Making nitric acid failed

[JHS]

I decided to make some nitric acid two days ago.
using 400g of sodium nitrate at 98% (from Reggies regents on Ebay)
250 ml of h2o
500ml HCL
5 oz copper
350ml 10% peroxide
and ice
After setting this up in a 1000ml side arm flask absolutely nothing more than the HCL turning green ,absolutely nothing happened.
So, I set it up again.
A few days earlier, Cheryl picked up some High yield nitrate of soda for me.16%.
As soon as I poured in the HCL the reaction started,and an hour later it stopped.At that time I added 2 oz. more copper and 100ml more HCL,the reaction restarted and I got another 50ml of nitric acid using the 16% high yield.

Here in lies my problem.I used reggies regent sodium nitrate? to make some poor mans ar in order to disolve some tested and inuqarted 18k gold.I added heat and finally added some 68% nitric to desolve the gold.After i finished,I added some sulfamic acid to be sure that there was no more nitric in the solution.I tested the solution and got a positive test.When I added one teaspoon of smb,it reacted violently,foaming white,with no other color ,and almost flowing over.I rechecked for nitric with sulfamic acid and got no reaction.Oh and I did try to drop the silver.I also trippled the solution with dh20.
The first three batched I used sodium nitrate from a different supplier,and they went off without a hitch.

Disgusted with it,I set the solution aside and added a bunch of copper turnings.The turnings turned white,and I have no idea as to why.I then contacted reggies regents as to what he actually sold me. No reply.Now I fear that the solution is beyond my ability to retrieve the gold,and since I do not know what the white powder was that was suppose to be sodium nitrate ,I do not know how to proceed without a chemical analysis.
Just complaining,john

 

[mitchd]

What in the world do these items have to do with making nitric acid?
500ml HCL
5 oz copper
350ml 10% peroxide
You really need to do a lot of research before trying things like this.
Mitch.

 

[JHS]

The peroxide is put into a ice bathed container to catch the nitric acid.
the combination of copper HCL and sodium nitrate are put into a reaction chamber to create nitric acid.NerdRage on youtube
has a very good video on how to do it.
Suggest you view it.
thanks john
P.S. I always study until I UNDERSTAND....
http://www.youtube.com/watch?v=2yE7v4wkuZU

The second process is what I used.Hope this clears up your questions.

 

[JHS]

What in the world do these items have to do with making nitric acid?
500ml HCL
5 oz copper
350ml 10% peroxide
You really need to do a lot of research before trying things like this.
Mitch.

This is why I rarely share on this forum ,and I never proceed without research
john

 

[francis32]

The peroxide is put into a ice bathed container to catch the nitric acid.
the combination of copper HCL and sodium nitrate are put into a reaction chamber to create nitric acid.NerdRage on youtube
has a very good video on how to do it.
Suggest you view it.
thanks john
P.S. I always study until I UNDERSTAND....
http://www.youtube.com/watch?v=2yE7v4wkuZU

The second process is what I used.Hope this clears up your questions.

Nurdrage has some cool detailed videos, with a grave tone of voice

Francis

 

[francis32]

I use this process for my nitric, seems to work so far, gives about a rough 45-50% concentration, great for silver as is. Cost 12-13$ a liter to make.

I am newbie at this, been reading and trying for a few years, so far so good!

https://youtu.be/T-UkqAs2MWE

Francis

 

[Shark]

I tired making it the way John did with varied success, mostly hit or miss for me back then. I got some serious advice from butcher, after studying Lazersteves cold nitric thread. I then found metalicmario's post, and his video's, (the first one is posted by francis32). And have continued to use that method since then, and am very happy with it.

 

[mitchd]

I think you meant to write H2S04 and not HCL.
Mitch

 

[Shark]

The method John tried uses hydrochloric acid, copper and a nitrate salt, most commonly sodium nitrate. I can't fully explain it, (I am to chemistry illiterate) but the copper and hydrochloric acid plays the major part in replacing the sulfuric in this method. He is not trying to distill with this method, just use the reaction it's self to produce the nitric acid. The peroxide is used to trap a slightly larger amount of the gas that is produced slightly increasing the concentration of the acid produced.

 

[JHS]

I posted a video so you could learn perhaps a process you did not know about.
it is HCL

 

[goldenchild]

I saw the copper HCL method long ago but never tried it. It seems that no matter what, there will be some HCL contamination. I just don't see how you could avoid it. Especially using the first method in the nerd rage video. I am the owner of the video francis32 posted. I hadn't made nitric that way in a long time but did about 2 weeks ago with some sodium nitrate I found in the lab.

