# Is this the right track?



## Barren Realms 007 (May 30, 2009)

I have processed about 2 Lbs. of fingers and have the foils from that, they were processed in HCL/Peroxide and came out real good.

I have about a 1/2 Gal. bag or CPU's and packs broken apart to expose the foils. 
These were soaked in HCL for 24 Hrs. and the renside 4-5 times with tap water. Using filters or course.
Then they were soaked again in new HCL and washed with water again. 
They were then processed in HCL/peroxide for a 36 Hr period. The pins from the fibers fell off, the ceramic ones were not visably effected. And most of the visable gold on the packs were removed.
This was all washed and soaked again in HCL/Peroxide again for a 36 hr period ( each time this process was done about 1/3 of a cup of peroxide was added to an original 2 cup to 1 cup ratio.)
This batch was washed with water again as in the previous step.

The fiber boards and the packs were removed and set to the side.

A double hand full of ceramic CPU's have been setting in a mixture of HCL/CL for about 13 Hrs on a coffe pot hot plate.
Ratio of about 5 cups HCL/ 1 cup CL. About 1/3-1/2 cup of CL added twice about 6 hrs apart making a total of about 7 cups.
The mixture is a very dark color almost black when you look at it. You can see that it is yellow on the sedges looking at it from the top.
A staneous(SP) test shows an egshell blue.

Do I need to raise the temp to boil off the clorox? Or am I on the right track?

Am I using too much or too litle of this mix?

Do I possibly have other things in the mix. The color on the paper for the staniuos test was Yellow . About the same color as the camaro in the trasnformers movie.

I also see little circlsthe size of #2 pencil lead on the bottom of the coffee pot, What kind of metal might this be?

The CPU's are still showing the final parts of the pins lef and should be gone in 6-8 Hrs.

Unfotunately the pins from the fiber and the packs were added to the foils that had been previousely removed. 

This mix is currently in it 2 nd soak of HCL and am still getting a bubbling action from the copper coming off of the pins. I figure 2 more soaks and washes and they might be clean.

Should I wash this in Nitric before I attemp to melt this mix?

Should I add the flakes and pins mix to the HCL/CL and then drop all?


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## lazersteve (May 30, 2009)

007 said:


> Should I wash this in Nitric before I attempt to melt this mix?



Yes. After the nitric bath I would dissolve the lot in HCl-Cl or AR.



007 said:


> Should I add the flakes and pins mix to the HCL/CL and then drop all?



No. 

The dark color acid is a sign of one of two things :

1. Copper Chloride saturation 

or 

2. Iron Chloride.

The yellow test paper leads me to believe you have more of #2 than of #1.

The black circles are what GSP has called manganese oxide (?). It's used as a primer to get the gold to stick to the ceramic. Here's a photo of some I have laying around:







The ceramic CPUs are notoriously difficult due to the iron content in the legs.

Once the gold powder is precipitated and properly washed then combine and dissolve both lots in AR a second time.

I prefer to use the modified Poor Man's AR on them after the lids are removed.

Steve


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## Barren Realms 007 (May 31, 2009)

Thanks Steve, 

The pins and flake are almost free of the copper now, very little action in the container and it is a slight green color to the liquid. One more wash and soak and they should be ready to put in nitric for a soak and then put in HCL/CL.

Once I drop the gold in the CPU's in HCL/CL with SMB and then remove the copper that is in solution by electro. Would it be safe to run the gold back in the same HCL/CL or should I be safe and make a new batch?


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## lazersteve (May 31, 2009)

Make a new batch.

Steve


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## Barren Realms 007 (May 31, 2009)

Excellent thanks for your help and forthought.


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## Barren Realms 007 (Jun 2, 2009)

Ok here is what I've got now.

I took the pins from the CPU's tha didn't disolve in the HCL/Clorox and added them to the finger flakes that I had. I did this because there was still a green tint to my HCL I had been trying to clean the foild with after a 4th soak and a rinse.

I had washed them downlast night and had tried to add some HCL to my water hoping the flakes would settle so I could wash in HCL again. And yes I did add a couple of drops of dawn to break the surface tension. The flakes would not settle so I put this on the hot plate to boil off so that I could resoak. Well I fell asleep and awaoke to all my flakes on the side of the jar because of the bubbling action and a black burnt mess on the bottom of the jar. I said OOOOOOOOOHHHHHHHHHHHHH SSSSSSSSSSSSSSS!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!....

