# confused about ap drop?



## superten67 (Dec 7, 2012)

a couple of days ago i drained out another lot of ap foils and some powder that had come of of the same boards put it through some filters and had black mud speckled with gold foils.
washed that with water a couple of times,then hcl twice then dissolved it in hcl and bleach.
left that for about 4 hours then drained it through a filter to get rid bits of solder mask and any other foreighn bodies then added some water to dilute it a bit.
i precipitated the gold out with ferrous sulphate and within seconds it when a very cloudy brown colour and started to settle.
left it alone for about 24 hours and had settled at about 2 to 3 mill all the way across the bottom of a 1000ml glass beaker.
fantastic i thought finally ive cracked it.
now comes the funny part i then drained this solution through a filter and came back after an hour and the filter was stained slightly brown and the vast majority of the brown solution had gone through the filter and in the hour it had been left had settled on the bottom once again?
whats happening people...any ideas?


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## Palladium (Dec 7, 2012)

What kind of filters and system are you using?


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## superten67 (Dec 7, 2012)

when you say system do you mean acid peroxide or ar?if so im using ap but to start with i was using 9% peroxide so at the begining i was having the situation where the foils were comming off and turning into black powder but some foils did come off as gold as i diluted it down somewhat with water to lower the percentage if you see wha i mean.
so from being quite dark it went back to a nice emerald colour.


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## Palladium (Dec 7, 2012)

Tell me when you say filter what kind of filter media are you using. Charmin plug, coffee filters, buchner funnel with or without vacuum. I see the drip part you said now so i assume gravity filtering?


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## superten67 (Dec 7, 2012)

yes in a funnel with with filter papers using gravity down ito a second jar.


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## Palladium (Dec 7, 2012)

What type and size filter papers? And when you say it got through the filter paper are you talking about just the fine stuff or the fine and course stuff both? Are you pouring all your gold into the filter or just the bit that might escape from pouring off the solution?


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## superten67 (Dec 7, 2012)

this is what i dont get,all the videos ive watched show really clumpy brown precipitate that looks cryatalized.....now i know deep in my heart its gold,because one minute i had a greeny yellow clear fluid and when i added the ferrous to the mix the colours changed in exactly the same way as the laser steve vids and various you tube clips.
but the powder which is deffinately powder is really fine.
i had it boiled right down earlier but my partner was moaning about the kitchen door open and extractor fan on and a slight odour.
so i filtered it again and the same happened again.


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## Palladium (Dec 7, 2012)

Let it sit over night and then lightly pour off what you can without losing any. Redissolve it and drop it again from a concentrated solution. It will clump together real nicely. You will see the difference in grain structure of the gold and it will be a whole lot easier to deal with after that. I always drop my gold twice no matter what, sometimes more if i'm trying for top end quality.


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## Palladium (Dec 7, 2012)

Not to be hard but if you want to learn and in order for us to help you when people ask direct questions they need direct answers. You still have not answered what i ask about the filters and if your pouring you gold into them to catch the gold or just to catch anything that might escape.


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## superten67 (Dec 7, 2012)

well theres nothing in there now i need apart from the gold ......so yes to save the solids(gold)and be rid of the waste fluid.


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## Palladium (Dec 7, 2012)

That was my last answer to this post! Someone help the man please.


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## patnor1011 (Dec 7, 2012)

Your partner should run for her (or his) life. If you use HCl/Cl and SMB in kitchen you are (very mildly said) *crazy*.
Your extractor fan is not even close to keep you safe and you just contaminated whole kitchen. Good luck to you every time when you will be preparing your food there.

Now that question again, what type of filter did you use?


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## butcher (Dec 7, 2012)

How easy did the solution go through the filter, what color was the solution before you tried to precipitate the gold? Was it a clear yellow solution? From the green color, I suspect you have iron, from the foggy liquid something else insoluble, like tin or silver.

There is an awful lot of powders there, how much material did you process were these clean part or circuit boards with all kinds of metals involved?

I would decant the solution (adding liquids from the process below), and test it with stannous chloride and treat it accordingly.
I would wash the powders well in boiling hot water, bring them to neutral with dilute NaOH sodium hydroxide wash and rinse out salts well, incinerate the powder red hot, keeping the powders broken or ground up fine, stirring while red hot to get good air exposure, cool and then boil in HCl, add just a little water and let powder settle well before you decant liquid, but decant while the liquid is still very warm, give them boiling hot water washes till the water comes out clear, decanting while the liquid was still very hot, then re-dissolve in HCl/NaClO (bleach), heat to remove chlorine gas and then precipitate the gold again.


