Is there a way to tell if my potassium nitrate went bad

[steyr223]

I am doing 1 1\2 lbs of my ceramic ic's
Covered with hcl
Added potassium nitrate 2 tsps at a time while heating
Reaction seemed to slow or stop
After 6 or 7 tsps

Note** none of the reactions were extremely vigorous **

Stannous was yellow when i went to test :shock:
I made more(i am never confident with new stanmous
Until i see my 1rst purple stain)

Stannous gets a little brown but nothing like when gold
Is present and there is free nitric

3 people said there were still gold foils in the bottom
Of my container so of course i added more nitre

Being color blind i am hesitant on anyones color perceptions
Umless they have been in or around refining

Either no gold has gone into solution or i used way to much
Nitre(most likley the later)

I through in a nugget (did not have scale) heated for 2 more
Hours

Through this 5 or so hours i added hcl here and there.

This morning i have put it back on heat
I have removed the nugget and it looks
Like it has been eaten on the surface as there are craters
Where there was not before

With heat enough to slightly steam no bubbles i added
A 1/2 tsp of nitre absolutly no reaction
I put the nugget back in

Should i not see a reaction near my nugget
I have it at the edge so i can see it

But no bubbles

A little longer 15 min and small bubbles on surface

I can not tell if it is boil bubbles or reaction

How should i precede
Thanks steyr223 rob

Btw the color of my solution has looked like the pic
All the way though in never cleared on the nitre additions

 

[steyr223]

I threw in some white ceramics with all the black ones
In the top pic you can see my nugget in the front bottom
This is now weighed at 2g

Again thanks steyr223
Please feel free to tell me my mistakes

 

[steyr223]

Okay I just pulled my nuggit out and it is
definitely reducing. In size and weight
Is already more than a gram gone

I hope its big enough :lol:

Rhanks steyr223. Rob

 

[steyr223]

So my potassium nitrate is gpod 8)
But i put way to much in.
I have read a bunch on denoxing
The inevitable steaming down wow!
My nugget was.finally consumed so i let
The heat do its work for another 4 hours
I evaporated about 150 ml
Now harold says as soon as you see bubbles back of a notch
On the heat mark the spot and when you see bubbles(boiling)
Again to stop ,cool,add volume consumed with hcl

What no one does say is....my question
1.do i let cool and decant to ice beaker ,add sulfuric ,triple the water volume
Filter through a charmin plug
2.evaporate as described above,all the time testing for the
Purple stain
3 harolds washes
4 re-refine

Or
Do #2 first (evaporate) than to #1
If i am to evaporate first than do i continue to do so in my
Container with my material
Thanks steyr223 rob

Any help would be appreciated

 

[samuel-a]

How much HCl did you used?

 

[steyr223]

Hi sam thanks for the reply
Enough to cover the chips
Probaly 500ml at the start (100ml of h20 to
Wash the pieces off my hand)

Added 100ml 2 times when i was seeing no reaction
But yet everyone was telling me there was still visable
Gold

I have not added anything upon today just steamed for
About 5-6 hours

The container is a coffe pot/maker it says 4 cups an
Inch below the ss ring/holder handle (i dont drink
Coffe but i assume thats a quantitative measure)

Thanks steyr223 rob

Ps no base metals left this time

 

[steyr223]

Transferred solution, not material into sealed container
For transport safety .
Left material in coffe pot

This morning put solution back in coffe pot
Rinsed out transport container with approximately
100ml of hcl into coffee pot

Steamed with lid for 4 hours
Solution decreased by about 1/4" from before
Put solution back in transport container .

