cold nitric recipe, another observation

[joekbit]

Using the recipe properly you will not have nitrate salts left to reuse, Laser Steve done a good job of calculating moles needed for the reaction and conversion, your salts would be sulfate salts (that could possibly hold some trapped nitric acid depending on how you performed the reaction, a little water will pick up any trapped nitric acid), the sulfate salts can be reused in other chemical reactions where you may need sulfates.

Reusing the sulfate salts they cannot be used again to make nitric acid.

Unless you made bisulfate, from using too concentrated sulfuric acid, and less nitrate salt in your reaction, then it has a hydrogen that can act similar to sulfuric in a chemical reaction.

I am not sure what you mean by reusing your salt, but if you do not have sodium bisulfate NaHSO4, and have sodium bisulfate Na2SO4 as a byproduct, you cannot reuse it to make more nitric, at least not the way I think you may be trying to.

I had a mistake in my post NaNO2 was changed. I took the salts that settled from the first batch (Steves cold nitric), added 100ml H20 and heated, not to boiling, just until the salts dissolved. I then added another 56ml concentrated H2SO4. stirring it, after it cooled I put it in my freezer 4 hours then decanted. That batch yielded more than the first and was far more reactive. Likely it is a bit more dilute causing it to react very fast on copper. I put a few drops from the second batch in my solution and the reaction scared me, I thought it was going to boil over. The nitric from the first batch was no where near as reactive

In any event I love the recipe.

 

[butcher]

Sodium Nitrate is NaNO3, and can easily be used to make nitric acid.
Sodium Nitrite is NaNO2, although you can make nitric acid from it, is not as easily done, (the nitrite needs to be oxidized to nitrate before you could make nitric acid with it).

You probably were using nitrate NO3^- (sodium nitrate) in your recipe. (nitrite would not have worked as you discribed).

Small details like the I or A in the spelling (nitrate or nitrite), or the number of oxygen's (NO3 or NO2) make a big difference in chemistry, you really need to pay attention to these small details.

Like in our last discussion where we discussed sulfate salts, Na2SO4 (sodium sulfate) and NaHSO4 (sodium bisulfate), where the name is only slightly different and the formula only slightly different, but how they react in a chemical reaction can be very different, where one could react as an acid, like sulfuric acid, with its hydrogen, in a chemical reaction.

I am not sure, but you probably did not get a good conversion, (trying to make it stronger) without the needed water to dissolve the salts properly for the sulfuric to react with, or using the wrong proportions or get a good conversion, or did not get the salts dissolved well enough for complete conversion from the mechanical process of your experiment...

if making cold nitric acid using Laser Steve's method following his instructions and quantity's will work well, changing the formula or how the reaction is done, will not make it properly, (like trying to make it stronger with this method), would not work. there are different methods to make stronger nitric acid, but they are not needed in recovery and refining, if you need it stronger or purer, using Steve's recipe, and distilling for purity, and evaporation of the approximate 50% to 68%, will work best in what we do, (or diluting your nitric when needed for base metals, making it easier to react with these metals).

Stronger is not always better.


You can also make nitric acid using more water, or a more dilute sulfuric acid, and get a good (weaker) nitric acid (which is not a problem when you use heat to dissolve metals), in fact it can even be better as less NOx gases are formed and less of your nitric acid is wasted).

For homemade nitric acid using the cold nitric acid method, water is an important part of the reaction.


In this science we really need to pay attention to the small details, they really make a difference.

 

[necromancer]

i love this post, my problem is that i am in canada & i do not think i can buy it here

stated here http://www.nrcan.gc.ca/explosives/restricted-components/9981 i am not sure if i can order it from the USA without having it confiscated by customs.

has anyone in canada found "Sodium Nitrate" (NaNO₃) in canada or had it shipped to canada ??

thanks in advance

 

[butcher]

I do not know your laws or rules there, but if you are not making or selling nitrates or nitric for making explosives maybe you can get it by following the rules or law for refining?

Have you studied the law or rules?

It would seem very strange to me if I could not make my own fertilizer and use it to recover a metal.
If I was not harming anyone.
Now the government wanting some of it as a tax, control purpose, to keep others safe from some idiot, or to gather the nitrate for a nations defense purposes, I can easily see, as this has always been done in history.

