# Familiarization, Karat Gold and Stannous Chloride



## Phishin_ca (May 2, 2016)

First Post! I have been a member for a while, but I feel that I am at the point where I can post a question or two. Before I do, I want to assure everyone that I am not going to jump into a process without fully understanding the results (including what can go wrong). From my readings of "The Helping Friendly Book" and many posts on this board, I feel that my first acquaintance tests will involve; 

1. Creating stannous chloride. http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=52&t=22011 (Thanks kadriver!). My understanding from reading other threads is if I keep a bit of Sn in the bottom of the container, I can just replenish with HCL as needed to fill the bottle. Am I correct that the ratio of Sn:HCL is not as important as ensuring that the solution can no longer absorb more tin? 

2. Creating a known good test solution of gold. The best source for this is a button or karat gold. This is where I feel I need to really slow down, even though I never really got up to speed. I believe there are several methods to get this solution. Karat gold, flattened, in AR or NaNO3 in HCL with heat. Is it possible to dissolve higher karat gold in HCL+Cl? I think the additional metals would grind it to a halt. As evidenced by many threads I have seen on this board, I could just dump a lot of H2O2 and HCL on some fingers and get a positive test but who wants dirty standards?

I really want to take this first step and sit back for a while (maybe even repeat it a time or two) so I don't become a statistic. 

I also wanted to say Thank You to Dave (FrugalRefiner) for a warm welcome (even though it was private). 

And to Harold... With all the research that I have done over the past year, I think that your demeanor and class with handling this forum is wonderful. While it may seem heavy handed to some, I understand that we are not talking about making bracelets from bubble gum wrappers. I really appreciate the fact that there is not a lot of drama here. 

Too Long? Didn't Read?
1. Is it OK to keep feeding Sn to HCL until there is no reaction to make my stannous chloride test solution?
2. Can I use HCL+Cl to dissolve 18k gold for my standard, or do I have to use AR?

I would really like to talk about the how and why, more than just receiving a referral to another resource (search or document). Sorry if it seams basic to those of you who have done this in the past. I just want to learn everything I can. I think this kind of dialog facilitates that. 

Shawn


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## Phishin_ca (May 2, 2016)

Edited, unnecessary.


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## butcher (May 3, 2016)

Phishin_ca,

If you are just doing acquaintance tests, you can dissolve gold foils in HCl and H2O2, or HCl and bleach.
it does not take much to get acquainted with the reactions, small test tubes can be used.

After you get acquainted, if you wish to make a standard test solution it is a bit more detailed.
Keep reading Hoke's book everything you need is there. She also has a good book on testing I suggest reading it also.

Read up on stannous chloride. Stannous can go bad. if you keep a piece of metallic tin and (make sure to keep it acidic) and air tight it will last a little longer (do not dilute), all the information is here you just need to study it.


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## upcyclist (May 3, 2016)

A couple of other points on stannous chloride and testing:

- Your gold control solution does not have to be very concentrated. You can experiment with this when you make your control solution. If it's dark yellow, it's stronger than you need.

- Test your stannous with the control solution every couple of days (or every day if you want) to be sure it's still good. If it's not, you might be throwing out your gold!


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## FrugalRefiner (May 3, 2016)

upcyclist said:


> Test your stannous with the control solution every couple of days (or every day if you want) to be sure it's still good. If it's not, you might be throwing out your gold!


I've never felt the need to test stannous unless it gives a negative test. If I use it, and it gives a positive result, I know it's working. If I use it and it gives a negative result, then I check it with standard gold solution to make sure the negative is an accurate result, and not an indicator that my stannous has gone bad. 

No need to waste gold solution unless I have to. It's my frugal approach.

Dave


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## upcyclist (May 3, 2016)

FrugalRefiner said:


> upcyclist said:
> 
> 
> > Test your stannous with the control solution every couple of days (or every day if you want) to be sure it's still good. If it's not, you might be throwing out your gold!
> ...


True--an excellent qualification. 

Beginners like me, who don't know what to expect, may test more often then--because I'm essentially using the stannous to reinforce my learning. "I should not have any gold in solution at this point. Yup, test is negative. Am I sure the stannous still works?" I occasionally check the pH and visually check for solid tin in my dropper bottle instead of testing with known gold solution.


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## Phishin_ca (May 7, 2016)

Thanks everyone for the responses! I think that from Butcher's suggestion of using gold foils to create the control solution, I will process a small batch, 10-20g of fingers to recover foils and then use the HCL and bleach solution in a test tube. I may try this next weekend. I still want to read some more first. 

