and purify that. in My method I was going to try electrolysis of mag sulphate with copper anode to make copper sulphate, then go from copper sulphate to sulphuric acid.
So is this method in the rules or even in the spirit of the rules?
My source of nitrates has been very desert island (maggots and various animal poo etc etc) I have no idea exactly what nitrates are in it but its reading very high on my nitrate test kit :D

aga - 2-9-2015 at 07:46

Well, i dunno really.

Is it a competition to make Nitic acid by a New route, or a competition to make Sulphuric acid by a roundabout route that ends up beings used to distill a nitrate equally obtained ?

Anyone else have any thoughts ?

If nothing else comes up that is more Novel, then you'd win i guess.

It is a DAC, so i'll have a few more beers and ask myself what i think (if anything).

Little_Ghost_again - 2-9-2015 at 08:46

I could have saved time and ran the exhaust from the tractor into water :D. I havnt given up yet, I asked for clarity because my back up is carbon plates and mains electric to make ozone................

Get really drunk and have a think :P

NWS - 2-9-2015 at 15:34

So I have suffered a crippling setback. Apparently the apartment complex I'm staying in this semester frowns upon building laboratories (or even hot things). In all seriousness, I will continue testing my hot copper pipe method in December (or possibly sooner if I have time off). I have all the ingredients/parts/tools, all that is needed is to put it together and heat it up. I'm thoroughly interested/invested in this now, so if anyone has/will/is thinking about trying it, updates will be greatly appreciated.

NWS - 2-9-2015 at 16:01

gatosgr
I just went through this step by step until I found the godawful, how-did-I-mess-up-this-bad error, so bear with me here.
18.02 g/mole*21 mole * 4.181 J/g*K =1582(H2O)
This is the thermal energy in the water vapor

30.01 g/mole*1 mole*0.995 KJ/Kg*K= 29.9(NO)
likewise for NO
1 mole * 37.5 J/Mole*K=37.5
and so on for each component of the exhaust gas
63.01 g/mole * 6 mole * 1.72 KJ/Kg *K= 650

1582+29.9+37.5+650=2.299 KJ/Kg
This is the total energy contained in the exhaust in Killo joules (There should be no Kg here)

4800/2.299=2087 Kelvin
This appears to be completely messed up, what should happen here is to divide the total amount of energy by the average specific heat capacity(SHC), found by multiplying each particular gasses SHC by the number of moles that gas contributes to the exhaust and taking the sum.
However since one of the SHC's I found was in KJ/Mole*K I can't do this very easily, so I'm going to cheat and estimate the average as 4. This is slightly less then the SHC of water, which would dominate the average.
This would give a (hopefully correct) ballpark of 600 K (minding sig figs)
This seems to be a much more reasonable answer so it's what I'm going to go with.




[Edited on 3-9-2015 by NWS]

j_sum1 - 2-9-2015 at 16:37

@LGA
The great drunken one has already spoken in this matter although his wise words are somewhat unclear through the mist of ethanol vapours.
http://www.sciencemadness.org/talk/viewthread.php?tid=48085#...
This suggests that the emphasis of the competition is a novel means for production of nitric acid. Although H2SO4 is not specifically excluded it would perhaps be allowable if manufactured yourself.
http://www.sciencemadness.org/talk/viewthread.php?tid=48085#...
This re-emphasises the spirit of the comp that a novel approach is required and that distillation of nitrates using sulfuric acid is somewhat outside of the spirit of the competition.


My take on all of this. I think maggots and chicken excrement is certainly novel. This looks like a legitimate way of attaining nitrates if you can get it to work. Once you have nitrates, you are onto a standardised route which may or may not be allowable if you are making your own H2SO4. Forgive my vagueness on this detail. i can't quite read the last line of the chart through the bottom of my beer glass.

aga - 3-9-2015 at 10:57

Yeah.

It'd so much more Worth It if the winning process is not just Sulphuric & Nitrate being distilled.

Novel procedures for arriving at that point would also be good, so worthy of a prize i guess.

WGTR - 3-9-2015 at 13:09

Here's what I'd suggest: if someone wants to obtain nitrates from organic sources, why not go further with this, and ferment

the matter in a silage bag? "Silo gas" is a problem in the commercial world, and is an undesirable byproduct of ensiling

organic matter with high nitrate content. Observe this red cloud of beauty: http://www.cattlenetwork.com/news/silage-safety-begins-field .