Well I added some HCL to get things back back in solution and get back to removing the copper I thought might still be in there. I boiled this for about 2 hrs and filtered the solution and washed it with water. Still had a green tint so I figured I would wash again in HCL but this time I put 4 ccups HCL and added 2 cups Peroxide to speed up the removal or the copper. 

Well things started foaming as would be expected bright yellow. I had the solution on boil. When I looked the gold went into solution, there was still some undisolved gold so I added another 1/2 cup of peroxide and let the fluid boil and all gold fell into solution.

This picture is the solution after I filtered it.


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## Barren Realms 007 (Jun 2, 2009)

These 2 picks are of the test for gold.


View attachment 1


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## Barren Realms 007 (Jun 2, 2009)

These 2 pictures are of the HCL/Clorox solution that the CPU's had been soaked in. The gold still needs to be dropped out of the solution.

View attachment 1


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## Barren Realms 007 (Jun 2, 2009)

Question I thought that gold was not supposed to go into solution when just HCL/Peroxide was used?

It is possible I got a trace of Clorox some place but I had just washed the gold with water 3 times and had let the water boil off.


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## lazersteve (Jun 3, 2009)

007,

Check out the chart in this post:

Dissolving Gold

from the chart you can see that AP will dissolve gold, albeit very slowly. 

The foils went into solution easily due to the fact that they are thin and have a large surface area.

Steve


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## Barren Realms 007 (Jun 3, 2009)

I kind of understand the chart, it's only been almost 30 years since 
I had science class.

Well it wasn't very slow when it happened, took maybe 30-45 seconds.

Any way I have some MSB coming so I can drop the old out. 

Once I drop it out Would your advice be to melt it and then run thru some nitric and the rerun it thru AP?

Thanks for your help.


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## lazersteve (Jun 3, 2009)

The speed I was referring to as 'slow' is in respect to AR and HCl-Cl as can be seen from the dissolution rates on the chart. Thin foils will pretty much dissolve quickly with any of the mixes on the chart.

After precipitating the gold it should be properly washed and redissolved in AR to further refine.

Steve


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## Barren Realms 007 (Jun 3, 2009)

That is my next step, I should be getting my SMB in within the next few days.

I ordered some crucibles and stir rods from you yesterday. Waiting for them to come in as well.

Also picked up some 35% Hydrogen peroxide today. Cheaper than the Qt. bottles at Wal Mart. Gotta save that extra penny. It does a good job to. I like adding the less volume to my mixes.

Thanks for the help.


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## Barren Realms 007 (Jun 7, 2009)

Quick question, 

When making Nitric Acid can you keep remaking the formula with the undisolved Sodium nitrate until it is all disolved in the acid?

Or is there a point when the acid produced is not as strong as with the original Sodium nitrate used.

And do you need to keep it at 150F when it is going thru the whole process or just in the begining of the process for a little while?


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## Barren Realms 007 (Jun 8, 2009)

Steve thanks for the order of the dishes and the stir sticks. Everything came in fine.


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## nicknitro (Jun 9, 2009)

BarrenRealms,

The undissolved sodium nitrate you speak of may be something else. I assume you are using Sulphuric acid and sodium nitrate to make poorman's nitric acid. If so, there is a salt precipitated from the reaction that I have been told is similar to Sodium Meta-Bisulfite (SMB). It is not the same thing, I just can't remember the correct name for it. I doubt it would be good for further nitric acid reaction, however I was also told by the same person that it could be used for gold precipitation from AR solutions. However I never tried it, as I had already purchased plenty of SMB. 

Hope this Helps,

Nick


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## Barren Realms 007 (Jun 9, 2009)

Thanks Nick, That is some helpful info. I will have to do some checking on that.

I keep the heat on last nights run and got a lot more of the Sodium Nitrate to go into solution. I kept the heat at around 170f-190F and only had about 1/3 Sodium Nitrate left over this time compared to last batch.


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## Barren Realms 007 (Jun 23, 2009)

I guess I didn't answer your question correctly Nick. Yes I was using sulfuric acid diluted from the store and sodium nitrate. On my new batch I boiled down the sulfuric working on it tonight. I used that previous batch to work on some items it did a good job. But I'm having problems with a class ring. Can't get it to do a whole lot. going to put it in the new batch of nitric when it is done.

I tried to reclaim that previous batch of nitric and here are some picks on it. The battery charger I used on it was an old Dayton 6-8v or 12v with a low/high/boost for both voltage settings. Not much of an adjustment range.