One thing I did differently this time was reduce the amount of nitrate used from 700gr to 650gr per 500ml. The reason being because I remember an obscene amount of salt being precipitated during chilling when using the original recipe. Lazer Steve's recipe called for 170gr of sodium nitrate per 100 ml of water. Even when reducing the amount like in the video (140gr per 100ml) there was still precipitated salt although less. This time using 650gr (130gr per 100ml) there was very little salt precipitation.

Another thing I did was boil the nitrate in a large SS cooking pot with a top to keep all water in and not evaporating into the atmosphere. Evaporating water will definitely skew the results. I did a large batch of 2600gr of nitrate and 2000ml of water. After boiling all the nitrate I poured all the solution into large glass containers. I then added the proper measured amounts of sulfuric acid to each container.

If I ever make nitric this way again I'll try 120gr of nitrate per 100ml of water. I think then I may be close to spot on with very little to no salt precipitation. I also recommend doing another chill after the initial decanting. Sometimes all the salt just doesn't want to ppt out the first time.

 

[Shark]

Sorry, goldenchild, but I had forgotten your user name here. I like the idea of the large stainless pot, I need to look for one. I have been using the method that butcher posted here,

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=19806&p=201787#p201776

and really like it with sodium nitrate, potassium nitrate is really bad about the salts caking up thick. I always lost the extra by trapping to much in the salts. Thanks for your video, it really helped me to visually understand a lot of what I was reading.

 

[francis32]

I saw the copper HCL method long ago but never tried it. It seems that no matter what, there will be some HCL contamination. I just don't see how you could avoid it. Especially using the first method in the nerd rage video. I am the owner of the video francis32 posted. I hadn't made nitric that way in a long time but did about 2 weeks ago with some sodium nitrate I found in the lab.

One thing I did differently this time was reduce the amount of nitrate used from 700gr to 650gr per 500ml. The reason being because I remember an obscene amount of salt being precipitated during chilling when using the original recipe. Lazer Steve's recipe called for 170gr of sodium nitrate per 100 ml of water. Even when reducing the amount like in the video (140gr per 100ml) there was still precipitated salt although less. This time using 650gr (130gr per 100ml) there was very little salt precipitation.

Another thing I did was boil the nitrate in a large SS cooking pot with a top to keep all water in and not evaporating into the atmosphere. Evaporating water will definitely skew the results. I did a large batch of 2600gr of nitrate and 2000ml of water. After boiling all the nitrate I poured all the solution into large glass containers. I then added the proper measured amounts of sulfuric acid to each container.

If I ever make nitric this way again I'll try 120gr of nitrate per 100ml of water. I think then I may be close to spot on with very little to no salt precipitation. I also recommend doing another chill after the initial decanting. Sometimes all the salt just doesn't want to ppt out the first time.

Well Goldenchild, it's a pleasure to meet you! Do you still have those rings

Your recipe was one of my first ever process more than 3 years ago. Making nitric was the easy part, de-noxxing it was the part I didn't understand. I wasn't too succesful at the time, I didn't grasp the concept too much, so I put my e-scrap away until recently now that I understand a bit more after reading, reading and did I mention reading!

I will keep using your recipe and follow your latest advice.

Thanks again!

Francis

 

[goldenchild]

Here's what I ended up with after a 50 pound run of sodium nitrate and 2 gallons of concentrated sulfuric acid. 26 liters or approximately 6.9 gallons. I'll call it closer to 7 gallons as I filled these 2.5 liter containers to the very top (first container only has 1 liter of nitric in it). The nitrate cost $95 shipped and the sulfuric was $51.88 after tax.

 

[Barren Realms 007]

Nice.

Did you run some of your crystals a second time?

 

[Anonymous]

Hi golden you say concentrated Sulphuric, what percentage was it please?

Jon

 

[geedigity]

Golden - What do you estimate the nitric acid concentration to be? I would assume that using less sodium nitrate in the same amount of water as Lazersteves method would result in maybe a weaker end product? Also, I thought that the cooling of the solution to -5 degrees C was to drop out most, if not almost all, of the sodium sulfate salt, leaving relatively clean nitric acid?

As a side note, Lazersteves method has worked very well in the past for me at least. More recently, I started using the method the OP started this thread about, but instead of using copper, I just use all of the plated items I want to reclaim the gold from and capture the gasses produced by running them through the scrubber. Yes, the solution the reclaimed gold is dissolved in is a very dirty solution, but after the first drop and a redissolve of the gold powder, the solution is pretty clean, although I usually repeat the refine process two more times using the HCL and sodium hypochlorite method.

I must say that I have yet to use any of the scrubber solution since I have been using the sodium nitrate and HCL method. Since the gasses produced by the reaction of sodium nitrate and HCL would seem to consist of NOx, Cl2 and maybe even some HCL, I now wonder if the scrubber solution is just a weak solution of AR that will ultimately break down over time? Humm

 

[goldenchild]

Nice.

Did you run some of your crystals a second time?