You wouldn't even need to add other acids to obtain this; nitric acid would be produced directly from the silo gas. It may need

some purification though.


Work out the proper conditions to obtain the best yield. Perhaps supplement a grass fermentation with a little extra

nitrogenous "pony". Work out the optimal Dry Matter levels and temperature needed. How long does the fermentation take?

How much nitrate could be obtained from different parts of the grass? It might be useful to work out the fermentation process

using store-bought nitrates, until the bugs are worked out. Define the variables needed to make the process duplicable by

someone else, and document it well. Those are just my 2 cents.

aga - 3-9-2015 at 13:20

!!!

WGTR, that is the kinda thing this competition is all about.

Little_Ghost_again - 3-9-2015 at 15:11

Quote: Originally posted by WGTR  
Here's what I'd suggest: if someone wants to obtain nitrates from organic sources, why not go further with this, and ferment

the matter in a silage bag? "Silo gas" is a problem in the commercial world, and is an undesirable byproduct of ensiling

organic matter with high nitrate content. Observe this red cloud of beauty: http://www.cattlenetwork.com/news/silage-safety-begins-field .

You wouldn't even need to add other acids to obtain this; nitric acid would be produced directly from the silo gas. It may need

some purification though.


Work out the proper conditions to obtain the best yield. Perhaps supplement a grass fermentation with a little extra

nitrogenous "pony". Work out the optimal Dry Matter levels and temperature needed. How long does the fermentation take?

How much nitrate could be obtained from different parts of the grass? It might be useful to work out the fermentation process

using store-bought nitrates, until the bugs are worked out. Define the variables needed to make the process duplicable by

someone else, and document it well. Those are just my 2 cents.

Hmmm this has given me an idea! thanks alot!
I was going to make the sulphuric but Fermentation of grass........
A bag is a long process, however I guess I could ferment grass in the lab as a trial :D

Hawkguy - 3-9-2015 at 17:44

Dude it'll be easier to go all out with fermenting grass right away on a large scale, instead of wasting time on small trial runs. I'm finding out now that it looks like about 1 to 2 years before much can be produced by this method on a reasonable scale.

Little_Ghost_again - 4-9-2015 at 00:34

Quote: Originally posted by Hawkguy  
Dude it'll be easier to go all out with fermenting grass right away on a large scale, instead of wasting time on small trial runs. I'm finding out now that it looks like about 1 to 2 years before much can be produced by this method on a reasonable scale.


I am surrounded by farms! Plenty of silage pits around here, so the plan is too go get some silage from deep in a pile and mix with some maggot juice (as a trial) and see what I can do. I have something in mind................
The main problem is I have always lived around farms and never seen that before, so I asked my dad about it. Apparently many places like where we lived and where we now live are nitrogen sensitive areas. So there are strict limits on how much nitrogen you can put on a field, I suspect that this keeps the nitrogen levels in grass pretty low around here.
But if its starting to ferment then maybe adding in nitrates or ammonia will help kick it off, I have access to small bioreactors (1 ltr) so it might be worth seeing what happens if I help it with some heat in the jacket.
Maybe grass is the wrong material, there are alot of plants much higher in nitrogen (comfrey), I know in bio gas plants you can get hydrogen sulphide if it goes wrong. Maybe cow poo in a reactor under the right conditions would push things over to NOx gases?
Obviously I am wildly guessing so please jump in with sugestions

WGTR - 4-9-2015 at 08:01

Typically the idea is to avoid producing these gasses, so most of what I've read so far is geared towards that. This is
something that I've never tried myself, so I have little idea as to what the yield would be, or what the optimal conditions are.
Just on a whim, I added 0.9g of pulverized grass and root bits to a 3mL syringe; added 0.1g Mg(NO3)2 to 0.56g of DI H2O,
and suctioned it into the syringe; and then carefully removed as much air from the syringe as possible and capped it.

I got quite busy this morning and forgot the syringe at home. When things slow down today I'll bring it into work and incubate
it over the weekend. In years past when I put green grass clippings into a sealed syringe (without added water), within
several hours I start seeing gas fill up the syringe. I think this was mostly CO2, and it was produced mostly in the
beginning when there was still some oxygen left in the syringe.

When I'd add water to the grass, over the next several days the pH would drop. Adding Mg(OH)2 in small amounts
after a week or so would help raise the pH, since I was trying to make methane (I succeeded at the time).

After sitting overnight at room temperature, my syringe is still sitting there quietly, without producing any obvious amount of
gas. I probably shouldn't have added water to it.