Thanks Again,
Shawn


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## Phishin_ca (May 7, 2016)

upcyclist said:


> FrugalRefiner said:
> 
> 
> > upcyclist said:
> ...



This is where I think I would see myself for the near future


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## Phishin_ca (May 26, 2016)

I wanted to post a followup. I forgot to take pictures of the stannous chloride testing. I was able to take the foils recovered from some RAM fingers and produce a gold bearing solution. 



Obviously, I was excited to see it work as expected. Why wouldn't it? After I filled my 10ml dropper bottle with Auric Chloride, I figured I might as well take it to the next step.




So now I have some powder that I know I need to wash. That will probably take me another week (I like to take it slow). I know it isn't much, but I couldn't be happier! 

So I now have these separate containers of waste. I want to fully manage this small quantity by walking through the stock pot process. I am sure any recovery would be immeasurable, but I just want to know that I am being responsible. 

Thank you all again for all of the information shared. I really does mean a lot to me, and I just wish I had something to contribute!

Shawn


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## Anonymous (May 26, 2016)

Shawn

That's looking good mate.

Jon


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## Phishin_ca (May 26, 2016)

spaceships said:


> Shawn
> 
> That's looking good mate.
> 
> Jon


That means a lot. Thanks!

Shawn


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## FrugalRefiner (May 26, 2016)

Phishin_ca said:


> I just wish I had something to contribute!


You just did.

Dave


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## Phishin_ca (May 26, 2016)

Straight into question mode... Is the discoloration of the powder caused by a different metal? I thought that everything higher than iron would cause a green(er) tint to my solution. Will I reduce the powder by that amount when I do the washing? 

I am thinking Steve's 2-brick furnace (with MAPP) is going to be my best bet to get something shiny in the end. Should I post an intermediate step to show that I have remove base metals before melting?

Sorry for too many questions at one time. 

Shawn


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## Anonymous (May 27, 2016)

Hi Shawn

Given the base material that you used, the most likely contamination is copper. Do you have HCl available to you in a good strength? 

Jon


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## Anonymous (May 27, 2016)

butcher said:


> Read up on stannous chloride. Stannous can go bad. if you keep a piece of metallic tin and (make sure to keep it acidic) and air tight it will last a little longer (do not dilute), all the information is here you just need to study it.



It lasts for months and months stored with a little common sense, let's not get into instilling fear into people here please.


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## FrugalRefiner (May 27, 2016)

spaceships said:


> butcher said:
> 
> 
> > Read up on stannous chloride. Stannous can go bad. if you keep a piece of metallic tin and (make sure to keep it acidic) and air tight it will last a little longer (do not dilute), all the information is here you just need to study it.
> ...


 :?: 

Stannous can go bad. You keep tin in it and air tight to make it last longer. How is butcher's post "instilling fear"?

Dave


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## Phishin_ca (May 27, 2016)

spaceships said:


> Hi Shawn
> 
> Given the base material that you used, the most likely contamination is copper. Do you have HCl available to you in a good strength?
> 
> Jon


I do. Hot washes are in order for Monday! So you are agreeing that the multicolored powder is indicating contamination?


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## Phishin_ca (May 27, 2016)

spaceships said:


> butcher said:
> 
> 
> > Read up on stannous chloride. Stannous can go bad. if you keep a piece of metallic tin and (make sure to keep it acidic) and air tight it will last a little longer (do not dilute), all the information is here you just need to study it.
> ...


Cool, airtight, and excess tin are what I am doing.


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## Phishin_ca (May 27, 2016)

FrugalRefiner said:


> spaceships said:
> 
> 
> > butcher said:
> ...


 Dave, it may be just the way he read it. I appreciate both sides (Experiment/Study). After seeing how quick I can get a result from a little tin and a little HCl, I may even make some fresh for every experiment for now. I have dated the vial, and I kind of want to see how the reaction changes as the solution ages. Four tests on a spot plate... One old, one new, on the control solution and my current project. 

Shawn


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## upcyclist (May 31, 2016)

Phishin_ca said:


> After seeing how quick I can get a result from a little tin and a little HCl, I may even make some fresh for every experiment for now. I have dated the vial, and I kind of want to see how the reaction changes as the solution ages. Four tests on a spot plate... One old, one new, on the control solution and my current project.


Shawn, that sounds like a great little experiment. As long as you don't mind using two drops of gold solution for every test, you can't lose. Keep us posted!


