Sulfamic acid for denoxing solutions

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g_axelsson

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Help!

... well maybe not, but I thought this would be a good idea anyhow.

As has been pointed out to me in a PM, there is no good tutorial or instructions on using sulfamic acid to denox solutions. At least no easily found ones. So I thought we could do one together and then we add it to the library when done.

- So, post links to any good sulfamic acid threads, tips on how to use it... Lazersteve apparently uses it in dry form. Is that better than making a solution and add it in liquid form?
- Should it be used in a hot or cold solution, is it working fast enough to notice in cold diluted nitric acid.
- Will it remove nitric salts even if there is no other acid presents?
- Is it vital or even needed to stir the solution?
- How much is needed for each ml of 70% nitric acid.
- Any drawbacks?
- Describe how you are using it and cues to when you have added enough.
- I have bought a small package on eBay, any tips on where you can get it and how much it should cost in various package sizes?

When this thread has calmed down I'll make a copy and edit it heavily for the library.

Bring it on! Let this be as productive as the furnace thread! 8)

Göran
 
Excellent!

My experience with sulfamic

-i have tried just using the crystal, and it always seemed to leave a bit undissolved at the bottom.
So what i started doing, was filling up one of my teapots or coffe pots (corningware of course!) and bringing to a boil, adding the sulfamic and continue heating until.the solution became saturated

I have tried a couple different ways as far as using it (the saturated sulfamic solution) to denoxx my AR.

I have tried adding hot sulfamic to hot ar
Hot sulfamic to cold ar
Adding hot ar to hot sulfamic
And cold ar to cold sulfamic

What i think was best, honestly i have no clue, but, to be pragmatic about it..
It may be best to do hot ar into hot sulfamic...
The sulfamic turns into sulfuric, removing the need to add sulfuric to ppt out lead sulfate.

Then, it could be chilled with ice water, to remove the AgCl from the AR, where it could then be filtered crystal.clear. (the AgCl and PbSO4 could be later separated by hot water boil, as lead sulfate -as you all know- is slightly soluble.in hot water)

I would love to know if anyone has a good rule of thumb for how much sulfamic denoxes how much nitric (i believe i saw lou post this answer in the thread where him and 4metals were helping a refiner that had a HUGE refinery-I will find it and post it shortly)

Also, i read that a member (geo i believe) used sulfamic to remove excess nitric during a silver dissolution, and that it worked to help him consume less copper during the cementation process.
-but, it was suggested to him that it wasnt necessary and could cause problems down the line, and instead, to dissolve more silver to use up the excess nitric

-eagerly awaiting more replies to this thread!
-thanks Goran

-topher
 
g_axelsson said:
- Should it be used in a hot or cold solution, is it working fast enough to notice in cold diluted nitric acid.
- Will it remove nitric salts even if there is no other acid presents?
- Is it vital or even needed to stir the solution?
- How much is needed for each ml of 70% nitric acid.
- Any drawbacks?
- Describe how you are using it and cues to when you have added enough.
- I have bought a small package on eBay, any tips on where you can get it and how much it should cost in various package sizes?



Göran

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=22177
-lou, 4metals helping a refiner and mention sulfamic a great deal

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=16134&start=20
-gsp stating -
-re: aqua regia and alluminum foil
To neutralize 1 ml of excess 70% nitric, it takes about 1.5 grams of sulfamic acid, preferably dissolved in water first. Hot 80C water will dissolve about 470g of sulfamic acid per liter. Room temp water will dissolve about 150g/l."

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=49&t=21056
-another good one from lou
 
Generally I get it at Home Depot in a 1 Lb. plastic container in the ceramic floor tile section.

I use the 1 lb plastic container it comes in. I add hot tap water to the crystals in the container and stir to dissolve the crystals. I then pour a small amount into my completed hot/warm AR solution.Depending on how much excess nitric you have in your solution will determine how violent of a reaction you will have when you add the sulfamic acid. You need to stir your solution real good so you get it mixed up real good. During the conversion of the excess nitric it converts the nitric to sulfuric acid, so if you do not have much excess nitric you possibly should still consider adding some sulfuric acid to help with the removal of the lead in your AR.
 
Barren Realms 007 said:
Generally I get it at Home Depot in a 1 Lb. plastic container in the ceramic floor tile section..

Yes, i forgot to add that to my post. Home Depot is the only place that i have found it locally.

Lowes did not have it in stock, neither did Ace Hardware... Im not sure if they do not carry it at all, or if they just didnt have it on hand.

Attached pictures show the sulfamic container and its suggested directions. I am still looking for a solubility chart for it.

