Cold Nitric recipe problem

[boboxx]

Hello folks : )

I'm having a hard time producing some cold nitric using lazersteve recipe. I have tried twice so far and they both resulted in a bowl full of hard salt.
I’m using Potassium Nitrate (99+%) from Duda Diesel on ebay and Liquid Lightning (94.19% http://www.liquidlightning.net/download.php?act=download&docId=124) for my sulfuric acid source from the local hardware store.

When I’m dissolving the potassium, there is a gel like residue that sticks to the side of the pot and also forms a small film on top of the water. Is this normal?
Here are some photos I took while doing the process. The end result of this is that I want to be able to process my used jewelry gold and silver scraps so I can reuse them in new material in casting or forging.

 

[Noxx]

Dissolution of your KNO₃ should yield a colorless solution. No gel should be present.

Maybe you have some weird things in your water. Try with a small amount of bottled or distilled water.

 

[eeTHr]

boboxx---

Does Liquid Lightning have buffers in it?

Fresh battery acid from an auto parts store is nice and clear, but it's only around 30-33% concentration.

You can adjust for that by using proportionately less water. I tried it using no added water, and just adding the potassium nitrate to the battery acid. I don't know what the exact concentration of the resulting nitric was, but I was trying for 35% (which is the same as a 50-50 mix of 70% nitric with water), and I think it was close.

 

[boboxx]

The water I was using was RODI, It's the water I use for my salt water reef aquarium I will try it with distilled water.
I'm not sure if there are any buffer in the Liquid Lightning, but it has a redish/brown color. The gel is forming before I add the LL so I will see if it makes a diff with the new water first.

Thanks!

 

[TXWolfie]

The water I was using was RODI, It's the water I use for my salt water reef aquarium I will try it with distilled water.
I'm not sure if there are any buffer in the Liquid Lightning, but it has a redish/brown color. The gel is forming before I add the LL so I will see if it makes a diff with the new water first.

Thanks!

Dont mean to stick my nose where it might not belong, but i have had salt water aquria reef tanks mostly. Been out of the loop for sometime but never heard of RODI or dealt with it. But if your using salt water or an additive you might be adding minerals that will mess with your solution that might be your difficulty. Once again I am no chemist but if solutions are in need of being precise a foreign substance might mess you up.

 

[TXWolfie]

The water I was using was RODI, It's the water I use for my salt water reef aquarium I will try it with distilled water.
I'm not sure if there are any buffer in the Liquid Lightning, but it has a redish/brown color. The gel is forming before I add the LL so I will see if it makes a diff with the new water first.

Thanks!

Dont mean to stick my nose where it might not belong, but i have had salt water aquria reef tanks mostly. Been out of the loop for sometime but never heard of RODI or dealt with it. But if your using salt water or an additive you might be adding minerals that will mess with your solution that might be your difficulty. Once again I am no chemist but if solutions are in need of being precise a foreign substance might mess you up.

Ok I looked it up and a big DUH to myself Reverse osmosis ( never used it) equiptment that doesnt make sense onto why that happened, since reverse osmosis takes out all that things and makes it pure water.

 

[eeTHr]

boboxx---

There is obviously something in there besides potassium nitrate and water.

If it's not coming from your water, and it's not already in your glassware, then it's coming from the potassium nitrate.

 

[eeTHr]

boboxx---

When I first looked at your photo, the solution appeared to be orange-brown colored. But now I see that could be just the color of your glass pot.

So, is the solution clear or colored?

Also, it looks like the liquid level started out much higher in the pot than it is in the photo. Did lots of water evaporate out of it?

 

[boboxx]

Yes the pot is not clear : ) looking at the photo, photo #1 is the one with Potassium and Sulfuric cooling down, the salt creep around the edge is from when I was stirring it.
photo #2 is the one on the stove after the potassium has been dissolved... just before moving it outside, and you can see the jelly skin next to the spoon.
I will make a new batch tomorrow with distilled water, I doubt it’s the potassium as I have seen a lot of people on here ordering the same thing and I just received this the pas Friday so it’s fresh!

@TXWolfie, yes RODI is reverse osmosis deionized : ) I use it as a base then add my salt mix. This prevents a lot of algae!

 

[Geo]

this is not an efficient process for making nitric acid.i will describe a process quickly that will make a very strong nitric acid without a lab.you will need two large glass bottles,one with a larger mouth so the mouth of the smaller will fit inside the mouth of the larger.place a hotplate on level ground,place a iron pan on the hotplate and fill with sand.best to use the large wine bottle that is shaped like a ball for the reaction vessel and place 1 cup of potassium nitrate and 1 cup concentrated sulfuric acid in the wine bottle and lay it on the sand on its side.place a container(Styrofoam cooler works best)in front of the reaction vessel and place ice in the bottom a couple of inches deep.now lay the receiving vessel (or large mouth bottle) on its side in the cooler and slide together till the small mouth of the one is in the large mouth of the other (at least an inch or two) then cover the large mouth bottle with ice.do NOT create a seal between the bottles to let pressure escape,but DO place a dry rag around the neck of the small bottle and let it over lap large mouth to cut down on fumes.NEVER BREATHE THE RED FUMES!!this is nitrogen dioxide gas and is poison in every way.gently raise the temp on the hotplate till solution come to a gentle boil.nitric acid will condense on the cold glass on the inside of the receiving vessel.the solution will stop boiling when all the nitrate has been converted.keep a watchful eye for this to happen so you can reduce the heat as the solution will keep heating until the glass fails.when reaction is complete turn off hotplate and allow to cool completely before disturbing.gently separate bottles careful not spill the newly formed nitric acid and notice the solution in the other bottle is now a solid in the form of salts.if you try this do it outside and away from people and pets.use a rated extension cord so you can unplug at a safe distance if the glass fails.always wear safety gear when dealing with acids and if you must be close to this reaction wear a respirator rated for airborne organic acids.