View attachment 4


I had a saturated solution that I tried to remove the copper from. I got a great reaction from the charger and used some metal from some drives I had torn apart. I would recomend using angle iron tho it does a better job IMHO.

View attachment 3


I ended up with a greenish color probably still has some copper in it. It will not react with much. And it won't do anything to a piece of copper tubing. I guess I had my volage up to high and didn't take my time with it.

View attachment 2



After it sat for a few days it produced a clump of crystals. Any idea what this might be?

View attachment 1


I ended up with this in the bottom of my mix when all was said a done. I could see the gold flakes floating around when I was boiling with HCL, and this was after washing with HCL 4-5 times and I still got dirty mix.. My next step with this is to wash in nitirc to see if I can do anything with it. I had tried in HCL/CL and didn't get it to go into solution. I think I put too much clorox in it. I think part of it might be silver I can see silver when it selttles to the bottom now.



Any help on these items would be appreciated. Thanks in advance.


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## nicknitro (Jun 24, 2009)

Hello Barren,

Been a while.  

As far as your questions. I'm probably not the one to ask for a lot of them. 

Problems with your class ring? If you still can't get it to react very much in Nitric, it is most likely a high karat of gold. For nitric to be effective on karated gold, the item would usually be inquarted, or melted with usually silver. Leaving it in an end result of 25% gold, 75% silver. Then your nitric would attack the mass more efficiently. The reason being is that gold above 6K I believe tends to shield the reaction of the nitric on the base metals.

Green crystals? Hmm, guessing dried copper nitrate crystals?

As far as recycleing your nitric. I know there are other topics on the subject. I was under the impression that the nitric ions are depleted as NO2, and NO fumes. You can try to filter the fumes with water to catch them, forming very weak acid. It's is more of a way to scrub the fumes from the air for recycleing though.

As far as your powder, it does look to be a mix of maybe some gold, and silver? This was from some nitric? What was the material you were refining?


Hope you get the answers you need,
Nick


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## Barren Realms 007 (Jun 24, 2009)

I used it on some stuff that AP wouldn't touch. Ceramic CPU's,a couple of watches,a couple of key chains, and some plated writing pins.


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## goldsilverpro (Jun 24, 2009)

> The reason being is that gold above 6K I believe tends to shield the reaction of the nitric on the base metals.


Actually, you can leach all the base metals from 10K using hot nitric. I most always ran 10K class rings that way. When they were finished, they were brown and completely held their shape. You could still read the writing on them. When you punched them with a stirring rod, they collapsed into a pile of gold powder.


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## Barren Realms 007 (Jun 24, 2009)

Thanks GSP,

Then the brown color that the ring has taken is on the right track. I put it in a new batch of Nitric this morning that I had finished last night. I don't have it in hot nitric just outside temp that shold reach about 95 deg today. There is a silver cloud coming off the ring today so I guess it is working on it to some degree. Should I put it in hot nitric to speed it up or just let it set?


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## goldsilverpro (Jun 24, 2009)

I think you'll need to get it hot to completely penetrate the ring. I would use fairy strong nitric, maybe 60 - 70% by volume. I have never used homemade nitric on this. It may not work well. You can tell when it's finished by probing it with a glass rod. If is still feels solid, it is not finished. When it's finished, it will be mush.

If I had read the entire thread and found that you were using homemade nitric, I may not have made these suggestions. With homemade nitric, I would think that heat would be especially important.


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## Barren Realms 007 (Jun 24, 2009)

It has been having some sort of reaction, the nitric is milky looking in color this afternoon. I will see if I can get a picture of it up later tonight.


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## nicknitro (Jun 25, 2009)

Barren Realms,

Another Side note. When you speak of AP not touching it, AP relies on a build-up of copper chloride to etch the gold off of what ever object you are refining. Certain factors in base metal effect that statement such as, does the object have any copper in it? At any rate Nitric and AP are two different animals used for specific functions in refining. 

I would guess at best "your" homemade nitric like the kind I made before is likely less than 30%, so GSP aka Chris is very wise to advise heat. Just watch out for the fumes, they are very hazardous at best deadly at worst. I just figured an inquartation would help remedy this situation. If the rings weighed 2-3 grams, you could melt them with 4-5 grams of copper/silver then redissolve in standard nitric leaving the same brown powder. Then if silver was used cementing it back out with copper material. Still though heat would probably be advised so I guess I'm just adding a step. LOL

Homemade Nitric can be expensive, so I hope you have enough material to overcome the startup costs of the chemicals involved .
At any rate read up on the processes, it will help you out in the long run. GSP, Steve, Harold and others are your best friends in these situations.

