# Meet Mr Patty



## stihl88 (Mar 9, 2011)

Heres my latest button weighing in at 48g. I love the fractured surface look, truly incredible surface finish.

> Anyone care to tell me if it is better to pickle Gold in 98% or or Diluted Sulfuric acid?


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## Barren Realms 007 (Mar 9, 2011)

That's nice looking. If you don't have flux on it I would leave it like it is. If it is just a couple of small pieces of flux you can possibly scrape them off.


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## stihl88 (Mar 9, 2011)

Thanks Barren, Ive already pickled it in 98% Sulfuric but a while back i seem to recall reading elsewhere on the forum that diluted (30%) is perhaps better?


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## philddreamer (Mar 9, 2011)

Next time you need to add a gold button to get rid of nitric from your AR, put it in & watch the "Inside look" of the button... :shock: 
All I had @ the time was a 3 oz ingot, & brother, was I surprised to what they really look like inside!

I read that a 10% sulphuric boil would do the job of getting rid of the glass, so that's what I've been using, & it works for me.

Beautiful slug! 8) 

Phil


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## stihl88 (Mar 11, 2011)

Ahhh... I remember your bar indeed! 

Every bar is individual and unique and yours stands out.

I find more and more now that i can get the Nitric levels in my AR batch pretty much spot on, having taken advice from the Pro's and i bought and read GSP's books i always start out with less Nitric in my AR batch and add it in increments until the gold has fully dissolved, no need for Urea or adding further Gold to neutralize the AR, instead i just dilute it and drop with SMB after it cools and i find I'm getting my target weights in Gold every time now.


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## philddreamer (Mar 11, 2011)

stihl88 wrote:
"Ahhh... I remember your bar indeed! 
Every bar is individual and unique and yours stands out."

Thanks, I take that as a compliment

Also wrote"
"I find more and more now that i can get the Nitric levels in my AR batch pretty much spot on, having taken advice from the Pro's and i bought and read GSP's books i always start out with less Nitric in my AR batch and add it in increments until the gold has fully dissolved, no need for Urea or adding further Gold to neutralize the AR, instead i just dilute it and drop with SMB after it cools and i find I'm getting my target weights in Gold every time now."

That is very true indeed!
But, when speed is a factor, I like Harold, like to add enough nitric to quickly digest & then add a gold button to get rid of any extra nitric that might still be present. I also learned from this, what the gold button looks "under its skin".

We've learned our lessons well! 8) 

Take care!

Phil


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## Oz (Mar 12, 2011)

philddreamer said:


> But, when speed is a factor, I like Harold, like to add enough nitric to quickly digest & then add a gold button to get rid of any extra nitric that might still be present.


Maybe I am missing something here but if you are digesting your gold and add extra nitric to digest it at a faster rate, and then you have to add “extra” gold in order to consume your surplus of nitric, how are you saving time let alone reagents? You still must wait until all reaction ceases on the surplus of gold that you have added to be sure all of the nitric was consumed before precipitating.

Adding gold buttons or coronets is only done when you overshoot with nitric use. Yes you must be sure you go far enough with nitric additions on accountable lots, but not by much. It still does not increase your speed of process. Whether it is your gold from your lot, or added gold to consume the excess nitric, the rate of digestion will be the same.


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## Frankk12 (Mar 12, 2011)

I refining a batch and the AR was green and the gold I got was very good
I don't know if it was 9999 but it looked very clean
I have been hearing about AR being the color of orange juice with gold in it.
How come my AR was green when the gold was in there
Thanks


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## 4metals (Mar 12, 2011)

The green color of the acid was from the base metals which were in the gold you refined. You can still get good gold from green acid. If you inquart with silver and part in nitric before placing the gold in aqua regia, the acid will be red to orange because there are few if any base metals.


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## Frankk12 (Mar 12, 2011)

Hi 4metals
Than my pure gold was not pure 
I worked on it and it was perfect
Maybe the color was a touch red
I dont have pictures but do you think it was 9995 without looking at it.


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## Barren Realms 007 (Mar 12, 2011)

Frankk12 said:


> Hi 4metals
> Than my pure gold was not pure
> I worked on it and it was perfect
> Maybe the color was a touch red
> I dont have pictures but do you think it was 9995 without looking at it.



Not if the solution was green in color.


