ap precipitation?

[superten67]

well guys i did it after lots of reading and watching various videos on you tube etc ive done my first batch of ap.
was a bit in awe of the whole process but thought if i dont have ago at in the very least the ap process i never will.
so pins off,gold plated nuts and bolts and any of the other smaller bits i had in a glass jar,2 parts hcl and i part 9% peroxide the reaction was a good one straight away and there was an immidiate change in colour to the emerald green colour i was led to expect by the reading and videos.
but the solution soon darkened and was a dark cola colour.
i decided to double up on the ammount of ingredients so as to give everything a better chance to be submerged(it was allready mind) and therefore get cleaned a bit better.
again quite a good reaction efevescence,white fumes and then settled down and got on with itself.
but was still the dark cola colour which over the few days did get greener but not much still quite dark.
so today gave it a stir and checked the remnants of pins,nuts etc and every last scrap of gold was gone and all the metals were black and bare.
drained the solution through filters and as i did it cleared up a bit but then when it settled there was a slight white residue in the bottom of the jar,maybe a problem?
couldnt really tell it just looked that way,so then after looking and thinking lets precipitate.
so did just that put 2 teaspoons in at first and there was a reaction but not much slightly red coloured vapour if i remember right and then finished up having put nearly 3 teaspoons in.
now ive heard a lot of people say some gold will precipitate straight away.....so i waited and nothing happened.
i know it takes days but was expecting to see SOMETHING at least straight away.
have i done anything wrong?
any help greatly appriciaed cheers.

 

[qst42know]

If you over did it with AP, the solution is to cement with more metal. The black smut on the remaining metals is your gold. Don't let the appearance fool you.

Search the forum for stannous chloride you should always test your solution. Without it you are lost and will lose values.

 

[superten67]

ok i get that, what id been thinking is that maybe as the peroxide was 9% it had not just taken the gold off of the pins etc it had just dissolved it completely into solution....is this correct?
i was also am confused as to where the washing with hypochlorite bleach comes in?
ive watched that many videos of different processes of ap and ar and with the one im using at the moment the ap has quite a few variations and is easy to get sidetracked.
so i now could even start another batch and just include the solution in question in that batch?
and as to the peroxide percentage if im using 2 to 1 at 9% should i up the hcl to 3 parts as its stronger?
seems to me people only put a dribble of peroxide into their mixes just to start a reaction off?
whereas i used an exact ammount....when i poured the stuff together first off it was only green for a split second then went black.
but from what im now seeing is pour in your hcl and then just put your peroxide in in no measured ammount but just until you reach the the desired light to dark emerald green?
im going to have a look at it in the morning after putting the smb in tonight,because as i see it there has to be some gold in the solution that i have or else there would be no colour to it at all?
then if there isnt any gold precipitated out,what then?do i disguard the solution and redo the scraps that are caked in black sludge?
i know its irritating to people who allready know what to do but bare with me guys i am trying.
thanks again.

 

[Geo]

what you did was dissolve the gold foil with too much oxidizer. theres no gold in solution. there never was beyond the couple of seconds it took to dissolve it. as soon as the oxidizer was used, the gold cemented on any base metal left. you say you had black metal left. the black is your gold stuck to the base metal. put the left over metal in a glass container and add some water. swirl it hard until it turns the water dark. pour this into another glass container and let the black settle. decant the clear water down to powder. add a small amount of hcl to the powder and add a couple drops of bleach. test the solution with stannous chloride and see if you get a positive.

 

[qst42know]

With base metals remaining it would be difficult to have gold in solution. But test the liquid anyway.

Decant the liquid save all solids including the black dust add fresh HCL but no peroxide and aerate with a fish tank air pump. Repeat as many times as necessary until the solution will pull no more color. The remains contain your gold.

In between read up on the process it has been written about many times.

 

[superten67]

will do thanks again.

