Making Nitric Acid, oopsie

[yellowfoil]

Thanks a lot for all your tips. I have no idea what all those numbers mean, but as long as I know what to buy, its Ok.

 

[Daniel0007a]

Well, I had trouble finding a good video on making tin(II) chloride without tin. 15 g of tin (II) chloride in 100 ml of 31% HCl, add 50 ml of distilled water and you may want to add tin metal. Why? Slowly with Air tin(II) Chloride converts into tin(IV) chloride and tin metal reduce the reaction. Since Hydrogen gas is given off you need to vent the gas regularly or it could spray corrosive tin (II) chloride and HCl all around you. I use amber bottles 220 ml with caps for many storing of chemicals. The shelf life of tin (II) chloride salt is normally 12 months and solutions only last 1-2 weeks.

 

[Daniel0007a]

This is vital if you want to qualitative measure gold in solution. Tin. I think that is what you mean correct?

 

[Yggdrasil]

Well, I had trouble finding a good video on making tin(II) chloride without tin. 15 g of tin (II) chloride in 100 ml of 31% HCl, add 50 ml of distilled water and you may want to add tin metal. Why? Slowly with Air tin(II) Chloride converts into tin(IV) chloride and tin metal reduce the reaction. Since Hydrogen gas is given off you need to vent the gas regularly or it could spray corrosive tin (II) chloride and HCl all around you. I use amber bottles 220 ml with caps for many storing of chemicals. The shelf life of tin (II) chloride salt is normally 12 months and solutions only last 1-2 weeks.

You can not make Stannous without Tin.
One can of course buy it in salt form, but it cost more of course.

You seem to very dependent of videos and detailed lists of what to do?
Better study so you understand why we do the different things we do.
There recipe you listed up here is way to much for any one in here apart from the professionals maybe.

There is no need to view videos for making Stannous.
That is over complicating things.
And you should not make more than 50ish ml at a time.
That will go bad long before most of us managed to use it up.
Take any HCl you have 29-38% add some 20+ ml to a bottle put in a few grams of Tin metal, preferably not a single button.
Add a bit of water and let it dissolve with open cap.
If you have HCl with less than azeotropic strength just use as is, no water needed.
When the bubbling has stopped, if there are still Tin metal it is ready.
If all is dissolved add a bit extra metal and it is ready.

 

[Daniel0007a]

Yes I do over complex things but however, this is a method of making it but you need to heat up tin (II) chloride carefully in HCl with good stirrering and heating.

 

[Daniel0007a]

My background is in BioPhotonics, Electronics, and Biotech but I studied 10 years (Photonics, Biotech, Water and waste management) and work too. I do have a lab with hot plates, chemicals, Digital scale, etc. Not a cheap hobby but I branched out a lot.

 

[yellowfoil]

For distilling dilute nitric, I basically started with a 24/40 glass distillation apparatus:
https://www.ebay.com/itm/262814098023(This was years ago, so I can't find exactly the same set now, but it came with 1000mL round bottom flasks. Make sure the first T has three ground glass joints, not two and an O-ring for a thermometer.)

You need to use a glass thermometer adapter for nitric, because the default rubber O-ring thermometer adapter above will catch fire with hot NOx fumes.
https://www.ebay.com/itm/262805544013
The first few Keck clips should be stainless so they hold up to the heat without deforming:
https://www.ebay.com/itm/262809616433
A "powder funnel" makes it easier to pour materials in and out of beakers without smearing them all over the ground glass joint:
https://www.ebay.com/itm/262810054160
You'll need to hold all the glassware securely. These two seemed to work nicely together:
https://www.ebay.com/itm/262809690057https://www.ebay.com/itm/262809601668
All above links are the same store, deschem. I have no connection with them except buying glassware a few times several years ago--they packed the glass quite well in a foam box and each piece encased in bubble wrap.

I circulate the cooling water with a little fountain pump, and scrub the uncondensed NOx with an alkaline gas scrubber. You'll need something that won't oxidize to seal the glass joints: concentrated sulfuric acid is traditional, which should clue you in as to the level of hazard here! I tried a silicone & castor oil based vacuum grease the first time, which nitrated itself a vivid red. This should all be sitting inside a fume hood. Use ceramic secondary containment vessels for when the glassware breaks while full of hot acid.

