That With No Name...

[GotTheBug]

I'm not sure if I made a mistake in the process we don't talk about

100 mL plus 170g, almost to boil, and dissolved.

added 56mL of 96% and did not allow to boil

Let cool and in ice bath, then later covered and put into freezer overnight.

Next day, crystals in the bottom, poured an amber colored liquid off.

The original 96% is brownish, which would explain the color.

It seems I followed directions, and yet it has little effect on what it should affect very well, and no I'm not going to sniff it.

Any obvious errors?

 

[etack]

Are you making nitric?

If you don't say what your doing we can only guess.

Eric

 

[necromancer]

nitric would be my guess

 

[GotTheBug]

Making nitric is one of the things we tend not to discuss for the safety of noobs.

Is that enough answer?

 

[Geo]

Actually, it's been discussed to death and resurrected and then discussed to death again. Almost all new members (at some point) has tried the poor man's nitric acid recipe. Check out NurdRage on youtube for a good visual on making nitric acid.

 

[GotTheBug]

Failed nitrate test, ugh. That's what I get for switching ingredients I suppose.

 

[butcher]

From the recipe you posted I am assuming you used sodium nitrate, if you used as much water and reactants as you stated the nitric acid would be somewhere around 56%, but if you varied from the recipe, or boiled some of the water away, it could be stronger.

If you dissolved the nitrate salts before adding the sulfuric acid, you did get the nitrates in solution to more easily react with the sulfuric acid.

If the NaNO3 was not dissolved, you may not react all of the nitrates. This does not sound like the case here.

It does not matter if the nitric acid is weaker as it will still dissolve copper, or other base metals, ( cold will just take some time if very diluted) even pretty weak nitric acid with heating will dissolve copper and base metals, as water is lost in evaporation from the heating, ideally we try for around 30% to 40% HNO3, to dissolve base metals.

My guess is most likely your nitric is fairly strong, which can temporarily passivate metals like copper, or even silver, you may need to add some water and heat, and then see if it does not work better to dissolve copper and base metals.

 

[GotTheBug]

Found that the fertilizer I was using is 17% nitrate by volume. Tried again today with an excess, and ended up with a beaker full of cake after cooling.
350 grams of fertilizer
100 mL water
60 mL 96% sulfuric.

I am missing something here.

Ideas?

 

[butcher]

If you are using a fertilizer it has to be relatively pure potassium or sodium nitrate fertilizer, not blended fertilizer or a fertilizer that contains these nitrates mixed with other salts, which would not work to make nitric acid.

I think what you are missing here is doing enough study on the subject, before attempting to do the lab work.

 

[Geo]

A good source of quick potassium nitrate is Spectracide brand stump remover. Be sure to check the label before buying. http://www.spectracide.com/~/media/Spectracide/Files/MSDS/Other/Spectraicde_Stump_Remover_MSDSNov12.ashx

http://www.lowes.com/pd_188198-316-HG-66420_0__?Ntt=stump+remover&UserSearch=stump+remover&productId=4764059&rpp=32

The MSDS list the ingredients as 100.0% potassium nitrate.

 

[Shark]

These are posted else where on the forum by a member the best I recall by the name Golden Child. It shows Lazersteves method for Cold Nitric. I have used it a few times and it worked well with Hi-Yield brand Soda of Nitrate. Hi-Yield is a bit cleaner than the large bags of fertilizer used by bigger farmers and can be bought in 4 or 5 pounds bags.

https://www.youtube.com/watch?v=T-UkqAs2MWE

https://www.youtube.com/watch?v=d_isqNvcNlU

 

[GotTheBug]

Was doing some studying also in converting ammonium to sodium nitrate. I think I might just spring for a bag of potassium nitrate instead. Both are available locally, though the stump remover, per se, is not.

Thank You guys for pointing me in the right direction!