Whats in this solution?

[adam_mizer]

Here's a couple pic's of a solution I was working on.
The reason I'm working on it is that the stannous test has a nice black color which I believe to be a PM.
The solution has been boiled down and is slightly syrupy.
In the filter I poured out the test tube that I did a DMG test on.
On the edges is a pink color and the main color of salts appears blue.

I have much inexperience but am giving this a good try to figure out what it is.
Hate to ask for help but here it is.
Might as well bang my head against a wall.

Edit add: I removed the gold and silver a while back, then evaporated the solution from 2 pots into 1 pot.
It was made from poormans AR origonally, remove silver solids and salts then SMB remove gold.

 

[butcher]

I would take a sample and dilute it and retest that with stannous chloride test.

 

[Dr. Poe]

Pink edges of blue from DMG (dimethyglyoxime) sounds like nickel to me. From the picture, looks like you have a precious metal or metal sulfide suspended in a nickel salt. Test a drop with a blowpipe flame and borax. Dr. Poe 8)

 

[adam_mizer]

Thank you, will dilute and retest.
The blowpipe borax test, is there to be a color reaction?

Also forgot to mention this is my remainder waste liquids, and only because that stannous test, makes me believe something is suspended.
The q-tip swab had only a very tiny band of black very thin, and the remainder of the swab was yellow-green this morning.

 

[Dr. Poe]

HOW TO USE A BLOW PIPE

Take a long metal tube with about a 3/16" diameter or less and insert one end into your mouth and the other end into the blue part of a gas flame. Blow the flame gently to aim the flame to bend at an acute angle where it points down into a target area. practice to keep a steady slow pressure with your mouth. The part of the flame farthest from the blue is called the oxidizing flame. The tip of the blue part is called the reducing flame. Bend a platinum, palladium or nickel wire to make a small loop. Heat the loop and plunge the hot loop into borax. Heat the borax/loop until it forms a bead and touch your dry sample to be tested. Heat it again with the oxidizing flame and take note the color while hot and again while cold. Heat again, this time with the reducing flame and take note the color while hot and again while cold.
RESULTS FOR OXIDIZING FLAME/BORAX
COLORLESS: HOT or COLD--- Si, Al, Mg, Sr, Ca, Ba, Zn, Cd, Pb, Bi, Sb , Mo, Sn (Saturated tin is opaque)
YELLOW OR BROWN BEADS: HOT not saturated: Fe, U SUPERSATURATED: Pb, Bi, Sb
RED BEADS: HOT: Fe, Ce COLD: Ni
AMETHYST BEADS: HOT OR COLD: Mn HOT: Ni with Co
BLUE BEADS: HOT OR COLD: Co COLD: Cu
GREEN BEADS: HOT: Cu, Fe with Co COLD: Cr

RESULTS FOR REDUCING FLAME/BORAX

COLORLESS: Si, Al, Sn (supersaturated is opaque), alkali and alkaline earths
HOT or COLD: Mn, Ce HOT: Cu
YELLOW/BROWN: HOT: Ti, Mo
RED: COLD: Cu (supersaturated is opaque),
AMETHYST: COLD: Ti
BLUE: HOT OR COLD: Co
GREEN: Cr, Fe (supersaturated)
OPAQUE (supersaturated): Pt, Ag (white bead), Pb, Sb, Cd, Bi, Zn, Ni, Si, Al, Sn

You might also try the charcoal/soda ash fuse test:

A SUBSTANCE FUSED WITH SODIUM CARBONATE ON CHARCOAL:
Place a small amount of the sample in a hollowed spot on the charcoal block with a little sodium carbonate and fuse using the reducing flame.
RESULT OF TEST INFERENCE
Metallic flakes or globules without incrustation
Yellow gold
red copper
White, moderately soft silver
Metallic flakes or globules with incrustation
White moderately soft lead (volatile lead leaves a yellow coat)
White moderately soft tin
White, brittle beads Bi or Sb
8) Dr. Poe

 

[slickdogg]

Dr. Poe that seems like alot of trouble is it acurate? One could easly mistake one color for another like blue or green when it comes to a flame?

