ok wheres my deal.im both new to refineing and new to this site.what ive done so far.i took 330 grams of sterling added 495 ml of distilled water(1.5 ml. per gram) then added 412 ml of nitric acid (1.25 ml. per gram)digested with heat.placed thick copper wire in it.got alot of setiment.filtered then rinsed.rinsed again and again.i took and fired with torch.ended up with 225 grams of nice looking silver (i believe i used to much borax in my crusible one side is super glassy)ok heres my issue while rinsing i had some persipitant come thur filter and into my rinse.so i just added it with the spent acid now i have probably more than doubled the volume.i need to know how to get the rest of the silver out of that solution.i have bought some lye crystals from lowes(drain cleaner)and also have karo. im just now sure how much of each to add.and do i need to take the water off the top first.i will says im learning from my mistakes.first one dont put spent materials in a amber container.cant really see what you have.any help greatly appreciated.also wanted to throw a big thanks for this forum and all you guys that have done the utube thing.
newbie needs help
- Thread starter goldfor2
- Start date
Help Support Gold Refining Forum:
Am I missing something in the post, did you make silver chloride?
Woodworker1997
Well-known member
goldfor2,
Hello and welcome!
Would! you please give us your general location?
Derek.
Hello and welcome!
Would! you please give us your general location?
Derek.
Yes i do believe i had
Silver chloride. Maybe more like copper chloride now. By the way sorry for the lack of introduction. I'm 39 years old. And live in central ky. have been buying and selling previous metals sense 2001. Watched a 60 minutes special on tv. That year and thay were talking about gold rising so i started buying. Due to the fact that I'm not rich and am raising two kids money doesn't go far. So while buying jewelry karat. Then selling on eBay originally until I found local guy that pays 95% on gold. So i had been dealing with him for ten years. But the pay out on silver wasent what I felt it should be. (Not his fault) I started looking at utube. Well here i am now.
Silver chloride. Maybe more like copper chloride now. By the way sorry for the lack of introduction. I'm 39 years old. And live in central ky. have been buying and selling previous metals sense 2001. Watched a 60 minutes special on tv. That year and thay were talking about gold rising so i started buying. Due to the fact that I'm not rich and am raising two kids money doesn't go far. So while buying jewelry karat. Then selling on eBay originally until I found local guy that pays 95% on gold. So i had been dealing with him for ten years. But the pay out on silver wasent what I felt it should be. (Not his fault) I started looking at utube. Well here i am now.
Ok after putting on heat and all metal digested. I added about. 14 grams of 999 silver digested it as well but slowly(Trying to exhaust nitric). So i went to the next step and added copper. I believe my nitric was still a bit hot. Because my setiment would float then sink. Did i use to much nitric. I looked over this site and utube and went with the receipt that used the least amount of nitric because of the cost. But i believe i could have used even less. Any thoughts
goldfor2,
I was born and raised as a child in Kentucky, so I consider it home.
I would like to help you and discuss your problem, but unless you are more clear, in describing what you have or have done it is hard to give advice, or even to keep up with what you may or may not have, we cannot see what you did, we have to go by what you tell us.
So from what I understand so far:
You dissolved some sterling in nitric acid, and cemented the silver back out using copper metal, and melted the silver.
You had some insoluble material from originally dissolving the silver, and from the rinses, washes, that is now dilute from the washes.
It sounds to me like you may think you have dissolved silver in this dilute solution or in the insoluble material.
You speak about silver chloride, and the chemicals we use to convert the silver chloride, but you do not make it clear you made silver chloride, you do not mention anywhere how you think you got silver chloride.
Where did a chloride come from from your water, or did you add HCl or NaCl?
Why do you think you made a chloride of silver or copper?
I am having trouble knowing what the question is for sure.
You had 330 grams of sterling silver, (about 92.5% Ag, 7.5% Cu).
330g sterling X 0.925 Ag = 305 grams of pure silver expected.
330g sterling X 0.075 Cu = 24.75 grams of copper expected.
nitric acid needed can depend on several factors in your processes, and amount needed can depend on several factors. we normally try to calculate about how much we need.
We normally can use some numbers to go by to get a close guess to how much nitric we need.
Some number like:
1.2ml of 70% HNO3 for each gram of pure silver (mixed with equal volume of water).