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## 4metals (Mar 12, 2011)

The green solution does not prevent an aqua regia process from producing .9995 fine gold. you have to rinse well and the smaller the lot size, the more difficult it is to get clean gold when there are base metals in the acid. Rinsing is critical and for large production, vacuum filtration is a must. The liquid you are filtering from contains contaminating metals, if you don't rinse it all out, they contaminate your gold. 

That is why, for a small refining lot, inquartation is so important. It allows you to separate the base metals (and the silver) from the gold before you use the aqua regia. This results in less impurity from gravity filtration.

Harold has said this time and time again, he worked on small lots for his entire career, inquartation served him well. For small lot refining, you cannot improve on the inquartation pretreatment, JUST DO IT!!!!!!!!


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## HAuCl4 (Mar 13, 2011)

An extra benefit of inquartation is that the gold crumbs/mud that is left dissolves readily in HCL+clorox or HCL+sodium chlorate, elliminating the nitric acid gymnastics of AR.

Phil's digested bar is so pretty to look at, however, that the extra gymnastics are perfectly justified. I must get me one of those!.


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## lazersteve (Mar 13, 2011)

Here's oone I did some time ago:







Sorry for the blurry image.

Here's the bottom of the same button:







Steve


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## HAuCl4 (Mar 13, 2011)

One more thing guys: Everyone should learn how to assay their gold, and not go around trusting the first moron with an XRF and an opinion.

For example, it is almost impossible that Phil's bar to be so low purity at. 996. If it was inquarted properly and simply parted well in nitric, it should be 997-998 at least, and if it went through AR once, with the usual care I know you guys put in your efforts it should be 9994 minimum, and likely better.

I believe most of you guys are generally selling yourselves short and rely too much in what others are telling you about the purity of the gold that you work so hard to produce.

Not a criticism, but an observation. LEARN TO ASSAY!. Or at least have your product assayed properly just once and be surprised.


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## 4metals (Mar 13, 2011)

The problem with high purity buttons is a typical fire assay will not be able to discern the difference between .998 and .9999. And it takes a good assayer to even get .998. At those purities, the assay is determined by instrumentation and measuring the impurities and subtracting from 100%. 

Nobody is going to run an ICP on a 1 or 2 ounce button. It just costs too much to run. 

The best indicator is a pipe. A bar with a deep pipe and crystals showing in the center of it is as good as it gets.


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## golddie (Mar 13, 2011)

This is something I cant understand maybe someone can clarify it
Thanks



> The best indicator is a pipe. A bar with a deep pipe and crystals showing in the center of it is as good as it gets.


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## qst42know (Mar 13, 2011)

Golddie

The top two photos show a deep pipe. You can zoom in twice on these large photos. Left click and let it load then left click again right on the sink hole.


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## HAuCl4 (Mar 13, 2011)

4metals said:


> The problem with high purity buttons is a typical fire assay will not be able to discern the difference between .998 and .9999. And it takes a good assayer to even get .998. At those purities, the assay is determined by instrumentation and measuring the impurities and subtracting from 100%.
> 
> Nobody is going to run an ICP on a 1 or 2 ounce button. It just costs too much to run.
> 
> The best indicator is a pipe. A bar with a deep pipe and crystals showing in the center of it is as good as it gets.



I disagree completely 4metals and I may be wrong, but a medium skilled assayer with a 4 decimal balance using 1 gram samples routinely gets repeatability and accuracy within 2/10000 of ICP results, and within 3/100000 of ICP using a 5 decimal balance.

I haven't read or know of any assay books written establishing accuracy limits for assays using the currently even more precise balances.

(The above results using old procedures with double or triple assays, without proof corrections, and only the caveat that the assay should not spit, else it's discarded). IMO it's impossible that these are freak results.

I do not know much about ICP, and was using results produced by others using the machine.

I suspect that the ultimate accuracy of fire assay is even greater using a microgram or .1 of a microgram balance, but haven't researched the literature.

I can consistently tell between 9995 and 9999+ gold using a 4 decimal balance fire assay, and I'm not particularly skilled or experienced.


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## 4metals (Mar 13, 2011)

I used the number of .998 because that is the difference between an actual measured gravimetric assay and the silver retention of the sample which has to be attained by using assay proofs. A good assayer will generally get a correction factor of .9985 if all goes well. Proofs are run using .99999 fine proof gold. Proof gold sells at a premium but will cost about $25 for the gold for a fine gold assay, $50 for a 1 gram sample as you suggested. 

