Questions about lazersteve's cold nitric acid recipe

[Anonymous]

you make have had them freeze to fast, did you let cool to room them first?
I have a tall skinny glass that I wrapped in insulating foam to have the solution cool from the bottom up.

Jim

 

[2002valkyrie]

you make have had them freeze to fast, did you let cool to room them first?
I have a tall skinny glass that I wrapped in insulating foam to have the solution cool from the bottom up.

Jim

I missed the slow cool section. Can I reheat the solution and try again?

 

[Anonymous]

I would leave it thaw all the way out then you will have to gently heat to get everything back to the starting point.

Also, maybe you could add a little water and use it like poor mans nitric, it just wont be too good for stuff with silver/lead/cadmium in it.

Jim

 

[lazersteve]

Valk,

The solution takes about 3 hours in an upright freezer for the crystals to form. Mine stayed liquid until this point using the exact same chemical sources I sent you. I'm not sure why yours formed a gel.

Are you sure your getting to -5 C ?

Did you use distilled water?

I guess I'm going to have to break down and do a video of this process once and for all. I've been putting it off for some time now, I might as well get to it.

Steve

 

[Palladium]

I guess I'm going to have to break down and do a video of this process once and for all. I've been putting it off for some time now, I might as well get to it.

Steve

Alright !!!!
A new vid.

 

[lazersteve]

I'm doing the reaction tonight to be 100% certain of the ingredients I sent him.

My previous cold nitric batches have used the Bonide brand Nitrate of Soda and I sent him some Sodium Nitrate I bought from dudadiesel (sp?) on Ebay. Maybe the nitrate is not sodium nitrate. I'm sure it's a nitrate as I have used 15+ pounds of it for Poor Man's AR without any problems. I'm using Bisulfate from the same container I poured his out of.

I added the water and bisulfate to an empty 1 L beaker and put the heat on Simmer.
With lots of stirring and swirling I was easily able to dissolve the bisulfate in less than 30 minutes without boiling the water.

Next I added all of the nitrate and stirred and swirled until it was all dissolved. The water was steaming, but still not boiling. This step took another 7-10 minutes.

Next I filtered the hot solution.

Here's a photo of the hot (90C+) filtered solution of 167 mL distilled H2O + 120 grams of NaHSO4 + 85 grams of NaNO3 from dudadiesel. Total volume with 2- 5mL rinses of the beaker and filter is right about 250 mL.

The solution is 100% clear and free of sediment/crystals.

I'll put it in the freezer once it reaches around 50C.

More photos later.

Steve

 

[Oz]

Steve,

I have made a good bit of biodiesel and you may find that their source has changed as the chloride impurity is not so critical to their process.

 

[2002valkyrie]

Valk,

The solution takes about 3 hours in an upright freezer for the crystals to form. Mine stayed liquid until this point using the exact same chemical sources I sent you. I'm not sure why yours formed a gel.

Are you sure your getting to -5 C ?

Did you use distilled water?

I guess I'm going to have to break down and do a video of this process once and for all. I've been putting it off for some time now, I might as well get to it.

Steve

Thank you Steve, But Murphy's Law seems to be written just for me. I will wait for your instructions and results that I should expect to achieve before I try again.

 

[lazersteve]

I fell asleep last night a left the mix in the freezer over night. The last check I made was @12:30 last night (4 hours in the cold) and no crystals had formed yet.

This morning the mix was a slush like consistency, very different from my other batches using the Bondie brand nitrate. Now that I see the slush, I suspect it is hydrated sodium sulfate as the compound will absorb 10 moles of water per mole of sulfate. This leads me to believe there is a difference in the nitrates that I used.

What gets me is the dudadiesel stuff is labeled 99% Technical grade sodium nitrate. Maybe it has been relabeled? It works great for distilling nitric and for poor man's AR, but it appears to be different when it comes to the cold nitric recipe.

I'm going to run a new batch using the Bondie nitrate again just to be 100% sure. Previously when I've done the experiment the sodium sulfate formed very nice long clear crystals in the flask once it reached the -5 C.

As for the slush, I let it thaw to around 10C and filtered off the clear layer. This layer will go back in the freezer and we will see what happens next. The slush can also be distilled in a glass rig to get the nitric out, so nothing is really lost. If you are going to distill in the end, there is no sense in freezing first as this just adds an extra step.

I'll post more when I have some real conclusions.

Steve

 

[lazersteve]

Update:

I started a control cold nitric acid experiment using the Bonide Nitrate of Soda, and immediately noticed a big difference. The hot solution is not thick like syrup as the dudadiesel solution was and secondly the nitrate actually fizzes when added to the hot water and dissolved bisulfate.

I also detected a slight odor of NOx after adding the niter. It foamed about 2" thick in a one liter beaker when added. After the niter dissolved the foam all but disappeared.

These observations tell me already that the dudadiesel nitrate either has an additive or is a less soluble form of nitrate. I suspect it may be potassium nitrate instead of sodium as the sodium sulfate has very a unique solubility curve which makes this cold reaction possible. Maybe he mixed up the potassium nitrate with the sodium nitrate for my order? I'll send him an inquiry once I have the results of the freezing stage.