Since it takes about 3.4 times this amount of nitric to dissolve a gram of copper,
1.2ml X 3.4 = 4.08
so we can see it can take about 4ml of 70% HNO3 per gram of copper (mixed with equal volumes of water).
so using these numbers, we could figure:
For 330g Sterling.
305 grams of pure silver expected, and 1.2 ml 70% HNO3 per gram of silver.
305g X 1.2ml = 366ml of 70% HNO3 (mixed with 366ml water), is what we may expect to dissolve the silver.
And
24.75 grams of copper expected, and 4ml 70% HNO3 per gram of copper.
24.75g X 4ml = 99ml of 70% HNO3 (mixed with 99ml water) is what we expect to dissolve the copper.
So adding these together:
366ml +99ml = 465 ml of 70% HNO3 + 465ml water,
is what we expect to use to dissolve 330 grams of sterling silver.
We expect to cement out about 305 grams of a higher purity silver from this solution.
{this is wrong,We can expect to dissolve about 3.4 times that amount of copper from our copper metal buss bar to cement that 305 grams of silver, 305g X 3.4 = 1037g of copper expected to dissolve from out copper metal bar to cement the silver}
I made a mistake here and got this backwards, 1 gram of copper metal will replace 3.4 grams of silver from solution, for 305 grams of silver in solution we can expect to dissolve around 89.7 grams of copper from the copper buss bar. 305g /3.4 =89.7
If we do not use enough acid we may not dissolve all of the metals.
If we use too much acid, we will dissolve more of the copper buss bar, before we get all of our silver back.
These are not exact figures there can be many variables, like acid strength and how we use the nitric or do the process, like refluxing acids or working in open containers with large amount of the acid going up in smoke as a red cloud, Our metal content, and even the figures we use to calculate approximate usage, but this gives us at least a starting point, and can help us to get a fairly good idea of how much acid we may need, or a guess of how much metal to expect...
I was born and raised as a child in Kentucky, so I consider it home.
I would like to help you and discuss your problem, but unless you are more clear, in describing what you have or have done it is hard to give advice, or even to keep up with what you may or may not have, we cannot see what you did, we have to go by what you tell us.
So from what I understand so far:
You dissolved some sterling in nitric acid, and cemented the silver back out using copper metal, and melted the silver.
You had some insoluble material from originally dissolving the silver, and from the rinses, washes, that is now dilute from the washes.
It sounds to me like you may think you have dissolved silver in this dilute solution or in the insoluble material.
You speak about silver chloride, and the chemicals we use to convert the silver chloride, but you do not make it clear you made silver chloride, you do not mention anywhere how you think you got silver chloride.
Where did a chloride come from from your water, or did you add HCl or NaCl?
Why do you think you made a chloride of silver or copper?
I am having trouble knowing what the question is for sure.
You had 330 grams of sterling silver, (about 92.5% Ag, 7.5% Cu).
330g sterling X 0.925 Ag = 305 grams of pure silver expected.
330g sterling X 0.075 Cu = 24.75 grams of copper expected.
nitric acid needed can depend on several factors in your processes, and amount needed can depend on several factors. we normally try to calculate about how much we need.
We normally can use some numbers to go by to get a close guess to how much nitric we need.
Some number like:
1.2ml of 70% HNO3 for each gram of pure silver (mixed with equal volume of water).
Since it takes about 3.4 times this amount of nitric to dissolve a gram of copper,
1.2ml X 3.4 = 4.08
so we can see it can take about 4ml of 70% HNO3 per gram of copper (mixed with equal volumes of water).
so using these numbers, we could figure:
For 330g Sterling.
305 grams of pure silver expected, and 1.2 ml 70% HNO3 per gram of silver.
305g X 1.2ml = 366ml of 70% HNO3 (mixed with 366ml water), is what we may expect to dissolve the silver.
And
24.75 grams of copper expected, and 4ml 70% HNO3 per gram of copper.
24.75g X 4ml = 99ml of 70% HNO3 (mixed with 99ml water) is what we expect to dissolve the copper.
So adding these together:
366ml +99ml = 465 ml of 70% HNO3 + 465ml water,
is what we expect to use to dissolve 330 grams of sterling silver.
We expect to cement out about 305 grams of a higher purity silver from this solution.