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## superten67 (Dec 8, 2012)

these are the filters im using,
The Edu-Lab Filter Paper 125mm (Pack of 100) is high quality filter paper, widely used for qualitative analysis. Ideal laboratory resource for schools.
and ive got to say if yours is the kind of help thats on offer dont bother mate i dont need people like you talking down to me im a 45 year old man with a family.
i dont think ill bother asking a question on here again and i especially dont want any replies from the last bloke who answered.


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## Palladium (Dec 8, 2012)

Well good luck to you then mate!


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## nickvc (Dec 8, 2012)

superten67 said:


> these are the filters im using,
> The Edu-Lab Filter Paper 125mm (Pack of 100) is high quality filter paper, widely used for qualitative analysis. Ideal laboratory resource for schools.
> and ive got to say if yours is the kind of help thats on offer dont bother mate i dont need people like you talking down to me im a 45 year old man with a family.
> i dont think ill bother asking a question on here again and i especially dont want any replies from the last bloke who answered.




I'm sorry but I can't sit back having read that last part about having family...
If your processing in your home your putting yours, your families and neighbours health at risk plus contaminating your home possibly the neighbourhood and the environment. Please stop and read the safety section, if I'm reading this wrong then my apologies but if not please try to understand what we are trying to tell you!


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## superten67 (Dec 8, 2012)

see this is what i mean.....whats with all the negativity?ive asked a simple question and all im getting is abuse.
i know about safety i've used acids before in lots of jobs,i used to work for a firm that processed catalytic converters and have worked extensively with explosives synthesis.
it just seems to me that some like to be overbearing and exert their will on others and make out they know it all.
i suppose some of you do but it still dosnt give you the right to talk to people like children.
i've had lots of help and good advice from this forum but don't need to be patronised by people telling me i dont know how to do things safely and how to not put my family in danger.
why someone would want to pluck that from the air as yet another way to make out theyre god and go completely in a different direction and miles away from what the thread was about i dont know.
i have a secure shed in my garden and extraction from doing jobs with saws and furniture repair and chemicals are locked in a secure site box there........is everyone happy now?
as i said i think the search option will be better in future as the natives certainly dont have a kind and caring manner.


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## qst42know (Dec 8, 2012)

Help and concern, meets prideful and obtuse.

Remains confused.


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## superten67 (Dec 8, 2012)

right lets see,we know i know fairly well what im doing now as i have gold residue,ive followed all the steps ive been offered from all sorts of sources including here mainly.
i simply have a few niggling issues 1st being mainly that the gold i precipitate from solution is so fine it seems to go through any filters have to hand at the moment i have others comming as we speak.
my hcl is 36%,my chlorine bleach is 11%,i am using ferrous sulphate to precipitate,and the hydrogen peroxide im using(now)is 3%.
i have 2 sets of shoulder reach rubber gauntlets,a respirator,a pair of wraparound protective glasses,everything is being done safely and almost exactly as ive read.
the only thing i can think off is the bleach....do i need to dilute it 50% with water being as the concentration is nearly double what everyone else is using?
i dont think so it seems to me i should just use less.
ive done my recearch and lots of reading but something is missing.
now i appriciate that people dont like answering the same questions over and over again but im not asking the same question im asking a segment of a question.
if you can help me please do,if you want to nit pick or abuse then say nothing thats upto you.
an as for you nick i think i can tell what your like iasked you as a fellow brummie in the spirit of friendship where you were from as ive lived all over the birmingham area and you just blanked me completely your probably a university don who thinks its below you to talk to a factory serf like myself.
but let me tell you this im far from stupid and dont like being talked to like an idiot as you wouldnt so id appriciate no further input from you either.
any CONSTRUCTIVE input would be great but please dont have a go at people for the fun of it as life is hard enough as it is.
and before you do comment remember your motto"refiners helping one another"not taking the rise out of each other.
ive seen various europeans on here you can tell by the way they word thing and quite a lot of the time they just get ignored.
and they soon stop posting as they know no one is interested in answering the questions they ask.
if any of my questions are the apparently same "glaringly obvious to the experts"type of questions then do the same just ignore them and ill look elsewhere.
also if everyone IS so concerened about others safety why not put them straight instead of insulting people inteligence and just being plain rude.

anyway rant over and if you want to talk to me in a friendly manner ill do the same back if you dont then dont talk at all as im not gonna be syeam rollered into defeat.


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## qst42know (Dec 8, 2012)

No one here wants your defeat.

