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Author: Subject: Nitric acid
nezza
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[*] posted on 3-11-2015 at 02:34
Nitric acid


As it is impossible to buy nitric acid of any sensible concentration within the EU currently I thought I would have a go at a synthesis. I know distilling alkali nitrates with sulphuric acid is a well known route but sulphuric acid is also unavailable so I tried distilling syrupy phosphoric acid with potassium nitrate using a glass retort until oxides of nitrogen became obvious in the retort. This yielded a very pale yellow liquid which reacted as expected with a copper coin. It fumes slightly in moist air and gives a very faint opalescence with silver nitrate so may contain some phosphate carried over. On titration it calculates as 12.5M in strength.



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[*] posted on 3-11-2015 at 08:18


Interesting to read that phosphoric acid can be used as well. How well did your glassware withstand the phosphoric acid? I read that hot phosphoric acid tends to corrode glass vessels and if this is true then that may reduce the usefulness of the method.

I did not expect that sulphuric acid would become unavailable. In the Netherlands it still can be purchased. The new EU regulations only are for nitric acid (and 6 other non-acid compounds). As far as I know, citizens still may buy and use sulphuric acid. The only thing is that unusual transactions (e.g. purchase of very large amounts) need to be reported.




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[*] posted on 3-11-2015 at 12:25


Very nice, makes me wonder whether using calcium nitrate (a common fertiliser) and phosphoric acid might work even better because of the low solubility of the product salt.



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[*] posted on 4-11-2015 at 14:59


Of course phosphoric acid does work, it is not volatile, just like sulfuric. I've tried substituting it for sulfiric when making both HNO3 and HCl, both times it worked like a charm.

But you better do not use glass retorts for this, this glassware is too good to waste it like that (hot phosphoric acid!). Use some cheap ass flask and a condenser.




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nezza
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[*] posted on 5-11-2015 at 00:47


Thanks for the warnings re glass and phosphoric acid. I have not noticed any problems with corrosion of the glass yet, but I'll keep an eye on it.



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[*] posted on 5-11-2015 at 13:43


The etching of glass with phosphoric acid is much less significant than, i.e. molten NaOH/KOH. It takes prolonged contact at elevated temps to get noticable damage(it starts to look like frosted glass.)

It will weaken the glass over time/repeated uses though so like others have said, avoid using any glassware you wish to keep around.
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[*] posted on 28-7-2020 at 15:02


Can I make nitric acid without distillation using calcium nitrate and phosphoric acid?
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[*] posted on 28-7-2020 at 22:42


Calcium dihydrogenphosphate have solubility 2g/100ml. So if you don't mind some calcium and phosphate contamination, yes.



If you are interested in aqueous inorganic chemistry look at https://colourchem.wordpress.com/main-page/

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[*] posted on 28-7-2020 at 23:29


Quote: Originally posted by woelen  
The only thing is that unusual transactions (e.g. purchase of very large amounts) need to be reported.


Is the reporting done with the customer's consent (so you fill in a form saying why you need it) or is it done quietly without the knowledge of the customer?

What about what retailers consider "suspicious" enquiries, such as purchases of large quantities to residential addresses or even business addresses that have no use for those chemicals, like 100L of conc. H2SO4 going to a hair salon? :o
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[*] posted on 29-7-2020 at 00:52


In UK acids are restricted because of acid attacks by all kinds of gangs.

I think it's great to have alternatives to sulfuric acid. It's great to always have alternatives in chemistry, because many times you've got already the reagents when you substitute a little. I hate it when synthesis specify a certain type of reagent or solvent and later I find out that some other reagent could have worked very well which I already had.

Btw if you need to use sacrificial glass, chinese glassware is perfect for that. They are quite high quality but cheap.

[Edited on 29-7-2020 by Fyndium]
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[*] posted on 30-7-2020 at 11:13


Quote: Originally posted by Whathappensif  
Quote: Originally posted by woelen  
The only thing is that unusual transactions (e.g. purchase of very large amounts) need to be reported.


Is the reporting done with the customer's consent (so you fill in a form saying why you need it) or is it done quietly without the knowledge of the customer?

What about what retailers consider "suspicious" enquiries, such as purchases of large quantities to residential addresses or even business addresses that have no use for those chemicals, like 100L of conc. H2SO4 going to a hair salon? :o


In sweden at least, and I would suspect the rest of the EU as well, you cannot buy any amount of sulfuric acid privately, unless you have a permit. The permit is actually no big deal from what I've read, you just need to show you have the knowledge and the right conditions to handle it. You pay a relatively small sum(like 200€ as I recall it), and present your case and why you need it, it gets reviewed and either denied or approved. I'm actually thinking about applying for this as I honestly think that hobbies which require sulfuric acid is a valid enough reason to be approved. This rule is probably just to deter those who would abuse it and make them feel like it's not worth the hassle.