{this is wrong,We can expect to dissolve about 3.4 times that amount of copper from our copper metal buss bar to cement that 305 grams of silver, 305g X 3.4 = 1037g of copper expected to dissolve from out copper metal bar to cement the silver}
I made a mistake here and got this backwards, 1 gram of copper metal will replace 3.4 grams of silver from solution, for 305 grams of silver in solution we can expect to dissolve around 89.7 grams of copper from the copper buss bar. 305g /3.4 =89.7
If we do not use enough acid we may not dissolve all of the metals.
If we use too much acid, we will dissolve more of the copper buss bar, before we get all of our silver back.
These are not exact figures there can be many variables, like acid strength and how we use the nitric or do the process, like refluxing acids or working in open containers with large amount of the acid going up in smoke as a red cloud, Our metal content, and even the figures we use to calculate approximate usage, but this gives us at least a starting point, and can help us to get a fairly good idea of how much acid we may need, or a guess of how much metal to expect...
Butcher thanks for advice. I have not added any hci or anything else right now there is simply water nitric acid. Silver and copper. In that order. Guessing about 1000ml. Water close to 400ml. Nitric.still about 2.5 oz silver and what ever copper didn't go up in smoke or come off my copper wire. Nothing more nothing less. I didn't want to do something i regretted. So i stopped and came to you guys. You know the experts. I have read on here to add murtic then Lye then suger. But how much i don't know. Like i did earlier i believe my nitric was still hot. It did digest quite a bit of copper. Now my solution is very dark green. Well before i added all the wash water how this gives you a better idea where I'm at. And i do apologize for my lack of info. Not only am i new to refining but this is also the first time ever posting on any forum. And my brain seems to go faster then my typing. Lol....
When you say the solution is dark green, this gives me the idea there is still some free nitric acid in solution, copper nitrate is blue, but the NOx gases can make it look green, a tiny bit of palladium can give color to solution, but with sterling silver that is unlikely unless this was plated jewelry or something.
I would not make silver chloride if I can help it.
You can test the solution to see if you have silver left in it, take a small sample, add some NaCl (common salt), or HCl to the test sample, if you see a white cloud form, or a white powder precipitate it is silver chloride, proving there is silver in solution.
If the solution is green I suspect you do still have some silver in solution.
normally just letting the copper sit in it will cement out the silver and the solution will go blue.
Silver normally cements easier from dilute solutions, (if it is at least a tiny bit acidic), so you can probably just clean and return your copper bar to the solution and cement out any silver silver in solution.
Or
If solution is very dilute you can heat the solution in a corning dish on a hot plate, with your copper bar sitting in solution, the water will be driven off, the acid concentrate and consume copper and cement silver from solution.
Note heating can put more metals in solution while hot (dissolve or hold more metal salts in solution), and as the solution cools can precipitate this excess metal salt back out of the hot solution, so you could end up with a little more copper in your cemented silver once done. than you had with your first batch of cemented silver.
My brain does not work well with typing either.
Actually sometimes I find it amazing my brain works at all.
Basically just keep up with your study, most all of these questions you have will be answered for you as you learn more about it.
I would not worry about making silver chloride, or converting it yet, you will learn more about that when you get further along.
I would not make silver chloride if I can help it.
You can test the solution to see if you have silver left in it, take a small sample, add some NaCl (common salt), or HCl to the test sample, if you see a white cloud form, or a white powder precipitate it is silver chloride, proving there is silver in solution.
If the solution is green I suspect you do still have some silver in solution.
normally just letting the copper sit in it will cement out the silver and the solution will go blue.
Silver normally cements easier from dilute solutions, (if it is at least a tiny bit acidic), so you can probably just clean and return your copper bar to the solution and cement out any silver silver in solution.
Or
If solution is very dilute you can heat the solution in a corning dish on a hot plate, with your copper bar sitting in solution, the water will be driven off, the acid concentrate and consume copper and cement silver from solution.
Note heating can put more metals in solution while hot (dissolve or hold more metal salts in solution), and as the solution cools can precipitate this excess metal salt back out of the hot solution, so you could end up with a little more copper in your cemented silver once done. than you had with your first batch of cemented silver.
My brain does not work well with typing either.
Actually sometimes I find it amazing my brain works at all.
Basically just keep up with your study, most all of these questions you have will be answered for you as you learn more about it.
I would not worry about making silver chloride, or converting it yet, you will learn more about that when you get further along.