 

[superten67]

ok did what you said and i have my gold,just needs melting down.
just thought id add a note of caution for anyone using peroxide in any solution of 9% or higher(thats if you dont know all ready)might even apply to 6% i dont know i purchased 9% straight away as everyone said it would work quicker.
most of the proportions ive found on ar are 2:1 and one i think was 3:2 but for the 2:1 i know it for a fact that if you use 9% in this ratio it'll just burn the gold off and cement it back to the metal......then you will have to do the whole water swill,bleach wash and basically money and face save.
ive just put a fresh batch of chips on to cook and did the 2 parts hcl but did not even put half of the 200 ml bottle in and its the perfect emerald green we all hope for.
i followed the instructions exactly and still got the wrong results im just glad i never lost my gold.
so thanks to qst42know and geo for the help and advice.

 

[Geo]

what i told you to do was just a test to see where your gold was. theres still gold on the base metal even if all the black washed off. keep in mind, for a pound of metal, it will take a whole five gallons of solution to dissolve that much material. what i do is, i add the aerator hose with a bubble stone first. then i add the material on top of the hose as an anchor. for five gallons of fresh solution,add one and a half gallons of water, next add three gallons of muriatic acid slowly so it doesnt splash. add one quart of 3% peroxide from the market of your choice. the solution will turn some shade of yellow. dont worry, your gold is safe. the color shift is a chemical reaction between the hcl and H2O2 (if you add hcl and bleach together with no gold, it will still turn yellow).turn on the air pump, after a short time the solution will take on the green color. the four and a half gallons of solution will need adjusting a little as you go. if the solution gets low due to evaporation, add a little water or fresh hcl. if the reaction is slow to start, add another pint of H2O2.

 

[superten67]

yeah thanks geo all in hand now ive got the other batch perfect now,it was simply a case of me adding the exact ammounts in the different recipes for a ap ive seen and 2 to 1 dosnt seem to work with 9%percent for certain but like you say its trial and error.
i was just greafull for the pointer as to what had happened so thanks.

 

[butcher]

Study the copper II chloride document on Laser Steves web site.

 

[superten67]

cheers and i forgot to add the base metal from the lot that went wrong went in with a new batch to make double sure.
cant seem to find the link for the copper 2 chloride can someone stick it up for me?

 

[superten67]

also when people are talking bleach are we talking common all garden hypochlorite?

 

[maynman1751]

Yep! Just plain old laundry bleach.

 

[superten67]

guys what was putting the black gold in the hcl and bleach supposed to achieve?
i did it and nothing happened and either the stannous i have it past its sell by or something has gone wrong.
and going back to the liquid it came from that is still very dark does that need to be boiled down still further?

 

[Geo]

guys what was putting the black gold in the hcl and bleach supposed to achieve?
i did it and nothing happened and either the stannous i have it past its sell by or something has gone wrong.
and going back to the liquid it came from that is still very dark does that need to be boiled down still further?

NOTHING happened? did it fizz violently and give off chlorine gas? if not, you are not using the right chemicals. make some stannous chloride out of 95/5 lead free solder and hcl. dissolve a small amount of known gold and keep it in a sealed container to test your stannous chloride against.

 

[superten67]

no geo it was basically dry black powder this morning put hcl in till its was a slurry,swished it around and added some bleach.
it gave off moderate white fumes and warmed up slightly.
i left it to settle and it went to black dust in the bottom,with a slight green layer on top.
incidentally the new batch is now emerald green and has that snow globe golden flake effect so its gone the right way this time.
i think ill just put the black in with it and let it decompose back to state.

 

[superten67]

just a quick note to add to this post,i did ask in another post about hcl/chlorox process and what type of bleach is needed.
turns out i have been using hypochlorite but with way too much soap and surfaceants etc and thats whats been messing my processes up.
i have now go 25 litres of bleach from a horse supllies stockist.
i have successfully dissolved my gold and precipitated it back from solution on a couple of occasions now.
you guys say your chlorox is 6 percent the stuff i have is 11 percent and gives a very healthy fizz when mixed with hcl.
so now im sorted thanks for the help everyone.