Snowballs

[orvi]

Despite the >30°C outside during the day, I managed to prepare some snow. Very nice, crystal white, and nicely packing to the ball shape
Ah, it never gets old to wash it with glove inside the bucket with warm/hot water. I like to feel the structure and break the lumps. When properly washed with hot water, it changes the structure, and do not escape from the hand when squeezed - instead it could be squeezed into very compact shapes that hold the shape.

Expecting somewhere around 1,25 kg. We will see

(for those who do not know what is it, it´s silver chloride )

 

[Yggdrasil]

Despite the >30°C outside during the day, I managed to prepare some snow. Very nice, crystal white, and nicely packing to the ball shape
Ah, it never gets old to wash it with glove inside the bucket with warm/hot water. I like to feel the structure and break the lumps. When properly washed with hot water, it changes the structure, and do not escape from the hand when squeezed - instead it could be squeezed into very compact shapes that hold the shape.

Expecting somewhere around 1,25 kg. We will see

(for those who do not know what is it, it´s silver chloride )

Kids find fun everywhere
Don’t loose that spirit.

 

[4metals]

When you have enough to make a snowman it will really be special.

But don’t let him dry out!

Nice work.

 

[orvi]

When you have enough to make a snowman it will really be special.

But don’t let him dry out!

Nice work.

Yeah, I knew about dry AgCl issue the hard way, but that was small lot and long time ago.

Very troublesome batch (so I make fun about it ), as I currently do not have access to my large scale equipment, mixers and filtering PP cloth "suckers" (filters, two welded PP non woven cloths welded together with PE mesh inside, and tube welded to it for sucking the liquid).

So again, bench, 5L beakers and LOTS of time and work wastefully spent. I must purchase a new dril with mixing adapter today just to finish it in time, my old trusty drill is packed at my house 400km away...

And, also experienced very frustrating close-call today. In English, it even rhymes... Lye in the eye. Fully suited with face shield, coat, boots... Mixing it in the bucket. It splashed a few small drops towards my face (but shield still in place). But I instinctively jerked/blinked, and face shield fallen a good bit to my forehead (making a small empty space on top). To the point drill stop moving the stuff, another small swarm of tiny droplets flew in direction of my face and one sneaky b... droplet make its way over the shield and fallen right to the top of my eye and sneaked under eyelid. Whole incident took like 1,5 seconds.
Adrenalin 1000, pain 1000, smashing stuff to the ground and running to the sink... Washing and eye massage for 10 minutes under cold water... I will never forget it.
Luckily, I am able to see. Little blurred (but I assume just from irritation) for few hours, now very close to normal. I hope it will be completely fine in few days.
That feeling when you instruct every student you have to properly wear all safety gear, and then, when you wearing it, miserable coincidences can mess it up in fraction of the second and accident happen. Thorough lesson learned.

 

[4metals]

Glad you are OK. Yes, lye in the eye sounds cute, but is not in any way pleasant.

The problem with the mixing blades on a drill is the tendency to lift it out of the vessel when it is running and splatter it all around the room. Don’t ask me how I know this!

 

[orvi]

All of this for a the final "silver" beaker I do not know if it was worth it. But I needed to finish it till friday. And recover the money. I think that I am abandonong silver for some time, and espetially lye/sugar route without proper gear.

 

[Palladium]

I run mine in 55 gallon drums and it scares the blanky blank out of me. The mist is the worse! Anyway i run the blade in a counter clock wise motion so the solution is drawn toward the bottom of the barrel creating a suction instead of the other way where the solution is drawn upward and tends to spit at you. I DON"T LIKE LYE!

 

[orvi]

Glad you are OK. Yes, lye in the eye sounds cute, but is not in any way pleasant.

The problem with the mixing blades on a drill is the tendency to lift it out of the vessel when it is running and splatter it all around the room. Don’t ask me how I know this!

Yeah. Something similar happened to me. I was cautious about the speed, but your finger isn´t digital, and for second or two from the few minutes of mixing, it just happen tah you "overdrive" it, and bad things happen.