My understanding is that nitrates eventually get reduced to nitrogen, with nitrite as an intermediate step. If the nitrite
levels are high enough, and other volatile fatty acids are being produced, some of the resulting nitrous acid decomposes, with
some NO escaping from the fermentation. If the environment remains sealed, then eventually nitrogen is the end product.
Buffering the pH lengthens the time that the fermentation continues, and produces more VFAs.

I think the problem with silo gas is more likely to happen naturally in drought-prone areas. Here in Texas it's a bigger problem, I
think. It sounds like you're used to being on and around farm operations, but I'll mention it for other's benefit, that
fermentations can produce some interesting and sometimes unexpected gasses. Methane, carbon dioxide, sulfides, nitrogen oxides,
and possibly even cyanides. So, be careful. Some cattle down here got turned loose in a field that had just recovered from a
drought, and most of them died from cyanide poisoning. It turns out the grass had developed high cyanide levels.

http://www.wired.com/2012/06/cyanide-and-poisoned-cows/

I don't claim to know much about the grass fermentation process, I just play around in the lab from time to time.

Little_Ghost_again - 4-9-2015 at 10:06

Quote: Originally posted by WGTR  
Typically the idea is to avoid producing these gasses, so most of what I've read so far is geared towards that. This is
something that I've never tried myself, so I have little idea as to what the yield would be, or what the optimal conditions are.
Just on a whim, I added 0.9g of pulverized grass and root bits to a 3mL syringe; added 0.1g Mg(NO3)2 to 0.56g of DI H2O,
and suctioned it into the syringe; and then carefully removed as much air from the syringe as possible and capped it.

I got quite busy this morning and forgot the syringe at home. When things slow down today I'll bring it into work and incubate
it over the weekend. In years past when I put green grass clippings into a sealed syringe (without added water), within
several hours I start seeing gas fill up the syringe. I think this was mostly CO2, and it was produced mostly in the
beginning when there was still some oxygen left in the syringe.

When I'd add water to the grass, over the next several days the pH would drop. Adding Mg(OH)2 in small amounts
after a week or so would help raise the pH, since I was trying to make methane (I succeeded at the time).

After sitting overnight at room temperature, my syringe is still sitting there quietly, without producing any obvious amount of
gas. I probably shouldn't have added water to it.

My understanding is that nitrates eventually get reduced to nitrogen, with nitrite as an intermediate step. If the nitrite
levels are high enough, and other volatile fatty acids are being produced, some of the resulting nitrous acid decomposes, with
some NO escaping from the fermentation. If the environment remains sealed, then eventually nitrogen is the end product.
Buffering the pH lengthens the time that the fermentation continues, and produces more VFAs.

I think the problem with silo gas is more likely to happen naturally in drought-prone areas. Here in Texas it's a bigger problem, I
think. It sounds like you're used to being on and around farm operations, but I'll mention it for other's benefit, that
fermentations can produce some interesting and sometimes unexpected gasses. Methane, carbon dioxide, sulfides, nitrogen oxides,
and possibly even cyanides. So, be careful. Some cattle down here got turned loose in a field that had just recovered from a
drought, and most of them died from cyanide poisoning. It turns out the grass had developed high cyanide levels.

http://www.wired.com/2012/06/cyanide-and-poisoned-cows/

I don't claim to know much about the grass fermentation process, I just play around in the lab from time to time.


Really really interesting thanks for the information.
I might just be able to add a couple of things, grass and silage here spoils because it gets too wet, so when cut they dry to leave around 30% moisture (thats practice and not science test) what the farmers do is cut and turn but pick up a day or so before they would for hay.
This gives you enough moisture to ferment without spoiling and producing hydrogen sulphide. No one has ever mentioned the nitrogen gases to me and dad who has lived on and around farms all his life hasnt heard or seen it. He is also a Biologist, he thinks that because in the uk they are very strict on the amount of nitrates you can spread on grass in many areas this would account for the lower nitrate in the grass here.
We have the rules for the nitrates levels because of the damage they can do to the river systems etc with algae blooms (uk is very wet and it washes into water courses).
I am also trying the grass fermentation, but first I am giving it two days of free air but a little heat (26c), i chose this because I figured the stage would need air like a silage pit does, then its closed up to exclude most the air, in practice the farmers I know wait for the pile to drop a couple of feet then they seal the pit off (this is called a clamp in the uk), its different from the wrapped bales but gives much better feed. So I figured I would compact the grass a bit and wait till the level drops a little then seal up.
I might also add cow shit (tiny amount) as going the methane route as a start point is a good idea.
I am going to use one of these