Surely it is not illegal to buy and use fertilizer, or for an industry to use chemicals.
Making and using explosives is another subject all together.
Do you not have guns in Canada? Can you buy bullets for your gun, if you follow the law?

Maybe you need another country, or work to change yours if things are that bad there, where you could be in big trouble if caught gathering the white crystals from your barn walls, and dissolving copper with them.

 

[necromancer]

I do not know your laws or rules there, but if you are not making or selling nitrates or nitric for making explosives maybe you can get it by following the rules or law for refining?

Have you studied the law or rules?

It would seem very strange to me if I could not make my own fertilizer and use it to recover a metal.
If I was not harming anyone.
Now the government wanting some of it as a tax, control purpose, to keep others safe from some idiot, or to gather the nitrate for a nations defense purposes, I can easily see, as this has always been done in history.

Surely it is not illegal to buy and use fertilizer, or for an industry to use chemicals.
Making and using explosives is another subject all together.
Do you not have guns in Canada? Can you buy bullets for your gun, if you follow the law?

Maybe you need another country, or work to change yours if things are that bad there, where you could be in big trouble if caught gathering the white crystals from your barn walls, and dissolving copper with them.

i have read that it's also used for curing meats. i still cant find it.
companies i have emailed that supply meat curing items only sell it mixed with salt & spices. i am going to go to a large meat curing manufacture next week to see if they have it. there 10 minutes away, thinking if i go to the receiving area & ask to speak to a supervisor i may find it ??

it's all worth a try

there is also this document:
http://www.nrcan.gc.ca/sites/www.nr...pdf/expl-expl/13-1057_Chemicals_Concern_e.pdf

today i will email the Ministry of Natural Resources Canada, Explosives Regulatory Division.
hope they don't come kicking down my door :x

 

[rickbb]

Since this post is about making your own, I've found this;

http://www.instructables.com/id/How-to-Make-Sodium-Nitrate-A-Potassium-Nitrate-Su/

 

[necromancer]

Since this post is about making your own, I've found this;

http://www.instructables.com/id/How-to-Make-Sodium-Nitrate-A-Potassium-Nitrate-Su/

thanks, i will have to start reading labels, wish i was a farmer

strange thing is, i can find the address of storage facility's where they store 200 tones or more in canada (50km from my home)
but i can not find a place to buy it.

http://globalnews.ca/news/492924/ammonium-nitrate-in-canada-locations-and-regulations/

 

[necromancer]

also found this.
http://chemistry.about.com/od/makechemicalsyourself/a/make-ammonium-nitrate.htm

 

[necromancer]

i feel that i should start at square one again.

http://goldrefiningforum.com/viewtopic.php?f=49&t=315&start=100#p104689
going to try get some "sodium nitrate" or "potassium nitrate" i made an agreement with the landlord of my shop, he said ""no ammonia in my building""

i have to respect him, he is a great guy & lets me get away with murder 8) . the agreement was because of it's use during world war 2

 

[jason_recliner]

Since this post is about making your own, I've found this;

http://www.instructables.com/id/How-to-Make-Sodium-Nitrate-A-Potassium-Nitrate-Su/

Of all the awful hurt-yourself videos on Youtube, Nurdrage is one chemist that seems professional and legit enough to trust and follow.
I've used the coldpack method recipe to make my sodium nitrate. It's just as easy for beginners as is using too much acid.

 

[joekbit]

Sodium Nitrate is NaNO3, and can easily be used to make nitric acid.
Sodium Nitrite is NaNO2, although you can make nitric acid from it, is not as easily done, (the nitrite needs to be oxidized to nitrate before you could make nitric acid with it).

You probably were using nitrate NO3^- (sodium nitrate) in your recipe. (nitrite would not have worked as you discribed).

Small details like the I or A in the spelling (nitrate or nitrite), or the number of oxygen's (NO3 or NO2) make a big difference in chemistry, you really need to pay attention to these small details.

Like in our last discussion where we discussed sulfate salts, Na2SO4 (sodium sulfate) and NaHSO4 (sodium bisulfate), where the name is only slightly different and the formula only slightly different, but how they react in a chemical reaction can be very different, where one could react as an acid, like sulfuric acid, with its hydrogen, in a chemical reaction.

