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The beauty of what @anarxi says is you will learn how simple the inquartation route is, and it is also very scale able.

That would require large furnace (i have 1kg furnace now)
A 1 kg furnace is rated for 1 kg of pure gold so the quantities suggested will not fit in the furnace even though it is one kilogram. Inquarting larger lots in an inexpensive gas furnace is an option and parting the alloy in 1 kg quantities will be a good way to start.
 
Your losses were probably because of Silver Chloride in aqua regia. Especially if you approach 10% Silver.

I think your best bet will be inquartation and double parting with nitric acid. That can get your purity in excess of .995 without dissolving the gold in aqua regia. And you will recover all of the Silver you need to add for the process plus all of the Silver in the alloy.

The benefit of nitric parting is it can be done in stainless steel so no glass breakage worries. We have had members here measuring gold refined this way by XRF and getting results of .999+ (specifically a refiner in Vietnam).

The volumes you are working with can be easily transferred by vacuum and the final rinses with Distilled Water can be easily lifted and poured.
Inquartation will require silver twice the amount of gold content to make it susceptible to reaction with Nitric acid. This will be more expensive apart from stocking Silver if inquartation is required every time. 10% Silver for aquaregia should not be much of a problem if you have a very good stirring system and provide some additional time for reaction in the dissolution stage. With aquaregia one easily achieves 999 purity whereas inquartation after multiple wash will end up gold with 998 purity if acceptable for the market which normally trades in 995 or 999 purity gold as standard.
 
Inquartation will require silver twice the amount of gold content to make it susceptible to reaction with Nitric acid. This will be more expensive apart from stocking Silver if inquartation is required every time. 10% Silver for aquaregia should not be much of a problem if you have a very good stirring system and provide some additional time for reaction in the dissolution stage. With aquaregia one easily achieves 999 purity whereas inquartation after multiple wash will end up gold with 998 purity if acceptable for the market which normally trades in 995 or 999 purity gold as standard.
The Silver are not consumed so that may be considered a temporary investment
It will be reclaimed and reused.

Edit for spelling.
 
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just split it into parts.
250 grams of gold (no matter how many karats) and 750 grams of silver.
make a batch.
return the silver, and repeat the process.
a little more fuss, but with a homemade setup it will be even more.
Besides, by processing small batches, you will lose less if an accident occurs.
The more the number of processes, the contrary, you will end up with more loss than a single process. The multiple processes to finish the same qty of gold will require more time if you adopt to batch process. Of course, it all depends on the capacity of the equipment you have for each stage of refining.
 
I am hinting at a lengthy processing time you need to recover silver from silver chloride and put it back for inquartation.
There are many ways to do that including cementing.
And I commented because the
way you worded it it seemed to me that the Silver was lost.
The amount of Silver is dependent on the karat of course, but also depends on the alloying elements in the Gold.
But there are ways to do it directly without quartering but that may be too costly with respect to equipment.
Inquarting is a well proven and effective method.
 
No, Sir, I did not mean Silver is lost. I said one has to create an inventory of Silver to process gold by inquartation process instead of Aquaregia. One may have a 2Kg capacity refinery set but has 5-10 Kg of gold for refining with 10% silver in it. You may inquart first two kg with Silver and recover silver to make the next 2 kg batches and so on...thus requiring higher silver inventory. But in any case, Silver is an investment that remains and grows over time in value if losses are not there during the recycling and recovery of inqurted Silver. Thank you Sir for your observation.
 
Inquartation will require silver twice the amount of gold content to make it susceptible to reaction with Nitric acid.
Proper inquartation would require three times the nitric soluble metals to one part of gold. The Silver is the preferred method because it will use over 3 times less nitric acid to accomplish the same thing.