Concerns for your safety are genuine.

Help often requires more information.

Attacks, abuse, and attitude aren't tolerated here at all. If you weren't so defencive you might find what you need.

That is if you haven't insulted those that can help with all the accusations.


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## superten67 (Dec 8, 2012)

i havnt insulted anyone,ive answered questions ive been asked back in order to help me,ive even tried to befriend people through pms etc and asked for help in private rather than seeming too needy and asking a question every 30 seconds and ive been told i dont know what im doing and should'nt be doing in my own home and putting my family at risk....all without any of you knowing the conditions im conducting my experiments in,and its not any of you who have been ignored and had posts read and ignored its me.
and i cannot see anywhere in this thread anything that would prompt anyone to tell me im being dangerous or irresponsible.
ive said thank you to everyone who has commented sometimes even the ones that hav'nt been positive.
and still now the simple question about bleach percentages you've ignored and just started to correct me again about my attitude like you would a child.
have you got an answer about the question i asked?or did you not notice the humble me yet again asking for advice from people you think would know?


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## maynman1751 (Dec 8, 2012)

Superten, let me try to defuse this situation. I believe that some members where getting irritated when they ask you a question and didn't get a direct answer back. Maybe you thought you answered them but there was a misunderstanding....I don't know. Some of the statements that you made sounded as if you were performing these processes in an unsafe manner or environment. Even I picked up on that. We don't know what your experience and knowledge are concerning these dangerous ingredients and we are truly concerned for your safety and proper understanding of what you are doing. I know for fact that you have received very valuable help and information on this forum and it would be a shame for you not to take advantage of that. I do understand your defensiveness. I too felt at times that new members were being belittled until I understood that it was for their own good and not just to be overbearing and snotty. Just calm down, regroup and let's try to accomplish something beneficial. I hope that this helps. Now let's get to work!


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## superten67 (Dec 8, 2012)

im fine and i agree with everyone whole heartedly,as i said ive been involved in the manufacture and use of explosives over the years and its check,check and double check.
im sorry also if i seem abrupt some of what i said i stand by some might have been a bit over the top.
i have had lots of helpfull pointers and wouldnt be at the stage im at now without all your help so thanks.
and thanks to you personally for taking the time to explain yourself and talk to me at the very least like an ADULT who dosnt understand what he's doing.
i have the basics and am safe in all of the respects of the processes im using thus far.
and just in case anyone is wondering as ive allready been told my grammar and spelling is rubbish there are a couple of characters on me keyboard that get missed now and then i did well at english at school so please bare with me if theres any spelling errors a lot of the time it isnt me,or sometimes maybe it is as i have big clumpy fingers and a tiny keyboard and i admit i do get a bit excited as i love the hobby and the site.
and i know it seems im not taking advice properly and doing things step by step but i am i swear to you.
for one thing the chemical constituents of household bleaches etc seem to vary wildly from the uk to the usa.
i have had a problem with disolving foils because of this which is now solved with the purchase of some 11%hypochlorite.
ive had the foil and black powder situation and made a complete hash of what was looking good through putting what might as well have been fairy liquid in it when it said hypochlorite on the label.
the only outstanding problem i can see is the 11% bleach should i dilute it 50% with water or should i just use less?
anyone subscribed to this thread should take it as an apology but i really do think people who use this site should talk to each other a bit more repectfully.
thanks again maynman.


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## nickvc (Dec 8, 2012)

Superten67 I'm sorry I didn't respond to your query about where I'm from I probably missed the post, I try to read all the posts every day but sometimes fail, if you stay on here long enough you will see what I mean.
Right I was born in Bournville and lived around that area until I was in my mid 30s when I moved out into a little village on the borders of Shropshire and worcestershire until my divorce which forced me to back track a little and I now live in Bewdley. I fear your wrong when you assume I'm a university don, I was an art student studying jewellery design who ended up working at the Assay Office then Johnson Matthey and several other bullion dealers before setting up and running my own refinery which I have to say was very successful while we had a manufacturing base still in the UK but as all that died so did my business and marriage. I'm still based in the jewellery quarter and still do some small time recoveries and refining but all I learnt was from experience and trial and error, I didn't have Hoke or the forum to rely on, you do so I suggest a little less aggression and try to understand we all have every members best interests in our minds when we post replies we don't just yell because we like the noise we actually care, we don't get paid, we help becauase we can and we like to.
You can insult me all day I really don't care but I do care about any new members health and will post regarding that where I feel the need, i did notice you clarified that point but remember we have many members whose first language isnt english, I suggest you try not to antagonise any of the existing members any further if you want any further help as the forum can and does close ranks when people decide to take an attitude. 
We are here to help and as I said before no one gets paid so try and be a little appreciative when anyone bothers,no one has to.