 

[adam_mizer]

Very nice method of testing with borax Dr. Poe.
Thank you for detailing it.
Sort reminds me of a long time ago using charcoal block and blowpipe flame against mineral and checking color streak.

This evening the swab was just yellow-green.
Dropped some ammonia on the blue salts and they turned red color.
I think I remember Butcher saying something about ammonia in another post I read.
I'm pretty convinced the DMG dropped something like a hydrated Nickel II compoound.
The diluted stannous didn't show anything.
For that much salt to drop from a small test tube I must have a lot of nickel.

Before I did all this with the pot I had some large copper wire inside it for a few days thinking I could cement anything good out.
Also before I wrote this I must have poured the solution too quickly but it really appeared as nothing was on the bottom cemented out.
Well since I'm very convinced about the nickel I slowly poured the solution into a waste jug to process out the nickel and copper later.
Took my time pouring and got something on the bottom.
Looked like salt, cleaned it up twice in HCl and this salt remained.

Again I'm at the mercy of trying to find a similar experience or idea from members.
Any ideas on the white salt?

 

[butcher]

Will it dissove in water? --Table salt will.
Will it dissolve in boiling hot water? --Lead chloride will. (when cooled the lead chloride will form white crystals again)
Will it dissolve in ammonia? --Silver chloride will.
Remember to add HCl to silver dissolved in ammonia to get back the silver chloride and make solution safe, (if clean save the ammonium chloride solution and evaporate to crystals).

 

[Harold_V]

Do keep in mind, if a test with DMG is conducted in an acidic state, nickel will not yield a pink reaction. It does that only when the solution is basic. If yours is not, look elsewhere for the reason you're seeing a hint of pink.

Harold

 

[adam_mizer]

I think the solution is near basic after been boiled down so much.
Will test it a little further and add touch of acid.

The salt in the bottom of the beaker is sitting undernieth water right now.
Its very clear.
Will boil this later to see if anything else happens.

This is all helping me very much to deal with cleaning wastes and become sure of not tossing anything precious away.
Its so odd that the colors and variations I am having seem maybe a little uncommon and due to many various methods we all use maybe have different results from the wash outs and combinations of wastes.

Since I have even more waste from this run the jug will have its own label until I'm absolutely sure about the pink.
More tests on the white tonight.

 

[adam_mizer]

Butcher you nailed it with the boiling water.

As for the pink salt reaction, will try a piece of litmus paper and check the PH level.
Havn't given up on it yet, its a great learning experience a little at a time.
Even if the stuff is useless its all worth it!

 

[Harold_V]

As for the pink salt reaction, will try a piece of litmus paper and check the PH level.

Don't work this thing to death. A drop of the solution in a spot plate along with a drop of ammonium hydroxide will be all you have to do to conduct the test with DMG. Please note that you said you'd add a drop of acid -----that's the wrong thing to do.

When you have nickel in an acid solution, it will generally be blue or blue/green. You get about the same reaction from copper in acidic solution. When you add a drop of ammonium hydroxide, the solution, assuming it contains either copper or nickel, will turn a brilliant blue. When you add a drop of DMG, if there's nickel present, the blue is replaced by pink. If you don't get the pink reaction, you can forget the idea you may have nickel.

One thing I'd like to mention. The color of your solution appears to me to be black. Don't confuse that with the color of the reaction you get with stannous chloride. Did you do that? Hard to say when I read your comments again.

Harold

 

[adam_mizer]

Very much I do believe I have worked this thing very much and it is very clear to me that there is no PM left in the waste.

Just wanted to be absolutely sure and with your help much of this came to clarity.
There was a PH reading of 4-5 on litmus.
The solution I tested again in DMG 50% water added, no pink this time.
I dried it much slower so the filter paper would not blacken, the first sample was dried too quick and too hot.
When the nice blue green salt was dried I put a drop of ammonia on it and it showed the red type color.
It also was interesting a tiny bit of lead was present.

I am now very convinced that this sample waste has been cleared out of any PM's.
It feels very good to know this, because the waste was always on my mind if it contained any PM.