fermentation.JPG - 88kB
at the moment my grass is in a plain glass jar, but once it starts to do something I can transfer to the fer mentor. it should give me good control over the fermentation and i can add buffers ect via the septum or one the tubes. It also has a stir thing and any gas evolved could be piped into this


wash bottle.JPG - 43kB

I might add some form of wet sugar like honey or malases (again tiny amount). i will let you know if anything happens. If it start to ferment I will up the temperature to around 30C, I found out methane ect should stop at 40c, this was from a bio gas page about a car in the uk running from the gas made from chicken shit back in the 70's, I will try and find the page again

Little_Ghost_again - 4-9-2015 at 10:22

I will see what I can find on methane production, I know the nitrate cycle very well because I have kept fish from a very early age :D. I have seen aquariums go really bad (not mine) and produce hydrogen sulphide and the water goes a funny red black colour, this normally happens when a fish keeper goes away for two weeks and a friend feeds the aquarium with way too much food.
So I might add a little more maggot juice to the jar, i am thinking that in a dryer environment than an aquarium the sweet spot would be just before the hydrogen sulphide stage. Soooo this means fermentation and bacteria converting Ammonia - nitrite-nitrate then suddenly large increase in ammonia so the bacteria are overwhelmed a fair bit.
I honestly dont know what to expect as i have always tried to keep the cycle going right, I know if you close off early and dont have fermentation started you get methane, so somewhere between the two should make nitrogen gases, also in older aquarium systems they used a column that was dripped fed alcohol at a tiny rate and this converted the nitrate to nitrogen, it was the in thing ages ago until people got more into CO2 injection and nitrate stripping via plants (they do it really really fast under the right conditions).
Anyway time to stop waffling and see if I can track down some leads.
I might start at bio gas production and this could possibly go wrong and produce nitrous gases if the conditions are wrong?

Little_Ghost_again - 4-9-2015 at 10:25

found this.... http://www.nature.com/news/2010/100324/full/news.2010.146.ht...
Probably no use what soever but interesting considering the topic.

having read the original link again and going to the site about silage I can see some big difference between what they do and what I have seen done in both England and Scotland. I have no idea how helpful this is going to be though. The Uk has mainly two different ways of making silage, what is shown in the link with the brown gas is crosser to what we would call a silage clamp, these are pretty much like compost heaps that are allowed to heat up for a couple of days then sealed off with a covering.
The product from this is rich smelling and slightly damp, I cant describe the smell but it isnt unpleasant. I know its pretty high in sugars as it is normally used to supplement feed and just before calving time ect.
The other and probaly now the more common way is just like making hay except you harvest it very slightly moist and its wrapped air tight by the machine that bales it. These large bales are very common here and seen as black plastic large round objects all over fields in the uk (its being cut and done right now actually), this type of silage is much more dry and is used more as a general feed through out the year.
It also seems fields here are nitrated at different times to over there, in the uk ferts are spread just after the last cut of the year, then just before new spring growth then on occasion after the first cut.
I cant think of nor have I seen any situation where in the uk they would spray or use nitrates near a cut period, mainly I think because its cut during dry spells and it wouldnt make much sense to spread it then, plus also nitrate run off is highly controlled in both areas I have lived in.
But its really interesting to read the silage site and see the difference in the feedstock. I wonder if cattle breeds play a part? i think that amount of sugar and nitrate would bloat most breeds of british cattle, I know we cant have the ponies out on the spring or early grass because of the sugar content.
Funny I have grown up around farming but grass has always just been green stuff to me lol.



[Edited on 4-9-2015 by Little_Ghost_again]

Little_Ghost_again - 5-9-2015 at 14:43

Ok out of desperation mainly I came upon this but I am not sure its plausible, maybe I am just tired! Anyone want to comment on this?
https://www.google.co.uk/patents/US8327581?dq=making+nitric+...

The one thing i have totally overlooked is the reaction vessel, as you can see its mainly stainless steel! I have a busted glass version that I might be able to fix enough to use, the down side being it dosnt have a stiring mechanism so I would have to use normal stir plate and bar, I dont think that will work though.
I am not so much after the prize (although that would be great) But this has really caught my imagination once I got over the thinking of normal routes.
I now kind of see the point of this challenge

[Edited on 5-9-2015 by Little_Ghost_again]

WGTR - 7-9-2015 at 17:13

It's an interesting document, but I think it's referring to nitrates rather than nitric acid per se.