Sure a five place analytical balance or a micro-balance will help get the numbers closer. But they won't effect the silver retention so the .9985 ish factor will remain. My point is based on the fact that the majority of assayers out there today do not routinely run proof assays they use a correction factor developed from their assaying experience. As a result the difference between the uncorrected assay result and the corrected assay result is more of an assumption than a quantitatively measure certainty. 

Today, the accepted results are exclusively from instrumentation, the fire assayers are working in the realm of karat assays where a corrected fire assay is king. For very high purity gold the level of confidence drops. I suppose in a perfect world you could get believability to .999 with a fire assay, I would like to know how you can quantify .9995 from .9999. I'm always open to new tricks.

I don't expect our members would appreciate paying upwards of $100 for a corrected fire assay or $125 for an ICP result on top of the discount they are hit with for shipping in small quantities to begin with. 

I understand companies like ARA will pay 98% on beads with a pipe. For guys who call coffee pots a reactor, that's as good as it gets.


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## HAuCl4 (Mar 14, 2011)

Using 2.7 to 2.75 silver to gold ratio, retention never got to 1.5 per 1000.

I doubt I got paid 0.15% extra by the tightwads the gold was sold to.

When I ran proofs the retention was max of 2/10000 so...I stopped running them and wasting time and money, and allowed to be negotiated down by 3/10000. Only once went to umpire with a crooked client that wanted to stiff me far too deep and I chose to lose him and humiliate him, and did.

Maybe I was doing it all wrong, or maybe I was really anal while assaying.

P.S. With great nostalgia I now remember the details of my first fire assay, made on one of those small stamped credit suisse gold bars, and the expectation and nervousness I felt whilst waiting for the cupellation to end, etc. I kept telling myself: Soon we'll know, one way or the other. When the purity measured at exactly 1.0000 in the balance, I said loudly: We are in business!. Lol

Little I suspected the amount of crap that was coming down the line, naively assuming the business was more to do with technical proficiency than commercial acumen which I totally lacked and for which I have paid dearly not only in money terms, but more so in time wasted.

Sorry for the rant guys...LEARN TO ASSAY!. Lol.

P.S.2.: Just to be perfectly forthcoming, most of the gold we assayed and sold was 996-998 and rarely 999+. I do not understand how that would affect the outcome of the assays and/or of the assays on hallmarked 9999 gold used for proofs at the beginning, but maybe some gold was dissolving in the nitric parting, just enough to offset silver retention?. Just a guess, I really don't know. Maybe I just got lucky with the 2.75 ratio sweet spot.


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## HAuCl4 (Mar 14, 2011)

By the way, what is the generally accepted/de facto current bible for modern gravimetric assaying?. I think I could benefit from reading that.


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## 4metals (Mar 14, 2011)

That is a good question, I used some older text's when learning and have supplemented what I know with "hard knocks." From what have been told proofs run by the assay labs in the good gold deliverable houses also require the addition of copper to the proof alloy, from what I gather, copper effects the absorption of gold into the cupel (losses) and you have to simulate that as well for the "perfect correction" (if that isn't an oxymoron :lol: )

Over the years I have come to realize that when a refiner makes a mistake on a fire assay, it is usually a mistake on the low side, because of the losses that one has to correct for in an assay. Bottom line is he makes more money that way.


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## HAuCl4 (Mar 14, 2011)

There must be somewhere a "standard procedure" typed by the big companies on how to do all this stuff.

As an aside, if one generally uses the same process/procedures to refine producing a hopefully consistent product, then it follows logically that the fire assay of the output product is only a quality check and the results should be consistent as well, elliminating to some extent or completely the need for proofs. I mean if one produces 9995-9998 gold consistently doing XYZ, then the fire assay is just a check. No?.


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## 4metals (Mar 14, 2011)

You are absolutely correct, when processes are set up and done in bulk the fineness of the product is only checked occasionally as the process never changes. Of course when setting the process up testing is done to get it right. But remember, those guys don't post pictures of their out-turn in posts called "Meet Mr Patty" either. A good number of our members are working on a small scale either for hobby or for profit, and for them the pipe is the window to purity.