 

[TXWolfie]

@TXWolfie, yes RODI is reverse osmosis deionized : ) I use it as a base then add my salt mix. This prevents a lot of algae!

Thats why I never got into it or used it, my rule of thumb is 1 - 1.5lb of live rock per gallon of water not actual tank water but tank gallon. I would also look for uncured live rock, this would give me the possible goodies hiding inside the rock. I once bought a 3lb piece and got a small octopus out of it. then about 5 days would add only corals. About a month later would slowly add fish and only 1 fish per 10 gal of water. I never had algae blooms with this method...... Hey wait this is a refining forum not a fish tank forum.....
We now return uninterrupted to our regularly scheduled forum ... back to you Bob :lol:

 

[necromancer]

this is not an efficient process for making nitric acid.i will describe a process quickly that will make a very strong nitric acid without a lab.you will need two large glass bottles,one with a larger mouth so the mouth of the smaller will fit inside the mouth of the larger.place a hotplate on level ground,place a iron pan on the hotplate and fill with sand.best to use the large wine bottle that is shaped like a ball for the reaction vessel and place 1 cup of potassium nitrate and 1 cup concentrated sulfuric acid in the wine bottle and lay it on the sand on its side.place a container(Styrofoam cooler works best)in front of the reaction vessel and place ice in the bottom a couple of inches deep.now lay the receiving vessel (or large mouth bottle) on its side in the cooler and slide together till the small mouth of the one is in the large mouth of the other (at least an inch or two) then cover the large mouth bottle with ice.do NOT create a seal between the bottles to let pressure escape,but DO place a dry rag around the neck of the small bottle and let it over lap large mouth to cut down on fumes.NEVER BREATHE THE RED FUMES!!this is nitrogen dioxide gas and is poison in every way.gently raise the temp on the hotplate till solution come to a gentle boil.nitric acid will condense on the cold glass on the inside of the receiving vessel.the solution will stop boiling when all the nitrate has been converted.keep a watchful eye for this to happen so you can reduce the heat as the solution will keep heating until the glass fails.when reaction is complete turn off hotplate and allow to cool completely before disturbing.gently separate bottles careful not spill the newly formed nitric acid and notice the solution in the other bottle is now a solid in the form of salts.if you try this do it outside and away from people and pets.use a rated extension cord so you can unplug at a safe distance if the glass fails.always wear safety gear when dealing with acids and if you must be close to this reaction wear a respirator rated for airborne organic acids.

as i am rereading through the old post i came across this. i was wondering if you still use this same method & if there is any videos of the process ?

i am not getting a true picture in my head reading it.

 

[rickbb]

I believe he is describing a method to distill the nitric oxide vapor from the nitrate/sulfuric mixture, boil it and capture the vapor in an iced bottle where it condenses back to liquid and pure.

 

[necromancer]

below is a drawing of what i am seeing in my head after reading Geo's method.

the drawing is not exact (can not turn items to fit correctly)

what i don't get is the part about:

do NOT create a seal between the bottles to let pressure escape, but DO place a dry rag around the neck of the small bottle and let it over lap large mouth to cut down on fumes

i would have thought that the HOT vaper would need the COLD to condense into a liquid before dripping into the capture vessel ??

or do i have this all wrong ??

 

[Geo]

Almost but not exactly. It is actually two bottles. The neck of one fits inside the neck of the other bottle. The temperature difference in the receiving container will cause the pure nitric acid to condense and puddle up the the receiving bottle. Both bottles are laying on their sides. In the illustrations I was following showed a bottle with bent neck and a stopper for the reaction vessel and the receiving vessel was the same type bottle but with a larger neck. I used this method a long time ago and nearly killed myself doing it. I didn't understand the dangers of NO2. This is a "set and forget" type of reaction. For better or worse, once started, it's better to stay away from the reaction. The illustration can be found in the anarchist cookbook. Because of this, I can't recommend anyone repeat it. I understand the need to source what you can from where you can but this process should be considered a last resort and remember, you are taking your life into your own hands.

 

[necromancer]

that is clearly understood !! thanks Geo.

i will try the method posted by lazersteve, it seems to be my best bet, all i need is the Nitrates. major pain locating it in canada.

 

[Geo]

This is a homemade condenser I made with PVC and the glass tube came from a sign company. I pay a couple of dollars per piece. I used the equivalent of 3/8" glass tubing. I used a propane torch to heat and bend the glass tube into a 90° elbow.

 

[necromancer]

i can build that easy enough. so a straight piece of glass tube through the centre of the pvc tube ?? (not including the bend on the one end)

how long is the pvc tube ? 24 or 30 inches ?

there is a neon sign maker by my shop, sure he will have the glass tubing needed.

 

[rickbb]

You could also use a long coil of PVC tubing, coil it around in a spiral inside a bucket or such. Fill the bucket with ice water and run the vapors through it and then out into a catch flask.

Any basic distillation type of design should work, just use acid resistant materials and don't stop up the system to cause it to build up pressure.

Some examples here.

https://www.google.com/?gfe_rd=cr&ei=vRZpVMroE-nf8geM-4HwBA&gws_rd=ssl#q=distillation%20apparatus

 

[rickbb]

As for nitrates, I use a brand of stump remover sold at the big box home and garden stores. It's potassium nitrate, not sodium but it works.