AR test.

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mikes1066

Active member
Joined
Dec 13, 2014
Messages
25
Location
Ohio
IMG_20170208_173344.jpg
Oxalic acid and KCl in boiling AR. Oh tests between a 2 and 3 using the cheap Chinese test paper. Will have to rinse , melt and rerun AR at room temp to see what happens. Yes I cooked it down and went through the degas procedure. For the rerun I will use some test tubes for a HCl , Nitric , and AR for comparison.
 
Wow, no comments. I guess I finally got something on the right track. I figured the ore I am working with was going to be a pain to figure out.
 
Well, I have no idea what you are doing or what the picture is showing so I have no comments.

Oh test?

Göran
 
mikes1066 said:
Oxalic acid and KCl in boiling AR. Oh tests between a 2 and 3 using the cheap Chinese test paper. Will have to rinse , melt and rerun AR at room temp to see what happens. Yes I cooked it down and went through the degas procedure. For the rerun I will use some test tubes for a HCl , Nitric , and AR for comparison.
The post is hard to make any sense of. To a dullard like me, It reads like this :-

"I am testing my HCl/HNO3 AR mixture using oxalic acid and potassium chloride.
I have some chinese test paper made specifically for testing AR.
I will rinse and melt my HCl/HNO3 AR mixture before doing it again on a smaller scale."

That can't be right, so it would be great if you would please describe what you're testing in more detail.
 
Did you ever do a stannous test to see if you have any values in the liquid?

One thought I have is that treating ore with aqua regia could leach Ca from the rock, especially if it is a carbonaceous rock. This will precipitate calcium oxalate when mixed with oxalic acid, especially when cooled down.
https://en.wikipedia.org/wiki/Calcium_oxalate

Why did you add KCl to the solution? It might form potassium hydrogenoxalate with the oxalic acid.
https://en.wikipedia.org/wiki/Potassium_hydrogenoxalate
On wikipedia it says " Below 50 °C the much less soluble potassium tetraoxalate forms and precipitates out of solution." (solubility 25g/l)

Göran
 
mikes1066 said:
Sorry for the typo.

Working with an ore. Aqua Regia hot digestion near 85 degrees C. Almost zero reaction until getting close to 85 degrees C. 6 hour cook for digestion. Filter, degas procedure. Add 15 grams oxlic acid and boil. Add ph adjustment using NaOh. no reaction. Added 15 grams KCl got a small amount of yellow powder to drop cold. Not enough to worry about filtering. Decided to heat to boiling again. Before boiling began this is the precipitate that happened on its own. will do the filtering and rinsing. Will dry and then heat red hot. will rerun in three test tube size lots , one HCL , one distilled nitric cut with distilled water , one AR at room temp . Will let all three set without heating for 2 days . Will see what happens. I hope for no reaction. Will then make a larger batch of AR and heat hoping for a reaction.
Sorry, i must be very stupid indeed, as i still have no idea what you're saying/asking.

'Ore' can mean many things, and i can't imagine any common rock-ore not reacting with warm nitric.

'Degas' must mean de-gas by some unspecified method. Presumably nothing to do with a french artist.

Boil acid ... add NaOH ... no reaction ?!?! Explode from the pot might be one.

Sorry again : i find this whole thing unbeliveable based on the very scant detail given.
 
Please don't take it personally, just give the people here enough information to be able to help you.

i.e. :-

What kind of Ore ?
Where from ?
How has it been mined/heated/crushed ?
What exactly is the problem that you need help with ?

With the full details of all these things, i feel sure somebody will know exactly what needs to be done.
 

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