10% Silver can be dealt with with aqua regia refining but with tumbling not mixing. The tumbling action mechanically removes any Silver Chloride encrustation but simple stirring, no matter how powerful the mixing, is not as effective. While tumbling does allow aqua regia to be more effective with Silver concentrations approaching 10% it still leaves the issue of dealing with the silver chlorides which can hold as much as 1% of your gold with the chlorides. And the reducing of Silver Chloride to Silver metal is a more time consuming task than cementation on copper. And you have yet to address any platinum group metals that will dissolve in the acid and need recovery.
I have gold and silver jewellery business. For me refining is a side hustle.
Aside from the fact that I never considered refining a hustle, the OP is gainfully employed as a jeweler. And a silver jeweler as well. This makes attaining any Silver easier because he likely deals in sterling scrap as well. But inquarting will greatly simplify the process and eliminate chasing down all of the "losses" to get complete recovery if he uses aqua regia.

If he were to process the biggest lot he mentioned, 2 kg, that would require 6 kg of Silver or sterling silver to make an 8 kg melt. A number 6 bilge crucible in an inexpensive gas furnace would handle that quickly in a single melt. Shotting the entire melt, the parting process can be done in 2 kg lots in beakers small enough to handle. Two kg of the shot would require about 6,600 ml of a 2 part distilled water 1 part (68%) nitric acid mixture. This can be done in a stainless steel 10 liter pot which is easy to handle and resists cracking (unlike glass). The second parting is done with stronger nitric acid 50% distilled water, 50% nitric (68%) acid. For the second parting the insolubles from the first parting need only be covered by a few CM of the acid before heating. This process will get you to 99.5%+ gold with the major impurities (typically the only impurities when refining karat scrap) are silver and copper. Small jewelers using this gold to return to product can easily figure out the new proportions to make quality karat alloys in the karat of their choice.

Without going into it here the cementing out of the Silver from the parting solution is quite easy and fast.

Transferring the hot acids after parting, if lifting and pouring into a filter is too intimidating, can be done by using a vacuum transfer jug to suck out smaller quantities of the acid and pour them through a filter. If you need more details on making a simple vacuum transfer jug just ask and I will give you more details.

If the OP needs 99.99 pure gold, an aqua regia refine at this point will produce the purity he needs with no worries of PGM losses or Silver Chloride to deal with. We have members using the parting as described here and their XRF reads 9999 before any aqua regia refining. I do not know if that is a result of an inexpensive XRF, or the parting process producing a good enough reading for the buyer using XRF to call it 99.99.
Industry standard is ICP analysis and gold purity by difference to determine purity. A technique often bypassed by smaller buyers. (Much to the advantage to folks like the OP)
 
I am hinting at a lengthy processing time you need to recover silver from silver chloride and put it back for inquartation.
Me too same

There seems to be some confusion here between Silver Chloride and cemented Silver as what @Anil said above. I learned a long time ago that whenever possible avoid creating Silver Chloride. With aqua regia and karat gold containing Silver there is no option, you will generate the Silver Chloride and you have to deal with it. And it typically traps gold in the chloride. With inquartation and nitric parting you do not have to create Silver Chloride to recover the Silver although it is one alternative. But cementation is easier and quicker and will also put any PGM's present into the cement where it can be recovered later in a small Silver cell. If you drop the Silver from parting in nitric using salt or Hydrochloric Acid you will leave any PGM's in the acid and then you need to chase them down.
 
More details please


Vacuum transfer jug.jpg
This is a simple effective way to transfer acid into smaller volumes that are easier to handle. You need a vacuum source. If it is a vacuum pump, you have to bubble the air that comes from the reaction through a bubble trap filled with a caustic liquid to protect the pump. Some guys cheap out and only add 1 short pipe. That is a mistake because the second stub of pipe allows much better control of the flow. There is no flow until vacuum builds when you place your finger over the end of the pipe and the second you remove your finger the flow stops.
 