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## Phishin_ca (Jun 2, 2016)

So my hot plateplate finally arrived. I have reviewed so many threads on washing, I have turned plaid. There are quite a few that say hot water, cold HCl. Quite a few that say hot water, hot HCl. There are plenty that ignore the ammonium hydroxide step, but I see that it helps liberate base metals. Is there an explanation for this that I have not searched for properly? Is there something I should be looking for that I have not seen yet? I personally think that repetitive washes, hot or cold, serve to do nothing more than remove the base metals, and the order is mostly irrelevant. Can someone smack me down?

Even current posts on the subject provide no direct insight, and it leads me to say that Harold's method is where I should stay(proven). Can anyone provide reference to posts that would give me a different opinion? 

Sorry for multiple questions in one post. At the rate I go, this could be months of conversation. 
Shawn


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## FrugalRefiner (Jun 2, 2016)

Take a look at the procedure Lou posted in Gold has been refined and melted, now has orange hue.. It may help.

Dave


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## Phishin_ca (Jun 3, 2016)

FrugalRefiner said:


> Take a look at the procedure Lou posted in Gold has been refined and melted, now has orange hue.. It may help.
> 
> Dave


Thanks Dave, that is perfect. I had read the beginning of that thread, but I didn't go all the way to the end. It won't happen again.
Shawn


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## Phishin_ca (Jun 6, 2016)

2 simple questions. 
1. 5% weight/volume of HCl from 37% Muriatic acid = 2.7ml per 100ml water ?
2. I don't want to kill my vacuum pump just yet (compressor powered with lots of soft metal). Lou states that he uses vacuum to reduce the wait. Knowing that I am beyond patient, can I gravity filter or should I just break down and buy more stuff. Remember that I am just in the exploratory phase. 

A followup for upcyclist; Next batch of fingers comes out in a day or two. I plan on making a new batch of Stannous Chloride on Wednesday. I doubt I will see any difference, but if there is I will do it again and video it. 

I pick up my firebricks on Friday. I will still have to carve one out, so maybe early next week there will be a speck of something shiny. 

Shawn


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## upcyclist (Jun 7, 2016)

Phishin_ca said:


> 2. I don't want to kill my vacuum pump just yet (compressor powered with lots of soft metal). Lou states that he uses vacuum to reduce the wait. Knowing that I am beyond patient, can I gravity filter or should I just break down and buy more stuff. Remember that I am just in the exploratory phase.


When I decided to get with the program and use a Buchner fliter, I found a kit on Amazon that actually included the Buchner funnel, stopper, heavy-walled filtering flask, tubing, Whatman #1 filters, and a hand pump for $70. For my small scale, the hand pump is fine for now. When it finally succumbs to the acid fumes, I can decide then if I want to buy another one or buy an electric pump.


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## UncleBenBen (Jun 7, 2016)

Upcyclist, did you pay for that kit yet?

My wife ordered the same one for me. With expedited shipping it was supposed to arrive day before my birthday. Birthday came and went, no kit. A week later I finally got in touch with them and they hadn't even processed the order yet. I asked them to cancel the order and they agreed, apologized and refunded my debit card.

About two weeks later I ordered another kit that was about $20 more. It came the next week and I was happy. Seemed fairly well made, held good vacuum, worked fine.

A week later, the first kit shows up on the front porch. I guess they messed up again or felt guilty about messing up my birthday so they sent it for free! BUT, I'm so glad it all happened like it did. This one was a piece of junk. The glass barb for the vacuum line had an air leak where it attaches to the flask. The glaze on the inside of the funnel was about as smooth as 60 grit sandpaper (just bare porcelain in places). I tried it with my other flask and almost couldn't get the filter paper to seal. At least I got a spare hand pump out of it.

I hope I haven't scared you too much. I really hope they send you one made better than mine. They do save a lot of time.

Edit to add..pretty sure it's the same kit anyways. Same price and same company...


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## Phishin_ca (Jun 7, 2016)

The amazon kit for about $70 was the one I was looking at. I think I will look a more expensive one.


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## upcyclist (Jun 7, 2016)

That sounds like mine, at least the rough porcelain on the funnel itself. Everything else works fine with my kit, and the only thing I need to work on is getting that funnel nice and smooth. The #1 filters have their place, though I wouldn't use them to catch precipitated gold. 

Amazon is kind of a crap shoot in general, but at least it's better than fleabay. Once when I ordered some beakers, the "Fullfilled by Amazon" pickers apparently thought you could pack them loose in a box with just a layer of bubble wrap around them. I had to send back the pieces to get a refund, but at least they gave me a prepaid sticker for it. In general, I look for vendors that look like they're stateside, and established companies (like Houston Scientific, not some random drop shipper).


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## Phishin_ca (Jun 26, 2016)

Go figure. My update to this was one month on the dot. I varied from Lou's procedure a little. 
1. Twice in distilled water
2. One dilute HCl (5%w/v)
3. One normal strength
4. Twice more in distilled water. This seemed to help me get the gold to clump. 
After drying the powder, I melted. 