During all of this i tested with stannous chloride at
Every step, transferring,wash,material,steaming,
From the bottom to the top ,even the drops on the lid

Still no purple
It is 6:45 pm southern cal Time
I will start another fun filled 5 hours of
Evaporation or denoxing. By 7:30

Since nobody has attepted to correct my procedure
I have to assume that i am spot on( ya right ) :shock:


All comments are welcome
I will post my results as i go
Thanks steyr223. Rob

 

[squarecoinman]

Transferred solution, not material into sealed container
For transport safety .
Left material in coffe pot

This morning put solution back in coffe pot
Rinsed out transport container with approximately
100ml of hcl into coffee pot

Steamed with lid for 4 hours
Solution decreased by about 1/4" from before
Put solution back in transport container .

During all of this i tested with stannous chloride at
Every step, transferring,wash,material,steaming,
From the bottom to the top ,even the drops on the lid

Still no purple
It is 6:45 pm southern cal Time
I will start another fun filled 5 hours of
Evaporation or denoxing. By 7:30

Since nobody has attepted to correct my procedure
I have to assume that i am spot on( ya right ) :shock:


All comments are welcome
I will post my results as i go
Thanks steyr223. Rob

Steyn I just want to ask a few question as i am not sure if I understand everything
you used 1,5 lbs chips ( ceramic ) Black + white + 2 gram gold nugget
500 ml HCL ( how strong ) + 200 ml Hcl + 20 ml water
6 or 7 times 2 tea spoons of potassium nitrate ( or is the total 6 or 7 tea spoons )

from all this you did evaporate 150 ml so far ?

Did you dilute your solution ?

regards scm

 

[Geo]

Rob, did the nitrate happen to get wet and dry before you used it? even moisture in the air making it damp and then it drying will cause the nitrate crystals to "bleed out" of the prills. is the alot of dust, and i mean more than there should be. if it is, your nitrate might be to blame.

 

[steyr223]

Scm 12 to 14 tsps
Geo my nitre is fine
Thanks guys

I found my gold :mrgreen:
I put some sulfamic acid into the evap process
I read butchers post on not adding any dilution
Untill concentrated, but mine wouldn't

Last night around hour 18 of evaporatiom i started
To get super heated bubble explosion
I did a little reading. (De-luc)
Now i inderstood harolds explanation of the bubbles
I never. Seen big bubbles before

Todsy i decided to reference. Holked
I did a100ml test doubled with hcl
And added smb slowly untill the fizzing slowed
Always making sure no smb was on the bottom

Bingo almost a gram and i still had 1000ml to go
It droped quick
i seperated the solution 6 or so times
And dropped seperatly, i will post my results

MY first batch of 100 chips i was doing the same
Process is starting to turn black,dark but is already
Showiing powders. (I already did smb with these

My phone is going to be shut off in like 10 min
Thanks i post when i pay the bill
Thanks steyr223 rob

 

[squarecoinman]

Scm 12 to 14 tsps
Geo my nitre is fine
Thanks guys

I found my gold :mrgreen:
I put some sulfamic acid into the evap process
I read butchers post on not adding any dilution
Untill concentrated, but mine wouldn't

Last night around hour 18 of evaporatiom i started
To get super heated bubble explosion
I did a little reading. (De-luc)
Now i inderstood harolds explanation of the bubbles
I never. Seen big bubbles before

Todsy i decided to reference. Holked
I did a100ml test doubled with hcl
And added smb slowly untill the fizzing slowed
Always making sure no smb was on the bottom

Bingo almost a gram and i still had 1000ml to go
It droped quick
i seperated the solution 6 or so times
And dropped seperatly, i will post my results

MY first batch of 100 chips i was doing the same
Process is starting to turn black,dark but is already
Showiing powders. (I already did smb with these

My phone is going to be shut off in like 10 min
Thanks i post when i pay the bill
Thanks steyr223 rob

Rob I am happy it is finaly working for you

scm

 

[steyr223]

I still cant post pics frpm phone to the form
It says invalid file format
I even dowmloaded a converter/resizer and still
Error so,

http://m1274.photobucket.com/albums/steyr1/
Mobile%20Uploads/

Dont know if it works but this is a pic of last nights
Work 4.3 grams @ +99% as per xrf

Still have more setteling

Thanls steyr223 rob