I have learned over the years that typical black rubber stoppers used on the top of the flask get spongy in time with nitric acid. But you can get silicone stoppers on-line and they hold up better. Also, the 4 liter Erlenmeyer flasks use a #12 stopper size but some of the new 5 liter Ehrlenmeyer flasks use a #13 stopper.

These jugs can be used for any solution transfer and are particularly handy for transferring acid from drums into smaller bottles for ease of use.
 
View attachment 65927
This is a simple effective way to transfer acid into smaller volumes that are easier to handle. You need a vacuum source. If it is a vacuum pump, you have to bubble the air that comes from the reaction through a bubble trap filled with a caustic liquid to protect the pump. Some guys cheap out and only add 1 short pipe. That is a mistake because the second stub of pipe allows much better control of the flow. There is no flow until vacuum builds when you place your finger over the end of the pipe and the second you remove your finger the flow stops.
Thanks
 
Me too same

There seems to be some confusion here between Silver Chloride and cemented Silver as what @Anil said above. I learned a long time ago that whenever possible avoid creating Silver Chloride. With aqua regia and karat gold containing Silver there is no option, you will generate the Silver Chloride and you have to deal with it. And it typically traps gold in the chloride. With inquartation and nitric parting you do not have to create Silver Chloride to recover the Silver although it is one alternative. But cementation is easier and quicker and will also put any PGM's present into the cement where it can be recovered later in a small Silver cell. If you drop the Silver from parting in nitric using salt or Hydrochloric Acid you will leave any PGM's in the acid and then you need to chase them down.
I understand what you are saying. Here in my town and nearby cities gold refiners who test gold on xrf and exchange it for pure gold for a fee of 0.20% - 1%. They do it on medium to large scale and are profitable as they are in business since 4-5 years. Almost all use aqua regia method and machines available in market. Is there something we might be missing?

The silver chloride is soluble in ammonia hydroxide. Can it be seperated from gold using this?
 
I understand what you are saying. Here in my town and nearby cities gold refiners who test gold on xrf and exchange it for pure gold for a fee of 0.20% - 1%. They do it on medium to large scale and are profitable as they are in business since 4-5 years. Almost all use aqua regia method and machines available in market. Is there something we might be missing?

The silver chloride is soluble in ammonia hydroxide. Can it be seperated from gold using this?
Yes but it has its own drawbacks as it has to be acidified as fast as possible after.
If not, it may/will form explosive compounds.
 
Almost all use aqua regia method and machines available in market.
By this do you mean they refine gold using the commercial machines like you referenced above or machines from companies like Auro studio or Italimpianti? If that is the case they are not returning 9999 gold to you as none of those machines can produce 9999 gold in a single pass. (even though they claim to do so). you can refine to the purity they hit with their machines by inquartation and double parting if you do it properly.

It is quite possible they can produce gold that many XRF instruments would read as 9999 or 24 karat. But if that is true, so can you.

High purity gold cannot be determined by fire assay it can only be determined by difference using instrumentation. And an XRF result is not the instrumentation I am referring to.
 
The silver chloride is soluble in ammonia hydroxide. Can it be seperated from gold using this?
It can, but for one thing the ammonia boil fumes a lot and once you clean up the gold that didn't dissolve in the first place (by re refining in aqua regia) you have to get the silver out of the ammonia by acidifying with aqua regia. So you end up with Silver Chloride again, albeit without any gold mixed in.

Your primary feed stock can border on having too much Silver in the alloy for aqua regia to be effective which is why I suggested inquartation to begin with. If you were to buy a small tumbler plant that grinds off the encrusting Silver Chloride you may get by with aqua regia. This is a small tumbler plant.
C8C28F61-07F8-4045-9808-4FD955CF18B9.JPG
but keep in mind, after spending all of the money to get a plant like this you will not recover 9999 fine gold in a single pass and you will have Silver Chloride to deal with and all of the PGM's will remain in the acid for you to chase after.

Those are a lot of added steps for a side hustle! Keep it simple and you won't regret it!
 
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