As a side note for upcylist, or anyone else who is interested. The batch of stannous chloride I started with is still giving positive results and compared to the fresh batches I have made, it seems that the reaction my have slowed slightly. Neither was instantaneous and it may have just been my desire to find a difference in milliseconds, but I am still confident using the bottle I made a month ago. 
End result from 210gm of fingers;






It may be tiny and imperfect, but it is mine and I am proud of it. I am going to run this same experiment on the same weight of fingers a few times and see how the results change. I don't know how to say thank you enough for teaching me how to do this. I will be donating shortly!
Shawn


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## Phishin_ca (Jun 26, 2016)

Close up, because I can;


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## FrugalRefiner (Jun 26, 2016)

Very nice! Heavy, isn't it?

Dave


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## Phishin_ca (Jun 26, 2016)

For as tiny as it is, absolutely! Just so you know, I would not have actually tried to refine it if you had not questioned my username. Thank you, specifically. I really do mean it. The bad part is that I cant stop playing with it.


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## FrugalRefiner (Jun 26, 2016)

You're going to scratch it up playing with it! It will ruin that shiny surface!

Oh, yeah, that's right, you know how to melt it back down again. 8) 

Dave


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## UncleBenBen (Jun 26, 2016)

Be proud, Phishin, be very proud!!

It's hard to beat that feeling of the first time! :mrgreen:


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## goldsilverpro (Jun 26, 2016)

Great color but it doesn't seem big enough. That figures only $25/pound for fingers.


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## Phishin_ca (Jun 27, 2016)

goldsilverpro said:


> Great color but it doesn't seem big enough. That figures only $25/pound for fingers.



I felt the same way, but I also ran them as tiny batches so my losses would be higher I think. I also saved 30ml of the solution as my standard solution. 
I was concerned with getting experience with the reactions on a micro scale before I wasted chemicals and materials. I still have to deal with the filters and waste, so I am sure I will find quite a bit more. 

Shawn


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## Phishin_ca (Jul 5, 2016)

Another update. The Stannous Chloride is dead. 
Following Dave's suggestion of using a standard solution only when you receive a false positive, I went a step further. It is pretty quick to make up a tiny bit directly on my spot plate. I noticed an extremely slow reaction to the test with my trusty bottle and I wondered if it was caused by excess oxidizer. A shaving of lead free solder on the plate followed by a couple drops of HCl and waiting (argh), gave me a fresh batch that turned black immediately. 

I am almost tempted to no longer keep any for testing and just make new in spot 12 everytime before I start work.


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## Barren Realms 007 (Jul 5, 2016)

Phishin_ca said:


> Another update. The Stannous Chloride is dead.
> Following Dave's suggestion of using a standard solution only when you receive a false positive, I went a step further. It is pretty quick to make up a tiny bit directly on my spot plate. I noticed an extremely slow reaction to the test with my trusty bottle and I wondered if it was caused by excess oxidizer. A shaving of lead free solder on the plate followed by a couple drops of HCl and waiting (argh), gave me a fresh batch that turned black immediately.
> 
> I am almost tempted to no longer keep any for testing and just make new in spot 12 everytime before I start work.



If you read and pay attention on how to store it you would not have this problem.


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## FrugalRefiner (Jul 5, 2016)

Phishin_ca said:


> The Stannous Chloride is dead.
> Following Dave's suggestion of using a standard solution only when you receive a false positive,


I'm not sure I ever suggested that. I have said that I don't test my stannous as long as it's giving a positive result. I don't need to because it's obviously still working. If it gives a negative result, then I'll test the stannous to make sure the negative is valid, and not the result of oxidized stannous.

Dave


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## 4metals (Jul 5, 2016)

The stannous test solution is easy enough to make, I always leave a little bit of undissolved tin in solution, it helps it keep longer and I keep it in small bottles without a lot of air in them. The only time I ever test my stannous is when I get a negative test on my first test of the day. Other than that, every time you use it is a test of the solution.


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## Phishin_ca (Jul 6, 2016)

FrugalRefiner said:


> Phishin_ca said:
> 
> 
> > The Stannous Chloride is dead.
> ...


You are correct. I misspoke. I meant to say false negative. I knew there should be a positive result but did not get one. Sorry about that.


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## Phishin_ca (Jul 6, 2016)

Barren Realms 007 said:


> Phishin_ca said:
> 
> 
> > Another update. The Stannous Chloride is dead.
> ...


The tin in the bottom of the vial was depleted.


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