PLS HELP, MY POWDER ISN'T TESTING POSITIVE

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HELLO,
I HAVE USED THE A REGIA METHOD FROM SHOR A COUPLE TIMES. THE FIRST TIME IT CAME OUT PERFECT AND THIS TIME I GOT 18 GRAMS OF POWDER THAT ISN'T TESTING POSITIVE FOR GOLD AND I DONT UNDERSTAND WHAT IT COULD BE. HAS ANYONE EVER RAN INTO THIS BEFORE OR HAVE ANY INSIGHT AS TO WHAT THIS COULD BE, WHAT I COULD HAVE DONE WRONG, OR WHAT I CAN DO TO FIX IT! I HAVE WORKED REALLY HARD AND AM SO FRUSTRATED :cry:
 
OK first things first.......relax!Calm down and take a breath.

Ok now,have you checked your stannous to make sure it is good?If not,then you need to test it.
If your stannous comes up good,then check your powder.Put it in a CLEAN beaker and add Hcl(muratic),you will need a container no smaller that 250ml and add at least 150 ml of muratic.Stir slowly but stir well for a couple of minutes.Then let it settle.This may take seconds if your powder is pure,or could take minutes or hours depending on how contaminated it is.The darker your acid is.....the more contaminated your powder was.
Go ahead and try those things first and then we will go from there.
Johnny
 
THANKS FOR YOUR RESPONSE...LET ME BE MORE SPECIFIC...MY LIQUID TESTED FINE AND THE PHYSICAL POWDER IS ACTUALLY FINE. WHEN I MELT IT DOWN IT LOOKS LIKE AN ORANGISH YELLOW BUT DOESNT TEST POSITIVE WITH MY TESTING ACIDS. I DID WHAT YOU SAID AND IT IS CLEARISH GREEN AND YOU CAN SEE ALL THE WAY THROUGH IT, NOT VERY DARK. ANY MORE INSIGHT?
 
Hey bud.Can you please turn your "caps lock" off?No offense but it looks like you are shouting...lol.
Ok if you put the powder in muratic and the acid turned green at all,that means your powder is dirty.However am I to assume that you have already melted the powder?If so,and it was dirty,that is why it is "orangish".When gold turns from molten state to a solid state,due to its very high density it pushes everything to the outside,that includes copper and any other impurities.That may explain why your test is now coming up negative.At this point I am recommending that you dissolve your gold in AR and repercipitate.Then you need to wash the powder again with clean muratic.I know it sounds like a lot of work,but if done correctly you should have no problems having it done by tonight.There is a great saying by us that have been processing for many years.."garbage in,garbage out." Always make sure your powder is of the highest purety before you melt.If you have any more questions or problems just let us know,thats what we are here for.
Johnny
 
Thanks, I have 15 grams of powder still, I just melted a little to make sure first since I am new at this. Thanks for all your help...I am in Orlando,Fl. I noticed your in Cocoa. I am really trying to get this right as I injured myself a few years ago and am unable to go back to my old labor. I really appreciate your help!
 
Getting pure gold (shining) (Acid Wash)

This process is used to do your final wash to remove any impurities (Trash) that you may have carried over from your precipitation. This is one of the most important things you will learn in gold refining. Learn it and live it.

There are NO shortcuts. If you want pure gold, you MUST follow accepted practice. Remember, those that went before us have gone through this time and again----and have perfected a process that will yield good quality------so if you're interested in achieving that level, follow instructions that are at your disposal. Don't experiment-----leave that for others with time on their hands that are content to re-invent the wheel. This is particularly important for you, considering you're trying to establish a refining service.

Depending on what you're starting with, you may have a hard time achieving a good level of purity the first time through. That's to be expected. Part of the problem is mechanical drag-down, where you're working with very heavily contaminated solutions, part of which follow the gold. They're not always easy to wash out, even when boiling with HCL.

My advice to you is this:

Process your gold the first time, using conventional means. Allow as little in the way of contaminations (metals) as is humanely possible, to be included with the gold. Use only clean vessels. Wash them well between operations-----and use BonAmi cleanser if necessary to remove stubborn stains. Do not use other cleansers, for they scratch the glass. Filter before precipitating, and insure that the filter does not allow particulate matter to pass. If it does, re-filter, or go to a better filter grade. A Whatman #2 does an outstanding job for first refined metals, although they are not cheap. I used them exclusively for filtering first run gold chloride. I felt they were worth the extra money. At all times, keep your beaker covered with a watch glass of appropriate size, to prevent contamination from other sources.

Precipitate your gold using conventional methods, collect it and wash it well. It's best to use a precipitant that does not add contamination. I preferred SO2, but there are others that work equally as well, I'm sure.