Ok thanks. By the way there was a small amount of plated jewelry in there. I had quite a bit floating around. Just wanted to make sure i didn't lose that much a small amount i can handle one fourth is another story. Let me ask one more stupid question. Just by simmering the stream alone coming off wouldn't that lower my water content. With out the bar. Being in it. Or Will i lose pm that way
I made a mistake in the above post, I got it backwards of how much copper will replace how much silver from solution, I made a correction to the post above.
1 gram of copper metal will replace 3.4 grams of silver from solution.
You can evaporate a dilute solution water vapors off (first), if it gets concentrated, and there is free acids these free acids decompose and will begin to vapor off (or can dissolve more metal into solution as they concentrate, if there is metals the acid or gases from those acids can attack).
Metals will not leave the solution, (boiling can splash them out when bubbles pop) but in evaporation they do not leave the pot.
If the metal can make a salt with the acid, this metal salt will concentrate in solution, if evaporated far enough the metal salts can crystallize out of solution (depending on the salt and its solubility), the metal salts solubility plays a major roll here, sometimes we can have two different metal salts in solution and one will crystallize out before the other, there are times where we can use this to separate metal salts from each other. Temperatures can also play a big role in how soluble a metal salt will be in solution, normally a salt is more soluble in hot solutions than cooler solutions.
1 gram of copper metal will replace 3.4 grams of silver from solution.
You can evaporate a dilute solution water vapors off (first), if it gets concentrated, and there is free acids these free acids decompose and will begin to vapor off (or can dissolve more metal into solution as they concentrate, if there is metals the acid or gases from those acids can attack).
Metals will not leave the solution, (boiling can splash them out when bubbles pop) but in evaporation they do not leave the pot.
If the metal can make a salt with the acid, this metal salt will concentrate in solution, if evaporated far enough the metal salts can crystallize out of solution (depending on the salt and its solubility), the metal salts solubility plays a major roll here, sometimes we can have two different metal salts in solution and one will crystallize out before the other, there are times where we can use this to separate metal salts from each other. Temperatures can also play a big role in how soluble a metal salt will be in solution, normally a salt is more soluble in hot solutions than cooler solutions.
Pantherlikher
Well-known member
Hi...
To me there is too much thought going into the mix.
Butcher is great and educated guesses at how much of what does what but in the end, you only add alittle nitric at a time and wait untill it stops before adding more. That way, you have less of an excess nitric to deal with.
That said, I would let everything settle and pour off liquids. Adding alittle water and "decanting" again. This will rinse and rid the metal, solids, of acid.
First, do the silver test and see if the cloud appears to know for sure if there is silver still in solution. If so, put copper solid back in for a time and see what drops. Just remember the longer metalic copper is in the acid, the more copper will use acid.
If you plan on dissolving more silver, then I'd just save the "spent acid" and start your next batch in this solution, warmed not boiling. This will dissolve base metals and drop any silver that may be in it.
I have yet to do the silver side of "collecting" or "refinning" but I reuse spent solution from gold collecting to rid base metals before properly processing spent sdolutions.
This saves on acid as much as possible.
For learning and seeing how well you did, take a small solution sample and test to see if you got it all or need to rethink the process to get better results.
Hope this helps but definately keep reading through the forum as well as "Hoke's" book.
B.S.
...Most times the simple mind sees the best answer...
To me there is too much thought going into the mix.
Butcher is great and educated guesses at how much of what does what but in the end, you only add alittle nitric at a time and wait untill it stops before adding more. That way, you have less of an excess nitric to deal with.
That said, I would let everything settle and pour off liquids. Adding alittle water and "decanting" again. This will rinse and rid the metal, solids, of acid.
First, do the silver test and see if the cloud appears to know for sure if there is silver still in solution. If so, put copper solid back in for a time and see what drops. Just remember the longer metalic copper is in the acid, the more copper will use acid.
If you plan on dissolving more silver, then I'd just save the "spent acid" and start your next batch in this solution, warmed not boiling. This will dissolve base metals and drop any silver that may be in it.
I have yet to do the silver side of "collecting" or "refinning" but I reuse spent solution from gold collecting to rid base metals before properly processing spent sdolutions.
This saves on acid as much as possible.
For learning and seeing how well you did, take a small solution sample and test to see if you got it all or need to rethink the process to get better results.
Hope this helps but definately keep reading through the forum as well as "Hoke's" book.