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## nickvc (Dec 8, 2012)

To help clarify your point about the bleach the only difference in the strengths is that you will add more oxidiser to your solution with a stronger bleach solution which will react quicker but may take longer to remove the excess to allow successful precipitation, heating helps.


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## superten67 (Dec 8, 2012)

yeah cheers for the bio,and im sorry if you feel insulted,i should'nt have spoken out of turn like that without knowing anything about you,what you do or where you get your knowledge from.
but you did exactly the same accusing me of not knowing what im doing,being unsafe and threatening the welfare of my family and my rant was in self defence you just piped up and went off on one.
me ive worked in a lot of heavy industry,foundrys,chemical wharehouse lol you know they make you do safety training before letting you have free rein of a 4 ton fork lift in a shed full of acids and flammable oxidisers.
i then went on to work in a factory which manufactured explosives i was a lab assistant and one of my jobs was to aid in tests of the difference explosiveness or(brissance)to anyone who knows nothing about them and to also test other ways they could potentially be set off by accident,where spillages could occur with other chemicals,sensitivity to impact etc.
ive been a builder learned some usefull stuff there too,and finally my last job was in a factory the reclaimed pms from catalytic converters,did some lab work there too but not that much,mostly worked on heavy machinery,cutters presses etc.
cant say i know much about jewellery bought a bit for the mrs but not really my thing ive never wanted any after seeing a bloke fall off a ladder on a building site and end up hanging from a nail and loosing a finger that was i was 17 and swoar id never wear any on site.
unless i can buy some cheap and make a profit.
still to this day it make me laugh when i see all the young lads on sites done up like elton john not mad on jewellery or jewelers for that matter.
do you remember what gerald ratner said about his stock? or was it h samuels i cant remember but i do know most of its overworked overpriced tat i wouldnt touch apart from to melt.
anyway nick have a nice day and i hope the flood defences in bewdley hold up for you they deffo cost enough,i like bewdley used to go fishing there a lot years back for half a day and then go to holt fleet for the other half of the day and go shooting on a farm i used to have permission on.
sommat else i know about weapons safety but then i had to.
talk another day nick.


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## superten67 (Dec 8, 2012)

nickvc said:


> To help clarify your point about the bleach the only difference in the strengths is that you will add more oxidiser to your solution with a stronger bleach solution which will react quicker but may take longer to remove the excess to allow successful precipitation, heating helps.




thanks for that that may well be where the current problem lies.


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## Palladium (Dec 8, 2012)

Ok getting back on track here lets see if we can help you. After you precipitated your gold did you do any washes on it?


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## superten67 (Dec 8, 2012)

hi palladium,yeah i washed it a good few times in water and once in hcl....but am beginning to think it should have been more.
im also think as i said theres a problem with the bleach but i only added it in small increments until the gold and black gold had disolved and there were no more solids and was all in solution.


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## Palladium (Dec 8, 2012)

I had some gold last week that was almost that same color orange. I filtered and filtered it, i mean like 10 times. Usually once your filter is packed up with gold the fine stuff won't make it through. I kept filtering and would wait about an hour or two later and look at the filtered solution and their was gold settling out as a very, very, fine dust in the bottom of my vacuum flask. Aggravating was what it was. I even triple stacked the filter paper with no luck stopping it. Finally i let it settle, wash it with water, let it settle, poured it off slowly as not to lose very much, and redissolved it. After i precipitated it it was a courser material and i had no problems what so ever. I use a vacuum filter and trap my gold in a buchner funnel the first go around then incinerate the filter and redissolve it again so you might not do it exactly this way but maybe it will help you some. The second go around no gold should be poured into the filter, only left in the beaker for drying.


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## butcher (Dec 8, 2012)

How much oxidizer or bleach to use, I do not go by a recipe, but you can find one on the forum, sorry I cannot answer what is recommended, but maybe this can help.

Let’s look at how we dissolve gold.
Nitric acid HNO3 will not dissolve gold alone.
Hydrochloric acid HCl will not dissolve gold.
(Actually nitric acid will oxidize the gold at is surface to Au3+).