I didn't. And unfortunately I didn't use the ratios I said I would use above. The final yield would have been a bit more but I decided to go with what I've done in the past.
I would have no way of processing the ppt salt anyhow since I was boiling the water/sodium nitrate solution indoors. I would then put the solution in a 5 gallon bucket and add the sulfuric acid outside. I wouldn't re-boil the ppt salt inside again for obvious reasons. Until I get a good heat source for outdoors I won't be reprocessing the ppt salt.

One thing I did learn however is that even if I would have used the 120g nitrate to 100ml of water formula, it would still be way too much nitrate. With a little research I've seen a consensus that approximately 92 grams of nitrate is the upper limit that can be dissolved into 100ml of water. On the 4th 10 pound batch of nitrate I wanted to see what would happen if I simply put 10 pounds of nitrate in the 5 gallon bucket with same amount of water I had been using and then stirred it. The water was at room temp and I figured the heat created from adding the sulfuric acid would help even further in dissolving more nitrate.

After about 5 minutes of mixing (sulfuric acid in the mix) I realized that no matter how much I stirred there was going to be a certain amount of nitrate that could not go into solution. I let it cool and then froze it. Sure enough, there was still a very thin layer of salt ppt at the bottom of the containers. So even with the slight amount of heat comparative to boiling the water that the sulfuric created, it was still enough to put TOO much nitrate into solution (super saturation). This proved to me just how soluble sodium nitrate really is and just how wasteful my previous formulas were. In the future I will keep the cold nitric recipe just that. Cold. I won't waste time boiling the nitrate into water but will instead add about 95 grams of nitrate to every 100ml of water. The final yield should be substantially more.

Hi golden you say concentrated Sulphuric, what percentage was it please?

Jon

I use Rooto professional drain opener like pictured here. http://ecx.images-amazon.com/images/I/41V7xzNjZJL._SX425_.jpg True value is the only place I've ever found this brand. The MSDS says it's 93.2% concentration.

 

[goldenchild]

Golden - What do you estimate the nitric acid concentration to be? I would assume that using less sodium nitrate in the same amount of water as Lazersteves method would result in maybe a weaker end product? Also, I thought that the cooling of the solution to -5 degrees C was to drop out most, if not almost all, of the sodium sulfate salt, leaving relatively clean nitric acid?

As a side note, Lazersteves method has worked very well in the past for me at least. More recently, I started using the method the OP started this thread about, but instead of using copper, I just use all of the plated items I want to reclaim the gold from and capture the gasses produced by running them through the scrubber. Yes, the solution the reclaimed gold is dissolved in is a very dirty solution, but after the first drop and a redissolve of the gold powder, the solution is pretty clean, although I usually repeat the refine process two more times using the HCL and sodium hypochlorite method.

I must say that I have yet to use any of the scrubber solution since I have been using the sodium nitrate and HCL method. Since the gasses produced by the reaction of sodium nitrate and HCL would seem to consist of NOx, Cl2 and maybe even some HCL, I now wonder if the scrubber solution is just a weak solution of AR that will ultimately break down over time? Humm

The original recipe was claimed to be 50% concentration but I cannot confirm that. Maybe someone on here that is more familiar with stoichiometry can calculate it for us. You are correct about chilling the acid. It will precipitate the salts from solution leaving you with a very clean acid. My acid always comes out like water. I don't believe however adding less nitrate will reduce the concentration. Think about what was happening here. I was adding so much nitrate that the water couldn't possibly hold it all in aqueous form. This was evidenced in the video by the salt precipitating out before even adding the sulfuric acid. So after approximately 92 grams of nitrate per 100ml of water you would simply be wasting the nitrate. That is unless of course you are going to run the "left overs" again.

Look at it another way. When you make Kool-Aid and add sugar to it you can only put in so much before the sugar won't dissolve anymore right? You would be left with a super sweet juice with a pile of sugar at the bottom of the glass. A cup of juice with just the right amount of sugar mixed in would taste exactly the same as the cup with the pile of sugar at the bottom. The juice can only be so sweet. Now if you added water on the other hand then you would lessen the sweetness and would taste the difference as well. I know it's sort of a silly analogy but I think it works here.

And to put it into practice I've taken the liters that were made without boiling the nitrate into solution and added it to a whole bunch of GF watch band caps. Below are pictures. There is about 1 troy ounce of fine gold after refining worth of foils in this bucket. As you can see the solution is very clear and the digestion very complete. This batch worked just as well as any other batch I've ever made. I put enough tap water to cover the caps and then added the nitric. I put the lid on the bucket leaving a very small amount unsealed. 10 minutes later removing the lid out comes the B.A.R.C we are all so familiar with. Eventually all the base metal is digested.

 

[Shark]

Thanks for the updates. I hope to get back trying to make some nitric soon and will be adjusting my methods to adapt some of your ideas.