More to come later today.

Steve

 

[butcher]

I have noticed some difference in the nitrates I wonder if they are not changing them with other chemicals, or something?

 

[lazersteve]

The Bonide nitrate batch has been freezing since this afternoon. I checked it a few minutes ago and noticed it too is turning slushy. This leads me to believe that the previous batches I did, where I monitored the crystal growth periodically, turned out the way they did because I poured off the liquid once I saw crystal growth.

I think both nitrates are basically the same now that I have seen similar results out of both.

The solution to the problem of slushy or gel like formation is pretty straight forward. Simply thaw the solution to around 10C and pour off the liquid portion from the powdered salt that remains. You can vacuum filter the salt out with a glass frit if you have one.

Once you have thawed and poured off the clear liquid, refreeze the liquid. The second freezing should be monitored closely. When long clear crystals have formed, pour off the resulting dilute nitric acid. I have noticed that with this second freezing step the crystal grow relatively fast once the solution cools down. The crystals formed will be long and glass like.

Here's a shot of some of the crystals after the second freezing:

I'm going to distill the resulting acid and post the actual yield of acid and left over salt in the distilling flask in the liquid from the second freeze.

Here's a shot of the second crop of crystals after the second freeze:

Steve

 

[Anonymous]

I know that I had braught this up before, but if you cool/freeze to quickly the liquid gets overtaken by the crystal front.
I am pretty good at this because I work on water purification units that actuall freeze water then discard the waste water.
One of the main things that goes wrong is the unit freezes to fast encapsulating the waste water.

Jim

 

[lazersteve]

Here's a shot of the poured off nitric after adding a small silver nitrate crystal (~0.5 gram) and stirring then settling.

and the solids after pouring off the cloudy acid into a filter.

The large chunk on the right is what's left of the original silver nitrate crystal. About 1/3 of it dissolved.

Steve

 

[Anonymous]

Steve,
Working out a small batch of this bisulfate process today. Seems to be going according to plan. I cut the quantities based to work with 20 ml of water. I let it cool to room temp and a lot of the salts settled out. I know have a clear but cloudy solution that I am going to put in the freezer now.

Seems to be a good process to bad pool season is over and the bisulfate is kinda rare around here.

I do not have silver nitrate to clear out the left over sulfate, but I am going to try some calcium nitrate.

Jim

 

[depperl001]

Am i missing something, wheres the Sulfuric Acid? This is great news for me because Sulfuric Acid is hard to get here in Australia.

Steve, can i substitute Sodium Nitrate for Potassium Nitrate instead?

And can i pickle my silver in the Sodium Bisulfate also?

Hi stihl88,

Here in Rockhampton, QLD, you can buy it in 4L bottles of Battery acid for $ 22.00.
May pay to check sellers of lead acid batteries, car batteries.

Regards,

depperl001

 

[aurville]

Hi,
Here in NSW MO-FLO liquid drain cleaner is available from hardware stores for around $44/L. It is concentrated sulfuric acid.

cheers
aurville

 

[Anonymous]

HI,
My first experiment gives me false result. As I'm using Nitric acid, HCL, Urea and Sodium bisulphite for gold refining process with waste electronic parts. Firstly, I added Nitric acid (30ml for every once of scrap) and HCL (120ml for every once of scrap) and kept it overnight and filtered the chemical with buchner filter. After that I added urea (1 pound) in one quart of boiling water and mix it in the chemical and after that I added sodium bisulphite (one ounce for every ounce of scrap) with one quart of boiling water and mix it in the chemical. Finally, the mud was started stored it in the bottom. I refiltered with distilled water 5 to 10 times and allow it to air dry. And when I melted the mud it gives me copper instead of gold. I don't know where the mistake I've done. Please clarify my problem in brief.

 

[lazersteve]

HI,
My first experiment gives me false result. As I'm using Nitric acid, HCL, Urea and Sodium bisulphite for gold refining process with waste electronic parts. Firstly, I added Nitric acid (30ml for every once of scrap) and HCL (120ml for every once of scrap) and kept it overnight and filtered the chemical with buchner filter. After that I added urea (1 pound) in one quart of boiling water and mix it in the chemical and after that I added sodium bisulphite (one ounce for every ounce of scrap) with one quart of boiling water and mix it in the chemical. Finally, the mud was started stored it in the bottom. I refiltered with distilled water 5 to 10 times and allow it to air dry. And when I melted the mud it gives me copper instead of gold. I don't know where the mistake I've done. Please clarify my problem in brief.

You did not remove the base metals before using AR. The SMB just pushed the dissolved copper out of the solution as Copper I Chloride. Your gold (if any was there) is likely in the undissolved solids.

Did you test the AR with stannous chloride before adding Urea or SMB?

Steve

 

[golddigger2]

Hi steve
You probably mentioned this already but can you use potassium nitrate in this recipe?