Anyway, no need for sulfuric acid for HNO3 distilling. Sodium bisulfate works a charm, and is at least here widely available even in grocery stores as pool ph adjuster.

[Edited on 30-7-2020 by Junk_Enginerd]
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[*] posted on 30-7-2020 at 13:15


Over here in Spain sulphuric acid is not regulated at all and sold to individuals. Nitric acid used to not be regulated as well but now you apparently need a license to buy it. I still have a half-full bottle of 60% HNO3 that I bought online a while ago.

It seems hilarious (at least to me) that they regulate the sell of nitric acid because of it beeing an explosives precursor, anybody who has the knowledge to make explosives with HNO3 will almost certainly have the knowledge to make it from scratch.

Also, they should probably target more things like hexamine instead of nitric acid.
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[*] posted on 31-7-2020 at 00:49


It's intended to make the lowlife thugs lifes difficult. I don't know how many child blow up their hands and eyes with homemade explosives every year but I've been in impression that the number is dozens in Europe. An involved chemist will churn basically any chemical from anything.

Does anyone have any notes about bisulfite nitric acid? What are the reaction conditions? I've made HNO3 from sulfuric acid and a nitrate a long time ago few times with ease, but if I happen to need a reagent for nitrations it might come in handy due to being so OTC.
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[*] posted on 1-8-2020 at 06:08


Quote: Originally posted by Junk_Enginerd  
The permit is actually no big deal from what I've read, you just need to show you have the knowledge and the right conditions to handle it.
[Edited on 30-7-2020 by Junk_Enginerd]


By definition, if you need to provide something beyond nothing then it is only to your detriment. The question is how much is that cost going to be.

It used to be that Jewish people needed to register before Concentration Camps were set up. And then the murdering started and there was no where to run. It won't be as severe as this but what do you think the police will do, if there is a terrorist attack using nitrated organics and they had a list of all the people buying HNO3/H2SO4?

Quote: Originally posted by Felab  
Over here in Spain sulphuric acid is not regulated at all and sold to individuals. Nitric acid used to not be regulated as well but now you apparently need a license to buy it. I still have a half-full bottle of 60% HNO3 that I bought online a while ago.

It seems hilarious (at least to me) that they regulate the sell of nitric acid because of it beeing an explosives precursor, anybody who has the knowledge to make explosives with HNO3 will almost certainly have the knowledge to make it from scratch.

Also, they should probably target more things like hexamine instead of nitric acid.


Is possession of HNO3 without a license illegal in these countries (Sweden, Spain, UK, etc.?) Or is just purchase without a license? If you made HNO3 on your own like through the Birkeland-Eyde Process is it illegal?


Quote: Originally posted by Fyndium  
It's intended to make the lowlife thugs lifes difficult. I don't know how many child blow up their hands and eyes with homemade explosives every year but I've been in impression that the number is dozens in Europe. An involved chemist will churn basically any chemical from anything.

Does anyone have any notes about bisulfite nitric acid? What are the reaction conditions? I've made HNO3 from sulfuric acid and a nitrate a long time ago few times with ease, but if I happen to need a reagent for nitrations it might come in handy due to being so OTC.


Politicians want to be seen to do something when terror attacks happen. It doesn't matter whether the reality is that what they do is ineffective in preventing most future attacks.

It is like jails too. Politicians want to be seen to be tough on crime so they throw people for small things into prisons run by for-profit companies, so incarceration rates go up. The USA has the highest incarceration rate in the world 655/100k people.

The benefits of home experimentation is not so easy to quantify because their benefits are personal satisfaction (which society cares f- all about), possible synergies with work and new innovations/discoveries (<- society can't miss what you don't know they don't have)

As for kids doing stupid things, well why should my freedoms be curtailed because of someone else's stupidity? Maybe the reason why there are so many idiots around these days is because we keep on interfering with Darwinism.

[Edited on 1-8-2020 by Whathappensif]
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[*] posted on 3-8-2020 at 14:03


Per a preparation thread of mine and here https://www.sciencemadness.org/whisper/viewthread.php?tid=87... , Oxalic acid works to liberate an an acid from the underlying salt.

However, H2C2O4 may be control these days in select jurisdictions.
---------------------------------------------------

Whathappensif:

Don't worry too much about idiots in chemistry.

First mistake, they experiment with energetics in too large a scale (one should treat all energetics like there are drops of a HE).

Second, clueless and accidentally prepare large amounts of toxic gas indoors.

Third, create/experiment carelessly with highly flammable gases/liquids/solids (as in thermites) , with obvious consequences.

Fourth, when a substance is described as 'highly toxic', your goal in life should be to avoid it, and not attempt to prepare it.

Fifth, trying to ID an unknown gas by repeated inhalations, is far from the best/safest path.

