bunch of questions about silver chloride

[GoIdman]

Purchased silver nitrate crystals, dissolved im distilled water. Filtered. Solution was cloudy. Refiltered, same result. Proceeded anyhow.
I used the sugar lye method for this process.

Yes I added some salt to precipitate the chloride, when it settled, I decanted the liquid, gave it multiple cold distilled water washes. Then added cold water ( dont know if this was right or wrong ) and started adding NaOH. That was the point where I saw the chloride coverting into a very fine ' OXIDE POWDER'. Fine enough to make my conversion observation somewhat tough. Moreover, I added sugar to it and could see the reaction following through. I guess my only tell was this mirror effect.

So here I am, stuck with a mirror on the bottom of my beaker. Any methods to remove and recover?

Hi,

Dont want to interfere with your processes or methods, but if you had silver nitrate crystals, and you have dissolved it in distilled water, wouldn`t be the easiest way to recover and refine the silver, a copper pipe and a silver cell?

I think you overcomplicated simple things.

Pete

 

[lazersteve]

I assumed the same, but I'll repurchase it and retry with a different method. I was thinking a copper bar..

I would advise against buying any more if you don't find your missing 90% loss.

Start by adding more sodium chloride (rock salt) dissolved in tap water to the mother-liquor that contained the AgNO3 to ascertain if you used enough salt in the original AgCl precipitation. If that turns up nothing then my assumption would be you either started with impure AgNO3 or it was not the mass you think it was (grains vs grams comes to mind)

Key take away here is record data (mass, temperatures, volumes, molarity, etc) about your reactions at every stage. This way when problems arise you can trace back to find the problem. Another important factor is to know the purity of your reagents. In this case it's pointing me to believe you could have a bought a "misrepresented" batch of AgNO3 assuming you did everything else correctly, which adding salt, lye, and sugar are about as simple as any process gets.

Steve

 

[Martijn]

Can anyone tell me what this ?

This is the sludge I have post decantation process. Could this be silver or am I wasting my time tryimg to further decant and recover if any PM?

I did not see a reply to this question, so; Yes that does look like fine silver powder after Lye/sugar.

 

[J.Najam]

Dont want to interfere with your processes or methods

Hello,
Thanks for your response and I don't see any interference, its an open discussion forum

wouldn`t be the easiest way to recover and refine the silver

Yes, there more than a couple methods of doing this. Sugar/lye, Copper bar/pipe, Silver cell, sulfuric/iron, Pure Zinc/tin/aluminum (takes longer) precipitation.

I chose the sugar/lye method as it was enticing and I'd seen the entire process carried out and shown in detail by Sreetips. I did not want to experiment anything using my own intellect the first time, so I chose to follow his process step by step. I may have made mistakes (most certainly). As well as @mikeman001 , hence the result seemed indifferent. Although I do read that many people here suggest and practice otherwise (not so much in favour of sugar/lye). I may try the other methods at a later point in time.

 

[J.Najam]

I would advise against buying any more if you don't find your missing 90% loss.

Sir the only remains I have is the sludge I'd have posted earlier, its untouched so far. Have kept it out in the open sun to dry out. No colour change nothing there as well.

If that turns up nothing then my assumption would be you either started with impure AgNO3

True, this could be another factor.

Another important factor is to know the purity of your reagents. In this case it's pointing me to believe you could have a bought a "misrepresented"

Fraudulent activities are very common around the globe, it could lead me to believe in this too. It was sold as 99.8% pure.

I'm only hoping I'm wrong, after I treat the other remaining sludge I have.

 

[J.Najam]

I did not see a reply to this question, so; Yes that does look like fine silver powder after Lye/sugar.

Really? You mean its in a ready to melt position? Dry and melt?

 

[Martijn]

Test a bit if it darkens with lye. If it does, there is still silver chloride.

 

[J.Najam]

Test a bit if it darkens with lye. If it does, there is still silver chloride.