I hope it's possible to get good yields of NO from fermentations, but the approach might turn out to be a dead end, or not particularly high-yielding. That's an unfortunate possibility in research.

I'm still working on Dead Woodchuck. It's become much more refined, characterized, and...well...interesting than before. I spent the whole weekend 3D modelling different parts of it. It took so long, not because of the sheer volumes of work that I did on it, but because I'm a Solidworks beginner. I think that a beginner can do almost anything with Solidworks that a professional can do, due to the helpfulness of Youtube tutorials. A beginner, though (me), will probably take 10 times longer at the job than someone who knows what they're doing (not me).

I'm modelling everything before I build the final revision, but the latest prototype tests went well. The design still uses a high voltage pulse to trigger the main discharge. The amount of energy supplied by the high voltage is a small amount of the overall discharge, and is calculated to be within safe limits. The main arc current is supplied from a 65V power supply. Peak power is about 500W at 10A, but due to low duty cycle the average power is about 6W. This high peak power made it a challenge to design the filter network. All of the parts run cool to the touch, including the copper reactor tube and the electrodes, which are cooled with a small fan.

It's not really a contender for the competition since it uses a high voltage trigger, but it's a fun project nonetheless.

Little_Ghost_again - 8-9-2015 at 01:17

I think thats pretty neat! I can get to hydrogen sulphide really easy. That paper was a bit misleading but I have others that say something similar, I cant see it though. The only thing that makes me wonder its possible by fermentation is the fact methane reactors can suffer from NOx gases, I have to spend the next two days catching up on school work Grrrrr

no0ne98 - 10-10-2015 at 14:11

I don't know that this will fall under the challenge rules. However it's a good read that even covers nitric http://www.pyrobin.com/files/the_manufacture_of_chemicals_by...

j_sum1 - 10-10-2015 at 15:47

It's a nice reference.

aga - 11-10-2015 at 15:50

Which part of the Voltage Rule, or the workings of the Birkland-Eyde Process did you not read, look up or understand ?

Can somebody please complete this challenge soon, so we can get on with the AntiGravity Challenge ?

j_sum1 - 11-10-2015 at 16:01

Hey. I was just looking at my manganese-coated peanuts the other day.
I have everything I need and I need the bench space back so it will happen.

However, weekends are booked out for the next month and after that is crazy time at work. Then holidays. I might have a result by Christmas.

Little_Ghost_again - 12-10-2015 at 05:27



need to scale up and do pics so it can be verified. Turned out I was over thinking it :D

HOLD ON
I think its nitrous acid :(

[Edited on 12-10-2015 by Little_Ghost_again]

j_sum1 - 12-10-2015 at 05:32

Wohoohoo LGA. Looking forward to seeing it.

Little_Ghost_again - 12-10-2015 at 05:41

Quote: Originally posted by j_sum1  
Wohoohoo LGA. Looking forward to seeing it.


How do I check between nitrous acid and nitric?
Foof it I will take some and distill and see if it fumes red, man I wished I had my old fume hood working lol

[Edited on 12-10-2015 by Little_Ghost_again]

hamdusf - 27-10-2015 at 08:23

Quote: Originally posted by j_sum1  
Hey. I was just looking at my manganese-coated peanuts the other day.
I have everything I need and I need the bench space back so it will happen.

However, weekends are booked out for the next month and after that is crazy time at work. Then holidays. I might have a result by Christmas.

there is new way of make nitric acid


[Edited on 27-10-2015 by hamdusf]

aga - 27-10-2015 at 10:06

Quote: Originally posted by hamdusf  
there is new way of make nitric acid

Let me Guess !

#1 zap the air wth a high voltage arc
#2 distill a nitrate with concentrated sulphuric acid.

Oh the excitement.

Grantr - 29-10-2015 at 10:53

I know scrubbing exhaust was mentioned however I did not see reference to diesel.
Diesel exhaust has a high level of NOX due to lean hot combustion.


In the article below, The 2000 Volvo produced 112.5 grams of Nox in an hour idling at 1000 rpms and consumed .8 gallons of fuel. That seems like a good bit of nox.

http://nepis.epa.gov/Adobe/PDF/P10033E3.PDF

deltaH - 29-10-2015 at 22:51

Quote: Originally posted by Grantr  
I know scrubbing exhaust was mentioned however I did not see reference to diesel.
Diesel exhaust has a high level of NOX due to lean hot combustion.


