Nitric

[godofwar]

All temps in degrees F

not really asking for help figured this would be the best way to just double check myself.....

performed prior mixtures to make nitric and i figure i must have done it wrong in my previous attempts or missed a step.....

anyway

took sulphuric acid did a slow evap down to just below 40% of start value.... used sulfuric acid that was 36-38% sulfiric 98% 62-64% H2O

took distilled water brought to just below a boil mixed 200gm of ammonia nitrate( all i could get ahold of) throughout the temp rise due to the reaction of ammonia nitrate with H2O you know ex: instant cold pack....

did not allow to peak and boil but very slight evap....

ok now after allowing to cool to about 130 degrees placed outside 25 degrees and allowed to cool currently external temp is very low internal still at a room temp 70 degrees... and falling...

ok i know salts are suppose to form but i am getting a very heavy amount of salts. i broke up to free up any locked in liquid. and currently allowing to cool...

i followed every step it all looks right to me... if i am wrong let me know.... if i am right on the mark let me know...

but to curious what do you think the chemical composition of the salts may be....ammonium sulphate?????

ok i know this may stupid but after prior mistakes i am taking my self from square one and perfecting each process i perform before i take on the next step.....

 

[Barren Realms 007]

The only amount you give is the ammonia nitrate, the sulfuric and water you give no volume. Even with the solution being in 25 deg weather I would still put it on ice for the night and filter it in the morning.

 

[godofwar]

oh sorry i was going to formula .... as listed in handbook vol 1

100ml distilled water 56 ml sulphuric

i am going to let it sit all night no matter what i will just set it in the snow lol

 

[Palladium]

That formula is for sodium or potassium nitrate, not ammonia nitrate.

 

[godofwar]

That formula is for sodium or potassium nitrate, not ammonia nitrate.

well i don't know what would sound worse say hey should scratch this... and continue to go along with what i already said and save some face..

or the truth.... i just remembered that i actually changed my source for nitrate salt.. oh hell way before my last issue i had with this process in mind...
i don't know what's worse the fact i forgot what source material i switched into....
or the fact i used a formula while i thought i had a different material.. deadly mistake in other instance... it is actually potassium nitrate- Specticide Stump remover {NOT BONIDE}
oh well i really look like a retard.... and it really looks BAD... i am honest so whatever hazing comes from this comes from this...

HOLY HELL.... this really i mean really sounds bad the more i read it over OH WELL

 

[Palladium]

Sounds like you have already learned another lesson. lol
We all make mistakes. Just don't make to many, some times they are a lot less forgiving. Keep trying. I mean it only seems like yesterday Harold was burning a garage down. Just kidding Harold. I've made a few in my life, we all have.

 

[Barren Realms 007]

That formula is for sodium or potassium nitrate, not ammonia nitrate.

well i don't know what would sound worse say hey should scratch this... and continue to go along with what i already said and save some face..

or the truth.... i just remembered that i actually changed my source for nitrate salt.. oh hell way before my last issue i had with this process in mind...
i don't know what's worse the fact i forgot what source material i switched into....
or the fact i used a formula while i thought i had a different material.. deadly mistake in other instance... it is actually potassium nitrate- Specticide Stump remover {NOT BONIDE}
oh well i really look like a retard.... and it really looks BAD... i am honest so whatever hazing comes from this comes from this...

HOLY HELL.... this really i mean really sounds bad the more i read it over OH WELL

Don't beat yourself up. You should still be able to use what you made. Do a test run with it and you will get an idea on what it will do.

 

[godofwar]

we anyway i will be doing a test run tonight or tomorrow ...... i will be using it on base metals anyway......

but heres a thought ......

could you add nitrate to heated sulphuric acid not concentrated....38% sulphuric 62% H2O
then cool and get the same effect..... really just a thought

i like to ask why

 

[Barren Realms 007]

we anyway i will be doing a test run tonight or tomorrow ...... i will be using it on base metals anyway......

but heres a thought ......

could you add nitrate to heated sulphuric acid not concentrated....38% sulphuric 62% H2O
then cool and get the same effect..... really just a thought

i like to ask why

Yes, Steve has posted a formula/process for this. But I haven't used it.

 

[adam_mizer]

I used Steve's poormans formula yesterday.
Maybe I did it a little wrong but it worked out just fine.

CPU's and chips and some ceramic plated stuff was put in coffee pot.
Steve said cover with HCL and add same amount of water.
If you think about this when I covered with HCL I was at 4.5 cups line on the pot, but really maybe 3 cups HCL if that. Thats where I think I went a little wrong. It turned out fine, I added 4.5 cups tap water. Then instead of 2 teaspoons sodium nitrate I added 4 teaspoons because of the load in the pot I thought was large enough. My sodium nitrate was small balls type.

Something else bothered me, take into consideration the type of lid on the coffee pot because stopping the vapors in the beginning is important.
After seeing some vapor drip off the ceramic dish I tested the drip and behold I was loosing PM's in the initial vapors.
This tells me that until enough base metals are entering solution the gold plating has entered solution and can be boiled off and lost in vapor at the beginning.
Boiling dark solution loaded with base metals must not allow loss of PM's because I boiled many cups of solution off and in the end of this batch I recovered some grammage.
Still it bothered me that a stannous test showed purple on the condensated vapor from the dish.

I did not get salts after boiling 25% of solution away, makes me think I used too much water.
Oh well the powder dropped anyway.