 

[4metals]

I have one client who has a huge drill operated mixer he always uses. What he did is unique. He mounted the drill over a 15 gallon bucket and he puts the mixer into the bucket drops a funnel, upside down, over the shaft to catch splatter and attaches the mixer to the drill. There are 3 or 4 stainless bolts sticking into the bucket so the funnel rests on it. The funnel large OD fits nicely in the bucket so nothing splashes out but easily slides up so you can check on whats happening.

Actually an elegant solution.

 

[Shark]

Lye or sulfuric, to me is a toss up. Both can be nasty and unforgiving. Glad your O.K. I enjoy your posts to much for you to be out of action.

 

[orvi]

I run mine in 55 gallon drums and it scares the blanky blank out of me. The mist is the worse! Anyway i run the blade in a counter clock wise motion so the solution is drawn toward the bottom of the barrel creating a suction instead of the other way where the solution is drawn upward and tends to spit at you. I DON"T LIKE LYE!

I have designated 30L duplicator from two thick plastic (PP) drums for this type of reactions. Outer coat is circulated with hot water for necessary heating, and inner one has small hole in the lid for the mixer. Nice, closed system, you set the drill on the fixed stand and let it run for hour and work is done.
But it happen that I needed to pack my things and move to the other place... So this happened.
Ag2O to the Ag I have nicely optimized, ran in the same vessel afterwards, but through another hole, I stick the thermometer in, dose the sugar to the stirred slurry, watch the temperature rises and tame it under 110°C. Replacing the hot water with cold helps to manage the exotherm. Nice and steady additions and reaction is tame, temperature is maintained and consumption of sugar is minimized. When temp stop rising, I add last dose of sugar "for sure", wash the walls of the drum into the main body of slurry and let it stirr on minimal speed for like 1 hour, still running the cold water in the jacket. When it reach acceptable temp, I remove the mixer and lid, submerge the "sucking" pad into it and start the washing phase.

Yeah, man... How I hate that choking hydroxide vapors.

 

[orvi]

I have one client who has a huge drill operated mixer he always uses. What he did is unique. He mounted the drill over a 15 gallon bucket and he puts the mixer into the bucket drops a funnel, upside down, over the shaft to catch splatter and attaches the mixer to the drill. There are 3 or 4 stainless bolts sticking into the bucket so the funnel rests on it. The funnel large OD fits nicely in the bucket so nothing splashes out but easily slides up so you can check on whats happening.

Actually an elegant solution.

Very nice solution I am writin this up to my notebook, I maybe use this in the future built of the new equipment.

This is why I like this forum so much. So many knowlegable and experienced people here, sharing their knowledge for everybody´s advantage.

 

[orvi]

Lye or sulfuric, to me is a toss up. Both can be nasty and unforgiving. Glad your O.K. I enjoy your posts to much for you to be out of action.

Yeah. And for me, 65% or more nitric sits on top of everything. If it was nitric, I could have been Usain Bolt, and I will never run fast enough to salvage my eye.

 

[4metals]

The client who has this does not have a lot of hood space so a lot happens out of the hood. This funnel has about an 1 1/2” spout and where it comes out of the funnel he has glued on a PVC tee which connects to a good exhaust. I am not sure if his mixer has any blades that would direct the mixing up or down. But, bottom line, no fumes and the exhaust on a flex line doesn’t prevent lifting the funnel to check things.

Unfortunately his shop is kind of a reproduction of the black hole of Calcutta so I never snap any photos there.

 

[Palladium]

I like the way you methodically approach things with measurements and such.
I can't do it that way. I do my measurements for conversions and such, but other than that i just go by experience and roll with it! I'm kind of like a mad scientist, but in a cautious safe way.

I have used a 4 ft blending mixer attached to a 1/2 in drive drill. Then i used a couple of 2 x 4's to make a cross brace to sit across the barrel. For separating the bulk of the solution from the chloride i used a washing machine to centrifugally separate them. A diaphragm pump moves the chlorides from drum to drum. It can pump them without a problem. Once you get the bulk of the solution off washing is a breeze. You can do the same with the powder. It cuts down on a lot of water usage and help my evaporator fans keep up.