I am not sure, but you probably did not get a good conversion, (trying to make it stronger) without the needed water to dissolve the salts properly for the sulfuric to react with, or using the wrong proportions or get a good conversion, or did not get the salts dissolved well enough for complete conversion from the mechanical process of your experiment...

if making cold nitric acid using Laser Steve's method following his instructions and quantity's will work well, changing the formula or how the reaction is done, will not make it properly, (like trying to make it stronger with this method), would not work. there are different methods to make stronger nitric acid, but they are not needed in recovery and refining, if you need it stronger or purer, using Steve's recipe, and distilling for purity, and evaporation of the approximate 50% to 68%, will work best in what we do, (or diluting your nitric when needed for base metals, making it easier to react with these metals).

Stronger is not always better.


You can also make nitric acid using more water, or a more dilute sulfuric acid, and get a good (weaker) nitric acid (which is not a problem when you use heat to dissolve metals), in fact it can even be better as less NOx gases are formed and less of your nitric acid is wasted).

For homemade nitric acid using the cold nitric acid method, water is an important part of the reaction.


In this science we really need to pay attention to the small details, they really make a difference.

yes I was, I double checked (nitrate) pellets, purchased from the science company. 99% about $6 USD

Doing some research, I found out it was shipped by Rocky Mountain Reagents. I went to their site and found 70% nitric, 2.2l for about $50 USD, but, as best as I can tell you need to call to place an order. So I am going to call them. Need some good nitric for AR solutions.

 

[Geo]

Need some good nitric for AR solutions.

Any solid nitrate can be substituted for nitric acid in an AR dissolution. For the dissolution to work properly, the solution needs extra water and to be heated. Just the temperature of steaming water will work. Add the solid nitrate as you would nitric acid, slowly and in increments. The reaction Involves the nitrate dissolving the metal and in doing this evolves NOx which is absorbed by the water making nitric acid in solution. It's not something that happens in steps, it happens almost instantaneously. It reacts exactly like nitric acid.

Most people needs nitric acid when dealing with silver. Using solid nitrates is a work around for those that can't source nitric acid. It's the first AR dissolution that I ever processed. It's something that, as a refiner, you will need to master along with other work around methods.

 

[joekbit]

Need some good nitric for AR solutions.

Any solid nitrate can be substituted for nitric acid in an AR dissolution. For the dissolution to work properly, the solution needs extra water and to be heated. Just the temperature of steaming water will work. Add the solid nitrate as you would nitric acid, slowly and in increments. The reaction Involves the nitrate dissolving the metal and in doing this evolves NOx which is absorbed by the water making nitric acid in solution. It's not something that happens in steps, it happens almost instantaneously. It reacts exactly like nitric acid.

Most people needs nitric acid when dealing with silver. Using solid nitrates is a work around for those that can't source nitric acid. It's the first AR dissolution that I ever processed. It's something that, as a refiner, you will need to master along with other work around methods.

Thank you very much Geo. It has been my observation that it is true, but you just answered the question I never asked. I have added solid NANO3 to solutions with just a bit of H2O as well, and noticed copper being dissolved and the usual brown nitrate gas being emitted. What I have done to prolong the reaction is placed another beaker into the solution beaker, with my hot plate on warm, then put cold water into the inner beaker. While watching I noticed with every drop of condensation that falls off the inner beaker the reaction gets more violent / or better. Eventually it will quit but the recycle through condensation helps a lot.

Correct me if I am wrong, the brown fumes are the NOx, the condensation captures the NOx creating weak nitric acid, as it drips back into the solution the cycle goes on. Yes or No? My reasoning tells me yes.

 

[Geo]

Your assumptions are correct. There is actually many ways of capturing the nitrogen dioxide and returning it to the reaction. A watch glass for a beaker works pretty good. There is glassware made for the job called a "reflux condenser". Since I do my first dissolution in coffee pots, I have found what seems like a mated pair that the bottom of one fits perfectly on top of the other. I fill the top one with ice and sit it on top of the reaction and it collects almost all of the brown-red fumes.