Now, wondering what to do with the waste, as somewhere in it there should be a tiny amount of silver or palladium shouldn't there?

Also having trouble removing the heavy thick CPU lid, but the underside lids are very easy to remove, what to do for those haevy lids?
It appears that copper attached to the lid anyway. Is this good bad or what?

 

[Barren Realms 007]

I used Steve's poormans formula yesterday.
Maybe I did it a little wrong but it worked out just fine.

CPU's and chips and some ceramic plated stuff was put in coffee pot.
Steve said cover with HCL and add same amount of water.
If you think about this when I covered with HCL I was at 4.5 cups line on the pot, but really maybe 3 cups HCL if that. Thats where I think I went a little wrong. It turned out fine, I added 4.5 cups tap water. Then instead of 2 teaspoons sodium nitrate I added 4 teaspoons because of the load in the pot I thought was large enough. My sodium nitrate was small balls type.

Something else bothered me, take into consideration the type of lid on the coffee pot because stopping the vapors in the beginning is important.
After seeing some vapor drip off the ceramic dish I tested the drip and behold I was loosing PM's in the initial vapors.
This tells me that until enough base metals are entering solution the gold plating has entered solution and can be boiled off and lost in vapor at the beginning.
Boiling dark solution loaded with base metals must not allow loss of PM's because I boiled many cups of solution off and in the end of this batch I recovered some grammage.
Still it bothered me that a stannous test showed purple on the condensated vapor from the dish.

I did not get salts after boiling 25% of solution away, makes me think I used too much water.
Oh well the powder dropped anyway.

Now, wondering what to do with the waste, as somewhere in it there should be a tiny amount of silver or palladium shouldn't there?

Also having trouble removing the heavy thick CPU lid, but the underside lids are very easy to remove, what to do for those haevy lids?
It appears that copper attached to the lid anyway. Is this good bad or what?

This is a completely different puppy. He was talking about poor mans nitric, not poor mans AR. 8)

 

[lazersteve]

Also having trouble removing the heavy thick CPU lid, but the underside lids are very easy to remove, what to do for those heavy lids?
It appears that copper attached to the lid anyway. Is this good bad or what?

I process the entire cpu with the copper tungsten heat spreader still intact.

You can remove them with a lot of heat and an acetylene rig, I've done it, but the resulting lid is gray and alloys with the bulk of the gold, making recovery more difficult.

Steve

 

[lazersteve]

The formulas I posted for poorman's Nitric are designed around the solubility curve of sodium sulfate, any other nitrate besides sodium nitrate will not give the same results.

Potassium is the only nitrate I would consider substituting, but not nearly as insoluble as sodium sulfate.

If you are using the distillation method you can use any nitrate as long as the proper proportions are maintained for the differing formula weights.

Steve

 

[adam_mizer]

Ooops sorry for the reply in your nitric thread.

Thanks Steve about confiming the large heavy heatsink as its much easier to put it into this solution then to take it off.

Still wondering about the possible tiny bits of silver and or palladium that maybe in this waste, eventually need to study up on a method to approach this.

 

[lazersteve]

The heat spreader is mainly tungsten which will not dissolve to any extent in AR.

Silver will not dissolve in AR, and is recovered easily from nitric with copper, HCl, or NaCl.

Pd is recovered in the silver cell or fro the nitric solution if you use HCl to recover the silver.

Don't get too obsessed with the Ag and Pd, you won't find much, if any in most cpus.

Steve

 

[godofwar]

we anyway i will be doing a test run tonight or tomorrow ...... i will be using it on base metals anyway......

but heres a thought ......

could you add nitrate to heated sulphuric acid not concentrated....38% sulphuric 62% H2O
then cool and get the same effect..... really just a thought

i like to ask why

Yes, Steve has posted a formula/process for this. But I haven't used it.

i searched for it yet could not locate it i was just wonder what difference was......... strength wise
really doesn't apply for a while i made enough concentrated sulphuric acid... to keep me busy for a while.....

well i tested my mixture and only place the nitric in to remove base metals from gold bearing .... from the looks of it there has to be some Cl left in it from not remaining under freezing long enough or something.....
i will test for pm's tonight
we will see what i come up with

oh well nothing that can't be reclaimed bearing is all left overs from a AP i figured i would use nitric to help with any other base metals that MAY be present.....
all interesting experience

 

[godofwar]

ok heres a question .... i have a HUGE amount of compressed nitrogen

is there a way to use this to my benefit in making nitric acid

 

[Barren Realms 007]

ok heres a question .... i have a HUGE amount of compressed nitrogen

is there a way to use this to my benefit in making nitric acid

I'm going to go out on a limb here and say that is a different breed of animal and say nope.

 

[lasereyes]

ok heres a question .... i have a HUGE amount of compressed nitrogen

is there a way to use this to my benefit in making nitric acid

I'm going to go out on a limb here and say that is a different breed of animal and say nope.

You can but it is hopelessly inefficient. its called the birkeland-eyde process, and you could combine O2 and N2 in stoichiometric ratios to use instead of air (making it more efficient) and run a very powerful current through the gas, making NO. the resulting gas further oxidizes into no2 then you bubble it through water which dissolves it to produce hno3, but you will probably have to distill it to get up to %70 because of the solubility curve of no2.

 

[godofwar]

would be a cool experiment but damn costly
i have both pure oxygen and nitrogen i am not a chemist .....i will have to research it maybe someday i will give it a try ... just not anytime soon