Now I'll make sure that the other stored waste is all cleaned out of residual PM.

My next batch is started processing but before I started cooking it sat a day in HCl and got cooked on low heat after that for 6 hours then sat overnight.
Hopefully this little preliminary process will help remove some tin and lead.
I see to remove the lead salts, water should be added and heated to near boil and poured off while hot or the salt will precipitate again as butcher suggested earlier.
This time an incineration to red hot was perfomed.
Hopefully with these few preliminary steps my finish will be better, and/or the complete process might take less time.

Thank you gentlemen for your support and guidance.

 

[Dr. Poe]

Did you use a microscope to try and identify the crystal shapes of the white "salt"?
:?: Dr. Poe

 

[adam_mizer]

No I didn't use the microscope and funny you should mention that because the the microscope is sitting right there.
Have to admit I really wasn't interested at looking that close at the salts, although I looked at the nickel salts under the scope.
Never did identify the crystal structures with the textbook style.
Pretty much the waste spoke for itself.
Maybe I'm just interested in the semi-quick method of identifications.
Have to move on at some point.

 

[adam_mizer]

Figured I would still use this thread to try to identify my brew.

Still having some problems because of the material I'm cooking.
This batch had 13-14 grams of a couple nice dental retainers along with GF watch materials.
I use a poormans AR with crystal sodium nitrate salt.
Here's a couple shots.

Evaporated the brew, dropped gold with SMB and some salts came down with it.
First thought too much SMB as I was expecting 10grams gold added 20 grams SMB.
Havn't finished cleaning the gold because I have run into strange pm salts and colors.
On the first HCl clean-out it did pickup some of the salts, but after the water rinse I noticed the salts were still there.
Sort of reminded me of copper-chloride salts, but did not go up in HCl like they usually do.
I'm okay with that thinking I could do a second HCl, but decided to go to ammonia wash.
Well second wash with ammonia is what the pictures are displaying.
First off I don't know why the color is so strong, unless there was alot of silver. Usually I get pretty much all the silver before I start the wash/rinse cycles.
Next is whats on the bottom of the flask?
Lots of yellow.
Here's another twist to the story.
After the SMB drop, I pour off solution and get to the gold. Usually do this twice (sometimes 3 times) as it helps stir up the mix and I want to make sure I get all the gold. Funny after the first time much more salts were on the bottom of the solution.
Well I did not mix that in with my first drop of the gold powder.
But I did pour the ammonia from my wash cycle from the first gold drop into that drop of salts and thats when I got the yellow stuff.
A stannous test of the first wash of my gold in HCl, shows a little yellow lime-green on the wash out solution.
A DMG test on swab of the ammonia liquid wierd blue color kind of tells me theres something in the ammonia.
Also why is there a yellow salt, it was gray and white type salts before the amnmonia was added.
Is this a PM or just waste metal salt??

 

[Oz]

I am having trouble following what is going on as to your steps, but I did catch that you are adding back an ammonium hydroxide wash to your solution. You better know what you are doing there as ammonium hydroxide can ruin your day with a bang when mixed with metals in solution.

Remember how everyone is told after washing their gold precipitates with ammonium hydroxide to remove silver chloride to acidify their wash solution afterwards, there is good reasoning behind that step.

 

[rusty]

Thank you, will dilute and retest.
The blowpipe borax test, is there to be a color reaction?

Also forgot to mention this is my remainder waste liquids, and only because that stannous test, makes me believe something is suspended.
The q-tip swab had only a very tiny band of black very thin, and the remainder of the swab was yellow-green this morning.

Grab a copy of "You Can Smelt Too" starting on page 35 THE BLOWPIPE :ITS PURPOSE AND OPERATION

 

[butcher]

You had an acidic chloride solution with metals dissolved in solution (which metals I do not know) (some of them were insoluble as chlorides so that eliminates a portion on the list), then you changed the pH to alkaline (or at least more towards that direction), which would precipitate the metals that the acid held, depending on pH would also be a clue to which metals you possibly have in solution, again depending on the pH, if this is an alkaline solution (on the ammonia side) which it looks to be but looks can be deceiving, the blue is most likely a copper amine, or even possibly some nickel, the yellow could be a number of metal salts including copper, did you do a DMG spot test on this blue solution?