......

Darwinism at its finest.

[Edited on 3-8-2020 by AJKOER]
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[*] posted on 3-8-2020 at 15:55


Oxalic acid can be made by oxidizing ethylene glycol.
The usual method is nitric acid but there are large range of ways to do it.
peroxides and permanganates are two options.
manganese dioxide and air at close to boiling should also do it (haven't tried that one).
Finally there is always extraction from rhubarb.
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[*] posted on 3-8-2020 at 18:17


In relation to the synthesis of nitric acid
https://m.youtube.com/watch?v=CqzrTxshOXM
Nurdrage video on using sodium bisulfate and sodium nitrate


I did not know that although oxalic acid as a cleaner is getting more popular now. The last synthesis I've seen is nitric acid and sugar which seems like a waste of nitric acid

Historically oxalic acid was obtained exclusively by using caustics, such as sodium or potassium hydroxide, on sawdust

Pyrolysis of sodium formate decomposes to form sodium oxalate and hydrogen then is converted converted to oxalic acid.

Sodium formate
reacting chloroform with an alcoholic solution of sodium hydroxide

Sodium formate may also be created via the haloform reaction between ethanol and sodium hypochlorite in the presence of a base. Also is the preparation of chloroform using alcohol instead of acetone



[Edited on 4-8-2020 by symboom]
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[*] posted on 5-8-2020 at 11:23


Quote: Originally posted by Whathappensif  

By definition, if you need to provide something beyond nothing then it is only to your detriment. The question is how much is that cost going to be.

It used to be that Jewish people needed to register before Concentration Camps were set up. And then the murdering started and there was no where to run. It won't be as severe as this but what do you think the police will do, if there is a terrorist attack using nitrated organics and they had a list of all the people buying HNO3/H2SO4?

Is possession of HNO3 without a license illegal in these countries (Sweden, Spain, UK, etc.?) Or is just purchase without a license? If you made HNO3 on your own like through the Birkeland-Eyde Process is it illegal?


Politicians want to be seen to do something when terror attacks happen. It doesn't matter whether the reality is that what they do is ineffective in preventing most future attacks.

It is like jails too. Politicians want to be seen to be tough on crime so they throw people for small things into prisons run by for-profit companies, so incarceration rates go up. The USA has the highest incarceration rate in the world 655/100k people.

The benefits of home experimentation is not so easy to quantify because their benefits are personal satisfaction (which society cares f- all about), possible synergies with work and new innovations/discoveries (<- society can't miss what you don't know they don't have)

As for kids doing stupid things, well why should my freedoms be curtailed because of someone else's stupidity? Maybe the reason why there are so many idiots around these days is because we keep on interfering with Darwinism.

[Edited on 1-8-2020 by Whathappensif]


You have some very ingrained, very American thinking. Civilians who aren't up to no good aren't persecuted here. Shit, most of the time I *have* been doing illegal things that certainly would have warranted a ticket or worse, and been caught doing it, it has always been a matter of "Well... does this guy actually have any malicious intent or did he just forget to consider this wasn't the best idea? Nah okay, dude, just don't do that, yeah?"

I've honestly not even heard of anyone that was punished for a harmless technicality here.

I don't think posession is illegal, but I honestly don't know for sure. I do know however, that there's zero possibility I'd ever face legal action for possession. Worst case I could imagine, if police for some strange reason would ever find it in my possession, I'd explain I'm a weirdo engineer with nerdy hobbies. I'm absolutely certain they'd shake their heads, laugh at me and tell me I should be careful.

I don't even think purchasing it is illegal. Selling it to unlicensed people is though.

While it's gotten worse lately, I gotta say that swedish politics is not anywhere near the beauty pageant or popularity contest that US politics seems to be from here. Making useless decisions and power moves in the name of "war on terror" etc doesn't fly here.

Well. Kids doing stupid things is a fact... And I can understand how the same society/government that sweeps up the pieces of said kids and pays for the damage would prohibit the means for that.

I honestly think the license solution is a decent compromise if I have to be adult about it. I don't like it, because I want my chemicaaals, but I can see how maybe it's for the best, since the license in question doesn't actually seem hard to acquire for a serious individual.
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[*] posted on 8-8-2020 at 10:29


If you are in EU you can order sulphuric 95%, nitric 60% and most other acids online.
Some require a copy of ID as its 18 year limit and a few require a filled in form with description of intentional use.
But otherwise no problems, just order and its get delivered to the door.
Im in Sweden too and its no problem order sulfuric acid or any other acids.
There is no customs on deliverys inside EU so ordered chemicals will not pass customs.