I remember reading that it is an endothermic reaction, but for the life of me i cannot recsll if that was the initial dissolution of it in water, or when it is converting NOx to sulfuric.

-topher
 

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For anyone in Australia, I have seen 500g plastic containers of powder in Bunnings. I think they were about $6, but I have never bought or used any.
I probably should snap one up while I can. Pretty much all chemicals seem to be gradually becoming less and less available to the public.
 
Göran wrote:
- How much is needed for each ml of 70% nitric acid.

Wikipedia:
HNO2 + H3NSO3 → H2SO4 + N2 + H2O
HNO3 + H3NSO3 → H2SO4 + N2O + H2O

so, one mole sulfamic acid (97g) will theoretically remove 1 mole HNO3 (63g) - rule of thumb: 1g sulfamic per 1g (or 0,7ml at 25°C) HNO3 70%

Göran wrote:
- I have bought a small package on eBay, any tips on where you can get it and how much it should cost in various package sizes?

Amazon, Germany: Amidosulfonsäure, "Entkalker", 13€/1kg, 30€/5kg


Göran wrote:
- Should it be used in a hot or cold solution, is it working fast enough to notice in cold diluted nitric acid.

For me it works satisfying, when added as powder to hot AR. The dissolution of sulfamic acid is endotherm, so it cools the solution down, which is no problem with slight excess of nitric in a heated AR. I could be wrong, but I felt there was no reaction at all using it in the cold. Maybe it works just slower, but if we can't see it fizzing, we don't know, when we have removed the excess nitric. The advantage of using powder is that you do not expand the volume of liquid. The advantage of using it in dissolved form is that you will not cool down the AR by adding.

Göran wrote:
- Is it vital or even needed to stir the solution?

I can only say, that I allways stir it. Maybe some crystals sink to the bottom. I want to get them dissolved and I want to have equal temperature in all depths of the vessel.

Göran wrote:
- Any drawbacks?
At least for the case of dissolved gold in AR, I could never find any disadvantages. Under other circumstances it might be good to know, what reactions can occur. Sulfamic acid can form metal sulfamates, complexes, which sometimes are used for plating. This might be a matter, if there is large excess of sulfamic acid. I don't know, but not using excess might avoid unwanted reactions.
 
Göran wrote:
- Will it remove nitric salts even if there is no other acid presents?

Would be easy to test: Then it would precipitate sulfates with Pb(NO3)2 or Ba(NO3)2 . I doubt. If I don't forget it, I'll try this next time in the lab.
 
Spaceships suggested that I would copy his tutorial from the other forum...

Spaceships said:
Here's a process I have learned and modified to get the best results for denoxing AR solutions.

The process is very cheap to operate and once learned and applied correctly it will remove the hassle of denoxing, and dramatically speed up the process of refining gold.

Caveats:

1. I am assuming that all normal safety procedures are both known and followed.
2. I am assuming that the reader has a basic but working knowledge of refining gold using AR.
3. I am assuming that the reader has all the relevant equipment to carry this out.

Basic theory:

Excess Nitric acid in a AR solution that is pregnant with AuCl will prevent the gold being precipitated using your preferred method of choice (SMB, ferrous II Sulphate etc.) The plan is to remove this excess Nitric leaving a solution that is ready to cool, filter, and process in the normal way in order to add your precipitant of choice.

Effectively the use of Sulphamic acid (I am British so I spell it the British way- Americans then to know it as Sulfamic Acid) does this by converting the Nitric acid to Sulphuric Acid, Nitrous Oxide, and water.

The chemical reaction is: HNO3 + H3NSO3 → H2SO4 + N2O + H2O

That's great to know, however let's concentrate on the practical application of the process because it also has some other benefits to the process other than the removal of Nitric, but I will cover those later.

Preparation of Sulphamic Acid solution.

Prepare your Sulphamic acid as follows:

You will need a 1 litre glass beaker, a hot plate, a plastic spoon, an inert stirring rod, water, and a tub of Sulphamic acid crystals.

Add 150ml of water to the beaker, and place on the hot plate. You want this solution to be warm to hot, not boiling.
Add a couple of teaspoons of the crystals to the water, stir and let it dissolve- this will happen relatively quickly to start with.
Keep repeating this process until your solution leaves some crystals in the bottom even after plenty of stirring. Your solution is now close to being saturated. It doesn't HAVE to be this strong but experience will help you learn the required amounts.

In order to learn this properly without any risk of losing gold, I would suggest that you prepare a dummy solution of AR. Remember the purpose of the tutorial is to help you learn to denox a solution so why risk your money if it can be learned without financial risk?

Preparation of "dummy" AR.