Chris,

At what karat is inquartation recommended for refining karat jewelry 10K +, I thought I remembered Steve posting a topic about 6K which equals 25%. The 10K method produces a sponge of gold right? No? Is that why you say to break it up with stir rod?


Thanks all and Good Luck,
Nick


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## goldsilverpro (Jun 25, 2009)

> At what karat is inquartation recommended for refining karat jewelry 10K +, I thought I remembered Steve posting a topic about 6K which equals 25%. The 10K method produces a sponge of gold right? No? Is that why you say to break it up with stir rod?



I may have painted myself into a corner on this subject. 

The 2 fire assay books I have both say to use a silver/gold ratio of between 2 to 1 (8K) and 3 to 1 (6K). They say that below 2 to 1, some silver will be retained with the gold. In fire assaying, this is very important since any silver retained would be reported as gold. In my case (plumb 10K is only a 1.7/1 ratio), it didn't make any difference.

When I ran karat gold, I rarely inquarted or, even, shotted. When I had a mixture of various karat jewelry, I first leached in hot strong nitric. I poured this off and then used hot aqua regia. The first nitric, in most every case, ate through all the 10K, leaving only brown powder. According to the assay books, I most likely had traces of silver left in the gold powder. I didn't care about this. 

When I used aqua regia on what was left, usually a small percentage (probably a couple of percent) of the 14K, 18K, etc. was not totally dissolved because of a high silver content - it wasn't much unless there was green gold present. I accumulated this and, when I had a bunch of it, I inquarted it. Unlike Harold's situation, I didn't have to get 100% the first time. I might mention that most refiners use AR directly on the jewelry, without inquarting, although some may shot it first.

I recommend that you do not follow my procedure. I recommend that you inquart all karat gold to 6K, with silver, before processing. You then should have no problems and everything will come out automatically. A long time ago, I finally realized that for you guys, the inquartation method, as spelled out by Harold, is far better.


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## Oz (Jun 25, 2009)

goldsilverpro said:


> > I recommend that you inquart all karat gold to 6K, with silver, before processing.



Unless I am missing something would not 8K be advisable giving 1/3rd gold and the balance predominantly copper and silver? 6K works fine of course but leaves you with a powder instead of sponge and it is a little easier to have process losses the finer the powder is. 

With that thought in mind it is best to do all processes in the same beaker as has been recommended here before. Every transfer of material to a new container is an opportunity for loss. Given the small quantities many here process this becomes more important as to how great a percentage this loss is compared to total starting mass.

Laser Steve recommended something I have not heard for a while that is very good at scavenging losses. After removing PM powders from a beaker always wipe the beaker clean with coffee filter paper until you see no residue on a new piece of paper. It is not much, but just ask Harold how much of a savings plan used filters turned out to be for him.


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## goldsilverpro (Jun 25, 2009)

Oz said:


> Unless I am missing something would not 8K be advisable giving 1/3rd gold and the balance predominantly copper and silver? 6K works fine of course but leaves you with a powder instead of sponge and it is a little easier to have process losses the finer the powder is.


If you are inquarting, I would still recommend 3/1, Ag/Au or 6K. When fire assaying, the Ag and Au are combined in a cupel and they form a perfectly homogeneous alloy. When torch melting, this homogeneity is more difficult to achieve, especially for a novice. In a furnace, it's a little easier because you can stir it well before shotting.

If you're making 8K, the homogeneity must be nearly perfect in order to leach out all the silver. If not, you will have gold-rich areas that won't part. Also, these areas will not dissolve in aqua regia due to the high silver - been there, done that. If you reduce the gold to 6K, this will give you more lee-way in case the Au and Ag aren't blended perfectly.


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## Harold_V (Jun 25, 2009)

Oz said:


> goldsilverpro said:
> 
> 
> > > I recommend that you inquart all karat gold to 6K, with silver, before processing.
> ...


No. It isn't better. If you alloy to greater than 30%, many of the problems of running without alteration are present, more or less defeating the purpose in inquartation. Understand, I'm not saying it doesn't work--it's just that you have the same problems, especially if you inquart with silver. Copper would be far different, because it dissolves in AR, unlike silver. 



> 6K works fine of course but leaves you with a powder instead of sponge


Not true. If you inquart correctly, it does NOT turn to powder without help. It does that when you go below 25% gold, or if you stir. I had a strict policy about dissolving the base metals and silver after inquartation. NO STIRRING. It isn't necessary, not if you heat the solutions, and I did. Always. Follow the guidelines set forth by Hoke and you can't go wrong. 