Several metals will form amine solutions in ammonia, and you may find if you separated the yellow salts and treated these with more ammonia they too may dissolve, or a portion of them may (just speculation).

You may also try separating portion yellow powders and acidify them with HCl, a portion in H2SO4, this may give some clues also.

Flame tests
Experiments in qualitative analysis of Cations
Qualitative inorganic analysis
And other searches like these may help, in your search of finding out as much as you can.

Pay close attention to OZ's advice and do not let any of the ammonium powders dry out, acidify them first for your safety.

Without knowing (or having some good clues) what metals were dissolved into solution your search (or process of elimination, or identification), can get very intensive and time consuming trying to figure out what each metal is.

After getting out the valuable metals I am seldom concerned with what all the other metals are, although it would be nice to find out.

 

[adam_mizer]

Thanks Oz,
Its pretty fearsome thinking about a explosive reaction and after I read your reply it was the correct thing to do acidify the solution while I get some homework done.
Actually undo what I started.

Maybe I can clarify this once more.
The mix had my same old stuff and a little added goodies, the whole mix was about 200 gram of mostly GF metals which included watch cases, watch band tops only, a few grams of 10k gold from early 1900 pins and the most stupid thing (I did) to add was the 13.5 grams of dental retainers that I thought were gold carrying material.
I was wrong apparently, this dental mixture is the stuff with my problem.

What happened was I cooked in PoorMans as I always do.
Several clean-outs of the poormans later, a stannous test shows black like gold in solution (Solution not taking up anymore metals).
There was a bit of light green mixture on the stannous later a slight darker color change. A day later there was still residual black on the stannous swab like gold.
Here's something funny, after I poured this off and saw in the bottom of the pot was still some gold.
Well this has happened before that I got gold in 2 cookings from the same pot.
Okay the second cooking was done and got some gold (maybe a little more than half of the expected return).

On the first cooking, the one in question. It was evaporated to 1/3rd to remove nitric.
This solution was filtered. Clear dark green.
20 grams SMB added was a little overkill but thinking I could get 10 grams gold at best.
Now a drop reaction started. (Unusual)!
First drop looked like gold powder. Poured this off and had what looked like white crystal in it with the gold powder and thinking about it I thought it was excess SMB.
Okay set to side the supposedly gold powder with white salt. (Will post a picture when I get home, the mixture has been washed twice already in each HCl,ammonia,HCl,ammonia). Note: its still too dark.
Now looking at the original solution for maybe more gold powder, the solution dropped on its own white salts again. (Nothing added to the original poured off solution).
Kind of makes you think it was copper chloride from maybe being highly pregnant.
Well cleaned out that second drop of salts and it was grey and white mix being more to the grey side and pepper added like some residual gold powder.
Put this in a seperate flask.

Now back to cleaning my original supposedly gold powder drop.
HCl again, solution is clean clear. Powder still appears too dark.
Okay try ammonia again, very light blue and cloudy. Pour this off into my blue solution in flask.
Now a bunch of chlorides are dropping out of solution. After taking that picture posted earlier.
Pretty sure there are couple different metals in that flask with the ammonia.
I acidified the ammonia and there's still a yellow on the bottom, I will remove this tonight.

The blue solution test swab DMG is a previous post ammonia 3 with the DMG swab on the right side.
Will try some different tests on the existing yellow portion of salts sitting on the bottom.

Butcher you mentioned do not let any of the ammonium powders dry out.
So being dry is where the mixture may have an explosive nature.
Also if the ammonium mixture was left to sit (the blue mixture) could this cause a violent reaction?
I was quite a bit worried and put acid in the flask right away.

I'm only after the PM's and don't want to toss them and for any other metals I don't want to spend to much time analyzing them.
Not used to seeing yellow powder at all, but the powder may change color when dry, so first on my list is to take this yellow salt out of the flask and find out what procedure to take to clean the gold powders which are contaminated with a PGM I'm sure.