In the article below, The 2000 Volvo produced 112.5 grams of Nox in an hour idling at 1000 rpms and consumed .8 gallons of fuel. That seems like a good bit of nox.

http://nepis.epa.gov/Adobe/PDF/P10033E3.PDF


Yes, though the concentration would be much lower than burning fuels that also contain nitrogen in their structure and at such low concentration, it might be hard to capture/concentrate it out of the total exhaust volume.

What would the exhaust volume be for a 1h idle? It's easy to calculate and then back calculate the ppm NOx given your figures.

Agari - 30-10-2015 at 14:50

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.
Procedure:
Cut open the cold pack and isolate the nitrate contained.
Add the nitrate salt to a beaker.
Add 200 milliliters of water.
Stir the mixture until it has fully dissolved.
Gravity-filter the mixture into a beaker.
Heat the solution in the beaker to near-boiling (I did not record temperature) and add the potassium chloride.
Bring the solution to a boil(with stirring!) and gravity-filter it into a beaker.
Place the solution in a home freezer to precipitate as many Potassium Nitrate crystals as possible.
Carefully remove the upper water layer from the beaker,then recrystalize the remaining KNO3 crystals from water.
Freeze the solution again.
If done right,the result should be white potassium nitrate crystals and yellow-ish water on top,remove the water and wash the crystals with ice-cold distilled water (Available at Walmart).
Dry out the crystals on a watch glass.
Nitric Acid Preparation:
Materials:
110 grams of Potassium Nitrate obtained previously.
Copper Sulfate.

Dissolve the copper sulfate in water.
Next,extract the carbon core from a single battery and attach a copper wire to it,connect our home-made electrode to the positive terminal of a power supply such as a battery.
Next,place a copper electrode at the bottom of the copper sulfate solution and connect it to the positive terminal of the battery. Suspend the carbon electrode above the copper electrode,make sure they do not touch!
If the carbon electrode erodes to the point of the solution becoming almost black,filter it out and subject the remaining solution to the same cycle using a different carbon electrode until it is clear. Once the solution IS clear,remove both electrodes,the liquid should be sulfuric acid. Alternatively,battery acid can be purchased at an auto-shop and distilled to maximum possible concentration, just writing that in case copper sulfate is prohibited.
I only used 60 milliliters of acid for my batch.
Now that we got sulfuric acid and potassium nitrate,it is time to prepare nitric acid.
Mix the potassium nitrate and sulfuric acid in a round-bottom flask in that order and (maybe?) add boiling stones.
Set up a simple distillation with the receiving flask placed in an ice bath and cover the entire apparatus with aluminum foil.Now bring the mixture to a boil at 83 degrees Celsius,continue the distillation until no liquid remains in the flask that used to contain potassium nitrate and sulfuric acid. Repeat the entire above process until 100 milliliters of nitric acid is obtained. I did not wear gloves during the experiment as the acid is likely concentrated to fuming(and likely to ignite the gloves), but rather has a solution of sodium bicarbonate and water nearby in case of contact with the acid.
Edit 1:I got around 25ml of nitric acid per run.


[Edited on 30-10-2015 by Agari]

[Edited on 30-10-2015 by Agari]

copper sulfate.jpg - 46kB



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[Edited on 30-10-2015 by Agari]