First wash should be in boiling HCL and tap water. Boil for a prolonged period of time. Take up the solution with tap water, decant after the gold has settled, then rinse with tap water, which should again be brought to a boil. After it has boiled for a period of time, add more tap water to cool the lot, then decant as before. Rinse again, and do it until the wash water comes off clear. Next, wash the gold with ammonium hydroxide and tap water. Heat it until it boils. You'll notice that the solution gets discolored. How much is determined by how dirty your gold was when you started. The ammonia evaporates fairly quickly, so you can't boil very long. Add tap water to cool, decant, and follow up with a tap water rinse, again, boiling the water. Add tap water to cool, then decant. You now repeat the HCL and tap water wash. You'll be amazed that suddenly more contaminants will come off. Boil well, add water to cool, decant, repeat the water rinse, decant, then, and this is important-------start the refining process all over again by dissolving the well washed gold powder in aqua regia. I'll talk about that in a minute, but these are indicators you should have observed along the way, aside from the fact that you could see contaminants being washed from your gold powder.

The gold powder, which started out quite dark, is now much lighter in color.

It may have been rather loose and flocculent, but now is eager to agglomerate, so it forms lumps and settles quickly.

While these instructions sound like a lot of wasted time, when you process what you think is pure gold, you'll see evidence in the remaining solutions that it was not. The evidence of which I speak will be in your solution when you've extracted the gold for a second time. It's a lot of work which is why I re-refined my gold in large lots, often as much as 200 ounces at each refining, so the time spent yielded a large return.




When you precipitate for a second time, one of the things that you can do to help eliminate unwanted elements is to use a different precipitant than the first time. I never bothered with that, but it's good advice if you're fighting with a given contaminant and can't get rid of it by other means. That was never a problem for me.

Wash the gold powder the second refining by the same methods and sequences as the first refining. Make sure all your equipment is scrupulously clean. Force dry the gold when it's washed by heating the beaker at a very low heat for a long period of time. Avoid allowing the beaker to achieve boiling temperature---you get minor steam explosions that blow gold out of the container. As the gold dries, it's a good idea to swish it around the beaker occasionally, which prevents the gold from bonding to the beaker. The residual matter in water tends to form around the gold and bond it to the beaker. While it's a contaminant of sorts, it does NOT alloy with your gold, so it is not a source of lowering the fineness unless you have strange elements in your water. For me, it was not a problem.

Once dry, you can then melt your gold. A clean, never used for anything but pure gold, dish can be used. It should be covered with a coating of borax, but nothing else. DO NOT USE ANY SODA ASH. If there are any oxides present, they'll be reduced and absorbed by the molten gold instead of locked in the flux.

Your torch should be cleaned of loose crud before melting your gold. Run fine abrasive cloth over it until it's very clean, then wipe it down with a damp cloth to remove any traces of dust. Think clean every inch of the operation-----otherwise you undo all the hard work you've done getting your gold pure.

Your other option is to operate a small gold cell, but you must have several ounces of pure gold for the electrolyte.. That is likely not a viable choice for you at this point in time.

Harold
 
ARMANDO HEVIA said:
THANKS FOR YOUR RESPONSE...LET ME BE MORE SPECIFIC...MY LIQUID TESTED FINE AND THE PHYSICAL POWDER IS ACTUALLY FINE. WHEN I MELT IT DOWN IT LOOKS LIKE AN ORANGISH YELLOW BUT DOESNT TEST POSITIVE WITH MY TESTING ACIDS. I DID WHAT YOU SAID AND IT IS CLEARISH GREEN AND YOU CAN SEE ALL THE WAY THROUGH IT, NOT VERY DARK. ANY MORE INSIGHT?


May I ask which test acid?

If it is the stannous chloride you test your solution with for dissolved gold it will not work on powder or solid gold. If it is the standard acid test solutions (10k through 22k) it won't affect melted gold above 22k.

So what test procedure and which acid did you use on what form of gold? Please be more specific.
 
Thank you so much for the information, I truly need it right now! Yes, I am learning that the filtration is everything!

QST42KNOW: Yes, I was using test acids as in 10kt,14kt,18kt etc... I am refining using the AR method but from the company shor international. I am considering using the basic acids for this in the future though since it is cheaper. They give you a powder called subzero which is a substitute for nitric and it costs $9.95 for a 1lb bag and $99.95 for a 10lb bag which is a little expensive but easier and safer. Is anyone familiar with this?
 
Yeah, that sounds good Johnny! I have a super crazy schedule right now but that would be great! I will email you shortly.

So this is the standard process...wow, I didn't know about all the rinsing and re-refining. I truly appreciate this help from everyone. I was planning on using a "t-shirt" filter method but with three shirts. I got this idea from someone else that does this and they get good quality results. Does anyone have any thoughts on this?

Where would I get a "Whatman #2" filter from?
I have over 7lbs of 24kt plated pins right now that I am about to do, how much acid should I use for this?

Thanks again!
 
I know your excited but it looks like you will be getting personalized help from Johnny. It would be best to wait for that help considering what you have said so far, instead of making yourself a mess with what you have.
 
I have another question: On the little "plates" on the back of the cpu's...can you do those in this type of batch or do you have to do a reverse electroplate process?

Yes, I know...looks like I got extremely lucky and hopefully Johnny and I can have some fun with this!
Thanks again everyone...I just learned of this website today from a friend and have learned SO much already!
 

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