But if ordering isnt an option you could always make the nitric acid.
I would not recommend to try this without some lab experience as there are nasty fumes.
One can easily lead the fumes away but one should always take into consideration that unexpected accidents can happen.
A kitchen full of NO2 gas isnt fun at all.
Here are a video with preparation of nitric acid using the bisulfate method that doesn't need sulfuric acid.
He make a mistake and ruin the nitric acid in the video but that is easily prevented from happening.
https://www.youtube.com/watch?v=VLOY-Jp2w1I


[Edited on 2020-8-8 by Mateo_swe]
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[*] posted on 14-8-2020 at 07:17


I've got a question for all of you.

Do you do this outside? And how close are your neighbors and how close can someone come to your distillation?
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[*] posted on 14-8-2020 at 07:53


Quote: Originally posted by fdnjj6  
I've got a question for all of you.

Do you do this outside? And how close are your neighbors and how close can someone come to your distillation?


A question, not insults. That's an improvement.

To answer your question, I often gas people with solvent vapors at work. I actually let them come very close to the boiling solvent and people burn themselves regularly.
I know it'll annoy people (on Reddit!) but I dont feel responsible at all.
After all, it's my bosse's responsability: he bought those new kettles !




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[*] posted on 14-8-2020 at 11:44


Well at first in that thread I was trying to seriously help people and be civil but when met with such backlash being called a sissy, a bitch, a chemophobe, an asshole, and being laughed at by people whom the post didn't even concern, I'd argue that would make almost anyone pissed and insult them. I put a lot of time into that post and it was purely to help others not get in trouble, keep people safe, not have issues with neighbors, and not have to deal with the consequences like I did becuase I know for a fact that many people do things exactly like me and often even worse with less precautions. So I hope it was understandable that I was outraged. I admit I went a bit overboard and took things quite a bit too personally (life's not the best right now) but I was extremely fustrated and mad at how me trying to help would cause me to be bashed to pieces by people whom like I said, the post didn't even concern since they run heir labs so well (apparently). I don't care to expose myself to the chemicals, it's about others around me that I was getting at. I'm fine dealing with the consequences of my actions, I'm not fine with having others deal with the consequences of my actions. Does it kinda make more sense now?

And by the way depending on the solvent you're exposing them to, you really should change your ways. Ethanol? Meh. Toluene? Eehhh. Chloroform? No. Carbon tet? No. Benzene? No. Bromine (not a solvent I know)? No. You see what I mean? I'm not some lunatic contrary to what people thought of me in my previous post. I'm trying to help myself and others be responsible.
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[*] posted on 14-8-2020 at 12:49


I like to use carbon tet to dissolve my iodine crystals--much easier to intravenously administer it. I find 3cc's injected while enjoying a chloroform cocktail really helps me unwind after being exposed to whingers.

And I have distilled HNO3 (H2SO4 + NaNO3 method) more than once in my lab. Which is in my living space. Greased joints, metal keck clips, and a double necked receiving flask work great. The second neck is for the hose barb fitting, so I can like, you know, vent the damn rig outside. I'm just a dumbass redneck though..............




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[*] posted on 15-8-2020 at 00:04


Quote: Originally posted by arkoma  
I like to use carbon tet to dissolve my iodine crystals--much easier to intravenously administer it. I find 3cc's injected while enjoying a chloroform cocktail really helps me unwind after being exposed to whingers.

And I have distilled HNO3 (H2SO4 + NaNO3 method) more than once in my lab. Which is in my living space. Greased joints, metal keck clips, and a double necked receiving flask work great. The second neck is for the hose barb fitting, so I can like, you know, vent the damn rig outside. I'm just a dumbass redneck though..............


I like to put a condenser on the second neck to try to capture as much nitric acid as possible during the end phase when the contents of the boiling flask crystallize and throw off a lot of nitric acid vapors. Anyone reading this who wants to make nitric acid is advised to start with a small batch.

I understand that getting splashed in the eyes with nitric acid is somewhat less pleasant than getting a little chloroform or benzene in them.


[Edited on 15-8-2020 by JJay]
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[*] posted on 15-8-2020 at 00:17


Quote: Originally posted by fdnjj6  
I've got a question for all of you.

Do you do this outside? And how close are your neighbors and how close can someone come to your distillation?


Regarding the Nitric acid preparation in the video i linked.
This must be done either outside or in a flowhood.
It could be done inside but its very stupid and risky to do so.
If something breaks you would have the very nasty fumes inside and you would not be able to be inside to try vent the fumes without a gasmask.
These fumes will badly damage your lungs if inhaled so just do it outside if you want make nitric acid this way.
If doing the procedure correctly it will not be much fumes as most are dissolved in the water at the end of the PTFE tube and it will not be any problems to be around the procedure as long nothing breaks or a tube pops off.
If something unexpected happens, a flask breaks or a tube pops off there will be fumes but they will be dissolved in the outside air and they will not be any threat to neighbors except smell.
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