Put 100ml of HCl in a 1 litre beaker.
Add 100ml to 150ml of water - tap water is absolutely fine for this.
Add 3ml of Nitric acid (70%) or 6ml of Nitric acid (35%) or the equivalent of "poor man's Nitric."
Put this on a hotplate (WITH A CATCH PAN) and warm up. Again you want a warm to hot solution - as if you were truly dissolving gold but no need to boil.

Once you have the two warm solutions ready then move onto the next stage.

Application of the Sulphamic Acid on the AR.

Gently add a few (and I mean literally a few) ml of the solution you made from the Sulphamic Acid and water to the AR. You will immediately see a vigorous foaming of the AR. Put your Sulphamic solution down and then stir your AR. The initial reaction WILL THEN BECOME A LOT MORE VIGOROUS.

Now, this is why I suggested that you learn using a "dummy" solution. You will possibly add too much on your first attempt and then proceed to watch with little tears of joy, as your AR solution bubbles up and foams over the sides of the beaker.

I can promise you from experience that those little tears of joy are infinitely more preferable than the tears you will cry if your solution had been pregnant. I cried those tears once - and my AR was orange at the time....

When the reaction has abated, repeat it. Then repeat it again, until you get very little reaction after addition of the Sulphamic Acid solution and stirring. At this point leave it alone for 15 minutes and go and do something else. You may have to mix another set of Sulphamic Acid solution and this is a good time to do it.

After 15 minutes, come back, add more Sulphamic Acid solution to the AR, stir and see what happens. You may almost be at the point where the Nitric has been converted by now. You need to repeat the last step until there is no reaction with the AR. At that point you are denoxed and I would leave the solution on the hotplate for 30 minutes, then cool, add ice, and do all the things you normally do.

Learn the process using "dummy" AR or even Nitric and water until you are totally comfortable before applying it to your gold pregnant AR. You will make mistakes, that's fine. You will learn from them in a "risk free" manner."

Learn the process, make a few mistakes, then get comfortable with the application of it and it will serve you well.

Now here are a couple of practical pointers for using "live" AR.

1. Don't filter your AR before denoxing. Decant it from your spent , raw product, wash your spent product down and pour the liquid into your denox glassware with the AR, and denox it "warts and all." You will filter it afterwards.
2. One by product of the process above is that the sulphuric acid produced will precipitate out any lead as lead salts so it can save you adding Sulphuric acid later to do this.

I hope this helps. If I have missed anything, or you'd like further information then please let me know.

Regards

Jon

This looks like a well thought through tutorial, thanks Jon! I really like the tip of testing on a dummy AR solution as it seems boil over is a large risk when using sulfamic on hot solutions.

Any comments on this?

Göran
 
Hopefully, there won't be much of a reaction, if excess Nitric wasn't used in the first place. Excess Reagents cost you twice.

It's just good business sense.
 
Sooo what you are saying, Irons, is...

The excessive man pays twice!

:mrgreen:

Göran
 
Sulfamic acid is often prepared wrong. Test it by adding a little to some nitric acid. If it is correctly made, the gas N20 (laughing gas) will immediately form.
 
Irons said:
It reminded me of the question:

Why do we never have the time to do it right in the first place, when we always have time to do it over?

Patience is a Virtue.
You sire, is a very wise man!

I would love to share a couple of cold beers and trading stories with you. 8)

Göran
 
g_axelsson said:
Spaceships suggested that I would copy his tutorial from the other forum...

Spaceships said:
Here's a process I have learned and modified to get the best results for denoxing AR solutions.

The process is very cheap to operate and once learned and applied correctly it will remove the hassle of denoxing, and dramatically speed up the process of refining gold.

Caveats:

1. I am assuming that all normal safety procedures are both known and followed.
2. I am assuming that the reader has a basic but working knowledge of refining gold using AR.
3. I am assuming that the reader has all the relevant equipment to carry this out.

Basic theory:

Excess Nitric acid in a AR solution that is pregnant with AuCl will prevent the gold being precipitated using your preferred method of choice (SMB, ferrous II Sulphate etc.) The plan is to remove this excess Nitric leaving a solution that is ready to cool, filter, and process in the normal way in order to add your precipitant of choice.

Effectively the use of Sulphamic acid (I am British so I spell it the British way- Americans then to know it as Sulfamic Acid) does this by converting the Nitric acid to Sulphuric Acid, Nitrous Oxide, and water.

The chemical reaction is: HNO3 + H3NSO3 → H2SO4 + N2O + H2O

That's great to know, however let's concentrate on the practical application of the process because it also has some other benefits to the process other than the removal of Nitric, but I will cover those later.

Preparation of Sulphamic Acid solution.