Sure, ill test it first

Thanks

 

[J.Najam]

Since I'd left it in the sun to dry out, this precipitate has formed and the sediment is still somewhat moist.. should I still proceed with the melt? Ill completely dry it out on a hotplate though

 

[Yggdrasil]

Since I'd left it in the sun to dry out, this precipitate has formed and the sediment is still somewhat moist.. should I still proceed with the melt? Ill completely dry it out on a hotplate though

We would appreciate it if you use gloves.
Even if it is just a photo session the ourside can be contaminated with who knows what.

 

[J.Najam]

We would appreciate it if you use gloves.
Even if it is just a photo session the ourside can be contaminated with who knows what.

Well understood, i just picked it up for this snap, its back where it was. Hands washed right after

 

[orvi]

Test a bit if it darkens with lye. If it does, there is still silver chloride.

Actually, for me, it was always easier to take half teaspoon to the melting dish and melt it with oxy/propane torch. If there is AgCl left, you will see white fumes arising. You cannot miss it, and it is very reliable proof that you have AgCl locked in the material. By doing this, you can also judge about how much do you have in - meaning, if you need to re-work the lot, or you will mix in some soda to the charge and cover with thin blanket of soda and you will be fine

 

[J.Najam]

Actually, for me, it was always easier to take half teaspoon to the melting dish and melt it with oxy/propane torch. If there is AgCl left, you will see white fumes arising. You cannot miss it, and it is very reliable proof that you have AgCl locked in the material. By doing this, you can also judge about how much do you have in - meaning, if you need to re-work the lot, or you will mix in some soda to the charge and cover with thin blanket of soda and you will be fine

If there is one thing I cannot miss, is the details you point out @orvi . agreed and understood, ill first test it with lye as suggested by @Martijn. Then melt a little as you have suggested. Just waiting on my silica crucible arriving in a couple of days hopefully.

Since I'd left it in the sun to dry out, this precipitate has formed and the sediment is still somewhat moist.. should I still proceed with the melt? Ill completely dry it out on a hotplate though

In the meantime, how would you gauge what this might be and what is the suggest treatment?

 

[Martijn]

Looks like a salt that can be washed with water.

 

[J.Najam]

Looks like a salt that can be washed with water.

Alright. Noted

 

[mikeman001]

If there is one thing I cannot miss, is the details you point out @orvi . agreed and understood, ill first test it with lye as suggested by @Martijn. Then melt a little as you have suggested. Just waiting on my silica crucible arriving in a couple of days hopefully.

In the meantime, how would you gauge what this might be and what is the suggest treatment?

Your crucible arrive?

 

[J.Najam]

Your crucible arrive?

It did arrive, but I'm really disappointed in myself. I was so consumed with my DIY furnace having to work properly as I'd built it my first time, I forgot to test the remaining sludge with some lye and pretest a teaspoon of it in the furnace. I dried and added the whole powdered sediment as is, but the observation was quite surprising. No white fumes initially, but also after one hour, I lifted the lid just a little bit to check the status of the sediment added to the melt dish, It didn't seem to have affected by even a tiny bit? They were just powders, did not change its form anyhow. My crucible went red hot, there was a fire emitting the lid hole and it was quite hot, even the lid kind of cracked. When I used a graphite rod to stir and confirm the same, the dust kind of moved freely along the crucible. I thought maybe if I could hit it with fire from above, (than below as in my furnace) it may stick to the crucible better and start to melt from there on. As soon as I hit the flame directly onto it, BOOM! I lost all the powders in thin air. I was left dumbfounded as I'd no clue what to do from there on. Another hardworking week came to a shattering end.

As a blessing in disguise, looks like a portion of the dish wasn't glazed properly so I still have some of the powder stuck onto my crucible, I'll share its picture by end of day.

 

[J.Najam]

The little damage done in my butane furnace

 

[mikeman001]

Damn, Ive been gone awhile, that sucks your lid cracked... hey you can get kaowool off eBay. It's a high thermal resistant ceramic fiber glass like insulater. Just use a respirator if you do work with it. And all PPE for that fact. Also a fella that goes by the name of nighthawk on you tube has a blueprint for making a material that is the equivalent to starlite. Super easy and cheap to make, and a cutting torch, oxygen acetylene, doesn't even touch this stuff. I've tried it many times myself. I will post a hyperlink shortly!

 

[mikeman001]