In my 2nd lab build i changed a few things, but the concept is the same. I bet you never though you would see a washing machine in a refining lab.

You can see the first build here.

 

[orvi]

The client who has this does not have a lot of hood space so a lot happens out of the hood. This funnel has about an 1 1/2” spout and where it comes out of the funnel he has glued on a PVC tee which connects to a good exhaust. I am not sure if his mixer has any blades that would direct the mixing up or down. But, bottom line, no fumes and the exhaust on a flex line doesn’t prevent lifting the funnel to check things.

Unfortunately his shop is kind of a reproduction of the black hole of Calcutta so I never snap any photos there.

I, as refiner, grown in the place you name black hole and so I hated it that much, that I always wanted to have it as clean as effectively possible. No unlabeled beakers with whatever green black sludges, slowly climbing outwards. And myriad of smelly drums with waste in the "backyard" waiting for the another "next week we certainly work it and dispose it"
Exhaust is nice thing to have, espetially with lye and NOx-es... I have an advantage of the pro-fumehood (altough old, but working as it should), but it is out of capacity for "drum" sized reactions...

 

[orvi]

I like the way you methodically approach things with measurements and such.
I can't do it that way. I do my measurements for conversions and such, but other than that is just go by experience and roll with it! I'm kind of like a mad scientist, but in a cautious safe way.

I have a used a 4 ft blending mixer attached to a 1/2 in drive drill. Then i used a couple of 2 x 4's to make a cross brace to sit across the barrel. For separating the bulk of the solution from the chloride i used a washing machine to centrifugally separate them. A diaphragm pump moves the chlorides from drum to drum. It can pump them without a problem. Once you get the bulk of the solution off washing is a breeze. You can do the same with the powder. It cuts down on a lot of water usage and help my evaporator fans keep up.

In my 2nd lab build i changed a few things, but the concept is the same. I bet you never though you would see a washing machine in a refining lab.

You can see the first build here.

I am grown in precise lab, run by a boss with "German school". After many years in university, it make a sharp mark in your behavior you realize it when you use kitchen scales for measuring the ammount of milk for pancakes not graduated bowl because you realize you can tare the bottle and pour directly no need for washing another dishes... Long story short.

Yeah. Lye/sugar is something like pseudo-chemistry conversion. Always behave bit different, and absence of easy analytics make it nightmare for newbies.
But I am catching some experience hints from numerous reactions I ran. Colour of the silver when doing lye sugar for example. Consistency of AgCl during the washing steps (snowballs )... Colour judging of the reaction mixture when precipitating palladium out of copper solutions with formate. Etc. Saves a ton of time.

Washing machine is very, very clever invention very, very clever. I very appreciate the genius of inventions coming from lack of professional equipment (which cost thousands, we do not have).
When I am sucking the solution with "sucking pad" placed n the bottom of the drum, I use another as vacuum filtering flask. Second drum is filled with PVC pipes to withstand the negative pressure, and you can happily suck 50L of solution with small vacuum pump from Aliexpress. Then you just empty the drum and go for another cycle of washing.
Decanting is tedious, as too much solution is locked in the solids. I will need to decant at least 5-6 times to achieve acceptable washing efficiency. With sucking pad (essentially filtering), I am sometimes OK with two washings (pass NH3 test for copper, with AgCl for example). No more than 4.

 

[orvi]

So I finally dryied and weighed the stuff. To my surprise, I got lucky and scales shown 1,418 kg sweet bonus for all of the trouble and nerves connected with this batch. Melting loss is only 1% for the powder run without any flux (ca 8g sample), so conversion was relatively complete and practically zero AgCl made it through whole process.
Purity is nice, 99,93Ag and some AuCu impurity, but that could be from the previously used graphite crucible. Powder measured only Ag on XRF. No Cd or Cu, so I am happy.

 

[Shark]

I got lucky and scales shown 1,418 kg

I need a set of those scales when selling,

 

[Palladium]

I need a set of those scales when selling,

So much for the days of postage scales and nickles!