Harold


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## Oz (Jun 25, 2009)

Some of the difference I may have encountered as to the sponge breaking apart may have been due to my calculations on how much silver to add was based on hallmarking. When in doubt I would think that too much added silver is better than too little. Using 1 beaker throughout the process and careful practice results in little loss even if your sponge breaks apart. It sure beats silver trapped in your sponge!


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## Barren Realms 007 (Jun 25, 2009)

Here are 3 pictures of the class ring last night.

View attachment 3


View attachment 2


View attachment 1


I put it on a hot plate this afternoon and am getting more action. The nitric has also started turning green.


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## Barren Realms 007 (Jun 28, 2009)

Here is an update on what is happening with the class ring. need some guidence on this please.

You can see the ring in the bottom of the jar. I had dropped in what was left of a couple of other pieces to go along with the ring. Apparently the copper has reacted with the Silver Nitrate and dropped the silver out of solution. There is no more reaction taking place. There is still part of the ring left.

View attachment 2


View attachment 1


In this pick the gold has settled to the bottom under the silver. What is my best recourse for this?
Do I remove the current Nitric and replace with new and redisolve the Silver?
Do I wash it melt it and redisolve in Nitric?


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## Barren Realms 007 (Nov 1, 2009)

This is a test message to see if I have the right settings for picture up load.


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## goldsilverpro (Nov 1, 2009)

Barren Realms,

When I used nitric on class rings, it required a lot of heat - just below boiling. By the looks of the vessel you're using (a jar), you're not going to be able to apply that much heat without it breaking. Use a beaker or a Pyrex coffee pot and place it in a Corning Ware dish to heat, in case of breakage. You really have to drive the reaction with heat, even with 60 or 70% nitric. I didn't stir and often, after everything was leached from the gold, you could still read the writing on the now brown ring. When I mashed it with a glass stir rod, it crumbled.

I still don't know whether you're using home made nitric or the real stuff. If home made, you may be wasting your time.


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## Barren Realms 007 (Nov 1, 2009)

Thanks GSP. I was using home made nitric on the ring. I was able to get it to disolve after adding some heat to it. And yes those jars will crack! I have found if you raise the heat slowly they will work, althought it is a risky thing to do. I have had them crack but have not had them bust and loose my material. However I am not using them for use on the hot plate any more. I'm using glass coffee pots.

I do have a question for you tho. Will it mess up my solution if I use Sulfuric to drop any lead if I am using HCL/clorox? From what I am gathering it will not harm anything.


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## goldsilverpro (Nov 1, 2009)

> I do have a question for you tho. Will it mess up my solution if I use Sulfuric to drop any lead if I am using HCL/clorox? From what I am gathering it will not harm anything.



I don't think it will hurt but, since I have never used HCl/Cl, you'd better ask Steve.


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## Barren Realms 007 (Nov 1, 2009)

Ok thanks GSP. I have asked this question on about 3-4 threads but haven't gotten an answer yet.


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## Oz (Nov 1, 2009)

Barren,

I use HCl/Cl2 regularly and add sulfuric to clean the solution of lead before precipitating my gold.

It should be noted that free chlorine will interfere with SMB precipitation. For this reason I always give my chloride solutions a boil to remove the free chlorine first. It is at this point I add sulfuric. I of course decant before moving on to gold precipitation. 

I do not know what may result if you add sulfuric with free chlorine present.


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## Barren Realms 007 (Nov 1, 2009)

Thank you very much for that info Oz, that was what I was wanting to know. I was assuming this but didn't take into account the free chlorine.


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## butcher (Nov 1, 2009)

I believe that a small amount,of H2SO4 sulfuric, would only mix with the chlorine, as free SO4 ions, and if the had lead ions to attach to, they would and precipitate them, not free anymore, too much sulfuric and it will start to displace the chlorine, pushing chlorine gas from your solution, especially if strong heat involved, or highly concentrated solutions, the other thing to think about is any precipitants would be suspect of sulfides, which may need roasted.

in evaporating a solution with sulfuric and hydrochloric, the chlorine not only has a lower boiling point, but also is less likely to keep hold of the positive ion of metal, so the chlorine will evaporate from the solution easily, sulfates will stick around even till dry. and even then you must get them up to over 600 degrees to drive them off from metal salts ,

I believe small amounts H2SO4 should be no problem and can be benificial when lead is concerned.


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