For what it's worth, my standard operating procedure for distilling nitric is here: Nitric acid not condensing.

Thanks for your tips Olawlor, will look into this as soon as possible.

 

[Sancho_n_Pedro]

You can not make Stannous without Tin.
One can of course buy it in salt form, but it cost more of course.

You seem to very dependent of videos and detailed lists of what to do?
Better study so you understand why we do the different things we do.
There recipe you listed up here is way to much for any one in here apart from the professionals maybe.

There is no need to view videos for making Stannous.
That is over complicating things.
And you should not make more than 50ish ml at a time.
That will go bad long before most of us managed to use it up.
Take any HCl you have 29-38% add some 20+ ml to a bottle put in a few grams of Tin metal, preferably not a single button.
Add a bit of water and let it dissolve with open cap.
If you have HCl with less than azeotropic strength just use as is, no water needed.
When the bubbling has stopped, if there are still Tin metal it is ready.
If all is dissolved add a bit extra metal and it is ready.

Trying to make a small sample of Stannous Chloride, but the HCL I have is only Patio cleaner with a % of between 10 - 20. Will this still be suitable, just don't add extra water?

 

[Yggdrasil]

Trying to make a small sample of Stannous Chloride, but the HCL I have is only Patio cleaner with a % of between 10 - 20. Will this still be suitable, just don't add extra water?

Should be ok. Only a little more time needed.

 

[FrugalRefiner]

Yep.

Dave

 

[Rreyes097]

I too have this cheap distillation setup. It has rubber stoppers for now until I upgrade but I tried last night to make a batch of nitric. And I think I ended up water because it didn't react with anything the distillation process there were no fumes at all. And now I'm doing a second try. 80g potassium nitrate 100ml sulphuric acid (battery acid). And so again no fumes here and it's bubbling quite nicely. So any ideas as to where I'm going wrong?

 

[eaglekeeper]

I too have this cheap distillation setup. It has rubber stoppers for now until I upgrade but I tried last night to make a batch of nitric. And I think I ended up water because it didn't react with anything the distillation process there were no fumes at all. And now I'm doing a second try. 80g potassium nitrate 100ml sulphuric acid (battery acid). And so again no fumes here and it's bubbling quite nicely. So any ideas as to where I'm going wrong?

Battery electrolyte isn't strong enough. Most hardware stores carry drain cleaner that's roughly 92% sulfuric acid and that's what I've used for years. Make sure it's sulfuric acid and NOT sodium hydroxide. Ace hardware usually carries Professional drain cleaner in a white container and Liquid Fire in a red one. I think Lowes carries a different brand.






F

 

[Rreyes097]

Battery electrolyte isn't strong enough. Most hardware stores carry drain cleaner that's roughly 92% sulfuric acid and that's what I've used for years. Make sure it's sulfuric acid and NOT sodium hydroxide. Ace hardware usually carries Professional drain cleaner in a white container and Liquid Fire in a red one. I think Lowes carries a different brand.






View attachment 55730FView attachment 55731

Wow thanks I thought battery acid was strong. Ok I'll try that

 

[Hascrack]

For distilling dilute nitric, I basically started with a 24/40 glass distillation apparatus:
https://www.ebay.com/itm/262814098023(This was years ago, so I can't find exactly the same set now, but it came with 1000mL round bottom flasks. Make sure the first T has three ground glass joints, not two and an O-ring for a thermometer.)

You need to use a glass thermometer adapter for nitric, because the default rubber O-ring thermometer adapter above will catch fire with hot NOx fumes.
https://www.ebay.com/itm/262805544013
The first few Keck clips should be stainless so they hold up to the heat without deforming:
https://www.ebay.com/itm/262809616433
A "powder funnel" makes it easier to pour materials in and out of beakers without smearing them all over the ground glass joint:
https://www.ebay.com/itm/262810054160
You'll need to hold all the glassware securely. These two seemed to work nicely together:
https://www.ebay.com/itm/262809690057https://www.ebay.com/itm/262809601668
All above links are the same store, deschem. I have no connection with them except buying glassware a few times several years ago--they packed the glass quite well in a foam box and each piece encased in bubble wrap.