Edit:
Alternative method for making nitrates:
Obtain a tub of composted turkey manure (highly composted mixture of woodchips and turkey feces),6 kilograms is what I plan to use. Then add 4 liters of water,stir it with either a rod or manually. Then,gravity or vacuum filter the resulting mixture into a tub,discard to left-over insoluble material in the filter.Add a quart of a water and sodium carbonate solution at maximum concentration at room temperature. Boil off the resulting fluid ,do not include the precipitated calcium waste at the bottom of the tub in the boiling process. Next,reddisolve the left-over nitrate crystals in water. Gently boil the solution until the organic material precipitates at the sides of the container used to boil the solution,leaving a layer of nitrate at the bottom. Redissolve everything in water again,then use a separatory funnel to separate the darker nitrate layer from the lighter nitrate layer. Boil off the lighter layer. The resulting salt is now mostly nitrate,yet heavily contaminated.Do the same for the darker layer. Add just enough water to completely dissolve the salts.Mix the two solutions.
Boil off the nitrate extract,the potassium nitrate within should crystalize while other contaminants are largely in solution. After the boiling,place the resulting fluid in a freezer to further preipitate the nitrate,but not to freezing point. After 2 hours,remove the container with the fluid,there should be a layer of liquid above the nitrate crystals,decant and discard that liquid. Dry the crystals in the container on a watch glass with a paper towel to soak up the water. Do not hesitate to use water to remove the crystals,they will be dried anyways.
Alternative to Sulfuric Acid(This method must be performed with gloves,a respirator,and under a fume hood or outside):
Firstly,pplace 16 grams of dried sulfur powder in a beaker, then add a raft electrode consisting of 5 carbon battery cores, suspend the electrode above the sulfur,make sur ethey do not touch. This will be our anode. For the cathode,use a copper wire suspended below the top of the beaker. Now,use alligator clips to connect the electrodes to a car battery or other power supply,positive terminal for the anode,negative for the cathode. Next,add 200 ml of a 5 molar solution of hydrobromic acid to the beaker. Make sure that the carbon electrodes are sumbmerged at least 5 CM below the surface of the electrolyte(HBr) and that the cathode is under the surface of the electrolyte but at least 2 centimeters above the sulfur powder. Turn on your power supply and set the current to 2 amps. Should some sulfur start floating during the electrolysis process,stir the liquid until it is submerged. Water additions may be required should one electrolode end up too close to the surface. Run the electrolysis for 2-3 hours. After removing the electrodes,stir the mixture to dissolve all substances within and transfer it to an Erlenmeyer flask. Next, set up a reflux apparatus above the mixture and boil(With a hot plate)and reflux the liquid for half an hour. Then,stop heating and cooling and use a coffee filter to gravity filter the resulting fluid into an Erlenmeyer flask. Set up a simple distillation apparatus with stirring and heat the Erlenmeyer to 154 degrees Celsius until misting in the flask occurs and no more distillant comes over to the collecting beaker/flask.
Now,we must purify the sulfuric acid for it to be usable. Since most ehating mantles don't reach temperatures high enough to boil H2SO4,we must build one. For the mantle,we must unfortunately firstly buy special heating tape,I bought mine from Omega Engineering,model number STH051-040.
Roll up the tape and mold it into a cup shape to be able to accomadate a 100 ml round-bottom flask,you can use larger sizes to suit your needs. Once you have a satisfactory shape,use iron wire to hold the tape in place and maintain shape. Now,place the home-made mantle in a steel thermos to prevent heat loss during heating,then bend the iron wires to support the heating tape. Unfortunately,when the power cord is plugged in,there will be no way to regulate the current and the mantle will heat up at full power. To correct this issue, use either a light dimmer switch or a PID controller,but I had to buy a Variac auto-transformer for power control.
Now that our heating mantle is all set up,we can distill the sulfuric acid, a simple distillation apparatus with cooling(I actually used dry ice to keep the water cool) will do. The flask with the dark solution obtained from the simple distillation during our sulfuric acid synthesis must be connected to the condenser using high-temperature grease,normal grease will not work,it is also best to use high-temperature grease for the receiving flask for safety reasons. Next,turn on the heating mantle at low power and gradually increase voltage until condensate begins to come over into the collector. An important fact worth noting is that the flask wit the unclean acid must be filled only halfway,as thermal expansion will occur at such high temperatures. Due to water contaminating our distillant,we must collect when the concentration of H2SO4 is highest. To test the concentration,use a pippete to sample the distillant in the receiving flask and apply it to a paper towel. If nothing happens,the sulfuric acid concentration is still low and the contaminated distillant should be discarded. Keep performing this test until your paper towel begins to burn. Change the receiving flask to start collecting nearly pure sulfuric acid. Though our acid is highly concentrated,it is still not 98%. To determine when the acid concentration is at 98%,watch the receiving flask/beaker carefully. If the acid concentration is increasing,there would be oil-like patterns in the solution. Once this occurs,change out the receiver so that only the most highly concentrated sulfuric acid will be collected. Run the distillation until only 20% of the crude product remains in the heated flask,continuing the distillation after this point is likely to contaminate our concentrated acid. To create nitric acid,simply follow the original procedure once enough nitrate salt and sulfuric acid is obtained.

Before Aga calls me out on hydrobromic acid not being a common chemical, I am going to write a synthesis procedure for it as well.