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## HAuCl4 (Mar 15, 2011)

Thanks 4metals and point taken on the "pipe" thing. 
My original comment was in the direction that I am fully convinced that the purity that most of the members here are consistently producing is much higher than they themselves acknowledge, and if they measured it at least once they would be surprised, ans that allowing someone else to tell them the purity using an xrf or other is not the best way, and that learning to assay is more than fully justified, even for purely intellectual satisfaction.

IMO there are many more people capable of refining even to 9999, than to MEASURE the quality of their own work.

I think the straw that broke the camel's back was that thread with the electrolityc cell ...where a buyer with a rigged XRF was determining purity of the gold produced to pay on...when the truth is that the gold was 9999 or maybe even 99999...

Our members should be prouder or their work!. That's all and I learned something too about assaying, even better!. Cheers.


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## Harold_V (Mar 16, 2011)

HAuCl4 said:


> I think the straw that broke the camel's back was that thread with the electrolityc cell ...where a buyer with a rigged XRF was determining purity of the gold produced to pay on...when the truth is that the gold was 9999 or maybe even 99999...
> 
> Our members should be prouder or their work!. That's all and I learned something too about assaying, even better!. Cheers.


While I'm all for encouraging readers to pursue excellence, the very notion that you suggest they can routinely produce gold of exceptional quality isn't in tune with reality. If that were the case, industry standard wouldn't be 9995, but 9999 or better. 

The harsh reality is that achieving a level of quality equal to, or better than, 9999 is not easy, and unlikely to occur in the home refinery. It takes almost nothing to lower the quality, even in melting----so I think it prudent to keep everyone in tune with reality---pursue excellence (if that be your choice), but do not be unhappy if all you can achieve is industry standard. After all, that has worked for industry for a long time with no complaints. 

Important signs of purity:
The melting dish, after melting, is absent of any color aside from a pink through purple haze in the flux cover.
Gold, while molten, is absent a film that emanates from the center of the molten mass and is absorbed by the flux at the edges
The resulting solidified gold has a serious pipe 
The surface of the gold is free of a frosted appearance, although it may display a coarse crystalline structure---but is shiny, without discoloration. 

Harold


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## HAuCl4 (Mar 16, 2011)

Harold_V said:


> HAuCl4 said:
> 
> 
> > I think the straw that broke the camel's back was that thread with the electrolityc cell ...where a buyer with a rigged XRF was determining purity of the gold produced to pay on...when the truth is that the gold was 9999 or maybe even 99999...
> ...



As soon as I'm finished, probably this year, I'll post my simple kitchen-made 99999+ (FIVE NINES!) gold recipe, which I must admit is 99.9% similar to your posted recipe/others recipes posted. The biggest problem I face is measuring fineness accurately, and I suspect that I may never overcome that without paying for an external ICP (of which results I can never be sure about). 8)

The best way to deliver 9999+ is to produce 99999+ at almost the same cost!. :shock:


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## Lou (Mar 16, 2011)

See ASTM for the standard gold bullion analysis. They make them for all the metals as far as I know and with varying equipment. Fire assay, even with proofs, hits its precision at about 4N. That's the upper end of the technique, and then it's difference by subtraction ICP-AES. Less mechanical losses with ICP.

HAuCl4, I posted a method for 6N gold in Techniques.
If one can achieve 3N5, one can achieve 4N. For the record, you're supposed to use low chloride nitric (ASTM specifies max allowable) for parting.


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## HAuCl4 (Mar 17, 2011)

Lou said:


> See ASTM for the standard gold bullion analysis. They make them for all the metals as far as I know and with varying equipment. Fire assay, even with proofs, hits its precision at about 4N. That's the upper end of the technique, and then it's difference by subtraction ICP-AES. Less mechanical losses with ICP.
> 
> HAuCl4, I posted a method for 6N gold in Techniques.
> If one can achieve 3N5, one can achieve 4N. For the record, you're supposed to use low chloride nitric (ASTM specifies max allowable) for parting.



Thanks for the references Lou. Everything points at gaining easy access and learning to operate an ICP machine, to assess the fineness at 99999+ hopefully. A little daunting and unrealistic for me at this point, I confess.


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## HAuCl4 (Mar 18, 2011)

This is what I could easily find. Is that it for fire assays and ICP Lou or there is more?. :?: 

http://www.astm.org/Standards/E1335.htm

http://www.astm.org/Standards/B562.htm


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## Lou (Mar 18, 2011)

I was mistaken. 

Maybe I was thinking of the AOAC. They should have methods too!


Lou


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