I circulate the cooling water with a little fountain pump, and scrub the uncondensed NOx with an alkaline gas scrubber. You'll need something that won't oxidize to seal the glass joints: concentrated sulfuric acid is traditional, which should clue you in as to the level of hazard here! I tried a silicone & castor oil based vacuum grease the first time, which nitrated itself a vivid red. This should all be sitting inside a fume hood. Use ceramic secondary containment vessels for when the glassware breaks while full of hot acid.

For what it's worth, my standard operating procedure for distilling nitric is here: Nitric acid not condensing.

Actually got my thermometer adapter from them when I started and have been happy with it since... Also got a gas washing bottle which I connect between my distillation setup and my cheap amazon vacuum pump. I usually do shoot for RFNA in my distillation and have two amber reagent bottles I use for nitric, the first I store my RFNA in and the second I dilute down to 63%.

 

[Rreyes097]

Wow thanks I thought battery acid was strong. Ok I'll try that

I figured it had something to do with the acid but then again I've never used this chemistry set before.

 

[eaglekeeper]

I can't stress this enough......Hot 92% sulfuric acid is no joke..... it will scare you for life if any gets on your skin, even the vapors can damage your lungs. Just make sure you have protection.

 

[eaglekeeper]

Also got a gas washing bottle which I connect between my distillation setup and my cheap amazon vacuum pump.

Are considering a vacuum distillation for nitric? Too many risks, I haven't even attempted a vacuum distillation. If that lab glass fails under a vacuum with hot sulfuric...... I'm going to urge you to reconsider the risk/benefit ratio.

Besides, 99% of all your refining reactions absolutely require water... why waste your time and money to remove the water today, just to have to add the water back in tomorrow for the reaction. I would just distill everything over, the water is very helpful in carrying some of the nitric over.

Does your gas wash bottle use a frit disk or is it just small holes in the tube. If it has a frit, then I'm not sure how well it will hold up to FNA.

 

[Hascrack]

Are considering a vacuum distillation for nitric? Too many risks, I haven't even attempted a vacuum distillation. If that lab glass fails under a vacuum with hot sulfuric...... I'm going to urge you to reconsider the risk/benefit ratio.

Besides, 99% of all your refining reactions absolutely require water... why waste your time and money to remove the water today, just to have to add the water back in tomorrow for the reaction. I would just distill everything over, the water is very helpful in carrying some of the nitric over.

Does your gas wash bottle use a frit disk or is it just small holes in the tube. If it has a frit, then I'm not sure how well it will hold up to FNA.

Gas washing bottle uses small holes. I wouldn't trust a frit with FNA... I have had a flask fail when doing a filtration before when I was impatient and was using a vacuum pump designed for AC line purging, lost a 2000ml flask and learned my lesson. The vacuum pump I'm using is basically a reverse flow fish tank air pump that was ~$20 on Amazon and can't produce enough of a vacuum for glassware breaking to be a concern, if I remove heat from the system, the NOx fumes cooling actually causes a stronger vacuum if the system is sealed.

As for removing the water I don't add any. I know it helps carry the nitric over but I've found that as long as I keep everything before my distillation column well insulated then it keeps things moving at a reasonable rate, the vacuum mainly serves to keep the foaming from occurring and allows the boiling flask to be filled to a higher level which also helps with the speed of distillation.

For me the reason I distill FNA is for storage. I tend to take a day and just do nitric distillation until I have enough to fill my 1000ml FNA reagent bottle completely and my 1000ml 63% bottle to about 650ml. When I dilute the acid I always pre chill the acid and distilled water before dilution and keep it below room temp while diluting.

 

[Striker578]

So I was Making a batch of nitric acid ,

With Sodium Potassium , and Sulfuric Acid ,
And distilling Nitric Acid as it goes
( mostly like this video )

The oops came from my distilling apparatus,,,
The cheap one I have has a thermometer on top thru a unknown material rubberlike stopper

This stopper didn't like the nitric acid vapor and mostly all drip down in the flask

Did I accidently produce anything explosive?

 

[tiggertree]

I used the same cheap distillation set.
My thermometer adapter dissolved too.
You will need a sealed glass adapter if you want to use a thermometer.
The green plastic keck clips will not last long either.
The stainless clips from aliexpress are better.