Prepare your Sulphamic acid as follows:

You will need a 1 litre glass beaker, a hot plate, a plastic spoon, an inert stirring rod, water, and a tub of Sulphamic acid crystals.

Add 150ml of water to the beaker, and place on the hot plate. You want this solution to be warm to hot, not boiling.
Add a couple of teaspoons of the crystals to the water, stir and let it dissolve- this will happen relatively quickly to start with.
Keep repeating this process until your solution leaves some crystals in the bottom even after plenty of stirring. Your solution is now close to being saturated. It doesn't HAVE to be this strong but experience will help you learn the required amounts.

In order to learn this properly without any risk of losing gold, I would suggest that you prepare a dummy solution of AR. Remember the purpose of the tutorial is to help you learn to denox a solution so why risk your money if it can be learned without financial risk?

Preparation of "dummy" AR.

Put 100ml of HCl in a 1 litre beaker.
Add 100ml to 150ml of water - tap water is absolutely fine for this.
Add 3ml of Nitric acid (70%) or 6ml of Nitric acid (35%) or the equivalent of "poor man's Nitric."
Put this on a hotplate (WITH A CATCH PAN) and warm up. Again you want a warm to hot solution - as if you were truly dissolving gold but no need to boil.

Once you have the two warm solutions ready then move onto the next stage.

Application of the Sulphamic Acid on the AR.

Gently add a few (and I mean literally a few) ml of the solution you made from the Sulphamic Acid and water to the AR. You will immediately see a vigorous foaming of the AR. Put your Sulphamic solution down and then stir your AR. The initial reaction WILL THEN BECOME A LOT MORE VIGOROUS.

Now, this is why I suggested that you learn using a "dummy" solution. You will possibly add too much on your first attempt and then proceed to watch with little tears of joy, as your AR solution bubbles up and foams over the sides of the beaker.

I can promise you from experience that those little tears of joy are infinitely more preferable than the tears you will cry if your solution had been pregnant. I cried those tears once - and my AR was orange at the time....

When the reaction has abated, repeat it. Then repeat it again, until you get very little reaction after addition of the Sulphamic Acid solution and stirring. At this point leave it alone for 15 minutes and go and do something else. You may have to mix another set of Sulphamic Acid solution and this is a good time to do it.

After 15 minutes, come back, add more Sulphamic Acid solution to the AR, stir and see what happens. You may almost be at the point where the Nitric has been converted by now. You need to repeat the last step until there is no reaction with the AR. At that point you are denoxed and I would leave the solution on the hotplate for 30 minutes, then cool, add ice, and do all the things you normally do.

Learn the process using "dummy" AR or even Nitric and water until you are totally comfortable before applying it to your gold pregnant AR. You will make mistakes, that's fine. You will learn from them in a "risk free" manner."

Learn the process, make a few mistakes, then get comfortable with the application of it and it will serve you well.

Now here are a couple of practical pointers for using "live" AR.

1. Don't filter your AR before denoxing. Decant it from your spent , raw product, wash your spent product down and pour the liquid into your denox glassware with the AR, and denox it "warts and all." You will filter it afterwards.
2. One by product of the process above is that the sulphuric acid produced will precipitate out any lead as lead salts so it can save you adding Sulphuric acid later to do this.

I hope this helps. If I have missed anything, or you'd like further information then please let me know.

Regards

Jon

This looks like a well thought through tutorial, thanks Jon! I really like the tip of testing on a dummy AR solution as it seems boil over is a large risk when using sulfamic on hot solutions.

Any comments on this?

Göran
Goran, please don't refer to refinement of precious metals as the other forum. Thank you!!
Ken
 
jeneje said:
g_axelsson said:
Spaceships suggested that I would copy his tutorial from the other forum...

Spaceships said:
Here's a process I have learned and modified to get the best results for denoxing AR solutions.

...

Jon

This looks like a well thought through tutorial, thanks Jon! I really like the tip of testing on a dummy AR solution as it seems boil over is a large risk when using sulfamic on hot solutions.

Any comments on this?

Göran
Goran, please don't refer to refinement of precious metals as the other forum. Thank you!!
Ken

Ok, it was copied from http://www.refinementofpreciousmetals.com/ on suggestion of Jon.

Göran
 
g_axelsson said:
Irons said:
It reminded me of the question:

Why do we never have the time to do it right in the first place, when we always have time to do it over?

Patience is a Virtue.
You sire, is a very wise man!

I would love to share a couple of cold beers and trading stories with you. 8)

Göran

Irons is drippings wet from wisdom it seems!

And, Its because we end up making time, to do it over.
Which, when time is money.. Ends up costing thrice over i guess.

And, i hear that Goran!

Any chance you are ever on the southeast corner of KS, let me know!
 
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