B.S.
...Most times the simple mind sees the best answer...
goldfor2,
Keep up the good work, I know you will be teaching me many things.
We all learn from each other.
Keep up the good work, I know you will be teaching me many things.
We all learn from each other.
I believe you do lose a little when evaporating down! I do all my work outside without a fume hood (working on getting a lab) so I did a little test. I was evaporating a solution down just to make it more concentrated and I put my watch glass over it for a little bit. I then let the condensation build up on it, pulled my watch glass off and pulled out the stannous and sure enough the condensation on my watch glass turned purple. From there on I decided I will not be evaporating solutions down till I have a fume hood with a filter/scrubber that will catch these loses.
Tyler
Tyler
- Joined
- Feb 25, 2007
- Messages
- 8,360
A sign that you were evaporating too fast (too hot). If you evaporate at the suggested rate, and there's NO remaining metal to react with the acid, you should be able to process without a measureable loss. Out of curiosity, I processed a troy ounce of pure gold and recovered a troy ounce (to the grain) by careful washing of the filter. You can evaporate without a loss, but you must observe all the rules in order to succeed.moose7802 said:
Your comments are a perfect example of the importance of understanding the difference between the meaning of the words evaporate and boil. One does NOT boil when evaporating, and if one does, it can get very expensive.
Harold
I know what you mean Harold. I swear I was not boiling and the solution never bubbled. I don't know what the exact temp was but I know it never bubbled or bumped. I never thought that it could be too hot, as long as it wasn't boiling I thought I was fine. I was told that boiling bubbles are what carry your values out of the container once they pop. I am a newbie so I just want to know everything I can, I'm not questioning you Harold just want to get better at what I do.
Tyler
Tyler
If you set a cold watch glass over the beaker, and see a yellow or colored condensate, you are heating too high and loosing metals, the condensate should be clear, only gases of H2O, NOx, or HCl leaving the solution.
As we heat these in solution depending on what we have in solution, and the concentration, the boiling point of the solution changes, it also changes as the the solution concentration of the acids in solution change.
At the bottom of the vessel where the solution in direct contact with the hot plate we can have a heat higher than the boiling point of the acid, causing it to decompose and leave the solution rather violently as it rises through the solution as a gas, popping out of solution carrying metals with it. boiling is gases decomposed from acids at the bottom, (evaporation is from the surface).
Evaporation can happen at temperature way below the boiling point.
Water boils at 100 degree C, but we can evaporate water at room temperature.
Evaporation does not create bubbles large or small, it will not carry metals or salts from solution, it happens calmly and quietly at the surface of a liquid.
The bubbles do not always need to be like the very large bubbles we think of as boiling like when we get water moving in a rolling boil and where we see many very large bubbles of gases rising to the surface, we can heat the acid to a light boil and have many very tiny bubbles rising and popping and carrying metals with these many very tiny bubbles as they pop and spit up metals and acids solutions, as the gases try to escape.
As we heat these in solution depending on what we have in solution, and the concentration, the boiling point of the solution changes, it also changes as the the solution concentration of the acids in solution change.
At the bottom of the vessel where the solution in direct contact with the hot plate we can have a heat higher than the boiling point of the acid, causing it to decompose and leave the solution rather violently as it rises through the solution as a gas, popping out of solution carrying metals with it. boiling is gases decomposed from acids at the bottom, (evaporation is from the surface).
Evaporation can happen at temperature way below the boiling point.
Water boils at 100 degree C, but we can evaporate water at room temperature.
Evaporation does not create bubbles large or small, it will not carry metals or salts from solution, it happens calmly and quietly at the surface of a liquid.
The bubbles do not always need to be like the very large bubbles we think of as boiling like when we get water moving in a rolling boil and where we see many very large bubbles of gases rising to the surface, we can heat the acid to a light boil and have many very tiny bubbles rising and popping and carrying metals with these many very tiny bubbles as they pop and spit up metals and acids solutions, as the gases try to escape.
Thanks Richard I appreciate the explanation! There were no bubbles at all. I understand what you are saying though, so it seems that the solution can get to hot and carry values away without actually bubbling/boiling.
Tyler
Tyler
There is a possibility that when the condensate drips back into the solution small droplets splashes around.
Göran
Göran
g_axelsson said:
This is a very good possibility!
Tyler