Note:Use a conventional hot plate for this process,not the cutsom heating mantle built previously.
First,add 300ml of a 35% solution of sodium bromide(Available in pool stores) to an appropriate beaker,next add a stir bar and begin stirring rapidly, then add 200 grams of sodium bisulfate(Also available at pool stores),stir and heat until the sodium bisulfate dissolves. Once everything is dissolved,turn off heating and let the mixture cool to room temperature,then place the beaker in an ice bath. The products produced by the above reaction are sodium sulfate and hydrobromic acid. The ice cooling will precipitate the sodium sulfate out of solution. After an hour,remove the beaker from the ice bath and use a coffee filter to gravity filter the liquid into an Erlenmeyer flask,discard the remaining sodium sulfate crystals. To further purify the HBr,set up a simple distillation apparatus and distill off the hydrobromic acid.

Preparation of Nitric Acid.
Mix the nitrate salt and sulfuric acid in a round-bottom flask in that order and (not neccessarily) add boiling stones.
Set up a simple distillation with the receiving flask placed in an ice bath and cover the entire apparatus with aluminum foil.Now bring the mixture to a boil at 83 degrees Celsius,continue the distillation until no liquid remains in the flask that used to contain potassium nitrate and sulfuric acid. Repeat the entire above process until 100 milliliters of nitric acid is obtained. I did not wear gloves during the experiment as the acid is likely concentrated to fuming(and likely to ignite the gloves), but rather has a solution of sodium bicarbonate and water nearby in case of contact with the acid.

Pics soon to follow.


[Edited on 31-10-2015 by Agari]

Agari - 30-10-2015 at 14:52

I did not specify quantities because I did not record them during the production of sulfuric acid.

aga - 30-10-2015 at 15:02

Ooooh !

Sulphuric acid and a Nitrate Salt !

I fart in your general direction.

j_sum1 - 30-10-2015 at 16:30

To clarify, Agari...
Aga has specifically excluded readily available nitrated from this competition. The H2SO4/nitrate route is well known. The comp is for a novel route that is accessible to a wide range of people. Although long, the whole thread is worth a read. There have been a number of novel routes proposed. The execution of them remains a challenge. This comp is not as easy as it first appears -- if only because fo the investment of time to make progress. That said, the French Method, which was proposed early would be a viable method for nitrate production. It takes a long time and to my knowledge, noi one has actually attempted it. If they had, they would be well ahead of the pack by this stage.

Agari - 30-10-2015 at 17:47

Quote: Originally posted by j_sum1  
To clarify, Agari...
Aga has specifically excluded readily available nitrated from this competition. The H2SO4/nitrate route is well known. The comp is for a novel route that is accessible to a wide range of people. Although long, the whole thread is worth a read. There have been a number of novel routes proposed. The execution of them remains a challenge. This comp is not as easy as it first appears -- if only because fo the investment of time to make progress. That said, the French Method, which was proposed early would be a viable method for nitrate production. It takes a long time and to my knowledge, noi one has actually attempted it. If they had, they would be well ahead of the pack by this stage.

However,our drunkard implies that it is fine to MAKE the H2SO4 and nitrate salt:
Quote: Originally posted by aga  
You can't just Buy sulphuric acid, nor nitrate-based fertilizers to then go down the well-trodden 'distill to get conc nitric' route.
Even I could do that, so it would certainly not be challenging to you.
If you were to Make Sulphuric, concentrate it, and Make Nitrates, then distill, that'd be more like it.
The 'can't buy pure chemicals rule' does not include table salt, water, vinegar, booze, fags, hamburgers - stuff like that.
Bat guano would be fine, so long as the process includes details of where you might find bat dung.
Presumably in the Bat Cave, all over the Bat Mobile's windscreen.

The quote of relevance is "You can't just Buy sulphuric acid, nor nitrate-based fertilizers to then go down the well-trodden 'distill to get conc nitric' route.
Even I could do that, so it would certainly not be challenging to you.
If you were to Make Sulphuric, concentrate it, and Make Nitrates, then distill, that'd be more like it.", he is suggesting that it is OK to make the sulfuric acid and the nitrates,just not buy them.
Edit:the chemicals can also be bought at grocery stores,almost as easily as sodium chloride salt. Funny enough,my method seems to be a perfect fit for his "Exception policy" yet he dismisses it. Fuming nitric acid is mostly used for explosive synthesis,but can be diluted for more practical purposes.

[Edited on 31-10-2015 by Agari]

j_sum1 - 30-10-2015 at 18:01

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.

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