If we add HNO3 and HCl, then we can dissolve gold into gold ions (the strong acid taking electrons from the gold atoms) to make a solution of gold chloride in this highly acidic state as Chloroauurate acid HAuCl4.
the strong oxidizing reaction of the nitric acid forming AU3+ ions, and HCl with this reacting to form chloroaurate ions (AuCl4) (water soluble gold chloride salts), as atoms of gold from the surface lose electrons and dissolve into solution more gold atoms are exposed to these acids and oxidizers to react, and to dissolve more gold into solution.

A common equation for this reaction:
Au + 3NO3 + 6H --> Au3+ + 3NO2 + 3H2O
Au3+ + 4Cl --> AuCl4

Nitric oxide can also form in this reaction the chemistry involved is actually much more complicated than the equation above represents.
When we mix these two strong acids there are several reactions going on in solution (even more when metals are involved),
Mixing concentrated HCl and HNO3 it also produces volatile gases in solution, these gases will also react with our metals (these gases do not stay in solution long, that is why we cannot premix and store our Aqua regia to use later, the active ingredients like the gases can leave the solution leaving us with a strong acid that without these gases would not dissolve gold that well)
NOCl nitrosylchloride gas and Cl2 chlorine gas are two of these volatile gases that will also react in our aqua regia solution to help dissolve gold or platinum.

3HCl + HNO3 --> NOCl + Cl2

NOCL can decompose further to form more chlorine and nitrous oxide gases.

2NOCl --> Cl2 + NO

Nitrous oxide reacting with air above our vessel can give us the red fumes we see as NO2 gas
NO + O2 --> NO2
2

3HCl + HNO3 --> NOCl + CL2 + 2H2O

How much oxidizer do we need? Much depends on how you perform the reaction, if your solution was dilute (gases will not escape as easily and can mix with water to reform acids), or if your solution was cold (cold solutions can hold more gases), what all metals you have in solution can also make a big difference as metals lower in series would react differently than the more noble metals, so as you can see saying you need this much oxidizer as nitric acid with this much HCl, would not always be true if you used or ran your reaction different or under different conditions.

It is good to have a little excess HCL, and to keep the solution acidic, the oxidizer (nitric acid or bleach) can be added in small increments only using the amount needed to dissolve the gold.


Now let’s look at dissolving gold with NaClO bleach or sodium hypochlorite and HCl hydrochloric acid.
Some things we should consider 5% NaClO has 95% water, it will also be basic solution containing NaOH sodium hydroxide (to keep chlorine in the in solution), so not only will adding bleach dilute our acid but it will also form salts out of our acid (neutralizing the HCl to table salt) reducing our acids effectiveness to dissolve more gold into solution.

2HCl + NaClO --> NaCl + Cl2 + H2O
2Au + 3Cl2 --> 2AuCl3
2Au + 3Cl2 + 2HCl --> 2HAuCl4
HCl + NaOH --> NaCl + H2O

2HCl +NaClO + 2HCl --> 2NaCl + Cl2 + H2O
Cl2 +H2O --> H + Cl- + HCLO
HCLO --> H + ClO
Cl2 +Cl- --> CL3
Au + Cl- + 3/2Cl2 --> AuCl4

Here again temperature of the solution will also determine how much chlorine we generate and how long it will stay in solution, as well as the solutions concentration, adding bleach not only dilutes our solution more it also neutralizes the acid in solution (needed to generate chlorine) which will also affect how much gold can be dissolved, also the metal involved if fine powder or very thin such as you will find on plated glassware or the thicker gold foils from memory can also determine how much of the reacting acid and bleach we would need to get our gold dissolved, how easily it will dissolve, or how much gases will be formed from the reaction.

When I add sodium hypochlorite to hydrochloric acid to dissolve gold, I do not go by a recipe, but I do add small portions to create chlorine in the acidic solution let it react, and add more later as needed (sometimes I do the opposite having gold in a bleach solution and add portions of HCl acid to dissolve the gold), I also use heat to help speed the reaction (more chlorine gases form but also more unreacted gases leave the solution more hypochlorite needed, and also creates more salts in solution and neutralizes more acid), or give the reactions more time and dissolve the gold in a cooler condition where it takes longer but uses less bleach and less acid.

over use of bleach is generating chlorine gas that gases off without doing any work to dissolve metals like gold or platinum, it dilutes the solution with water and neutralizes more acid (making the solution less effective at dissolving metals), and creates more salts out of your acid, and if too much bleach is added when you need to rid the oxidizer, heating can create more salts that as the salt solution drives off the chlorine and water.

After we use an oxidizer to dissolve the gold or form gold chloride the oxidizer needs removed from the gold chloride for us to be able to precipitate or gold from solution, or to reduce the gold back to metal powders (reduction is to give the gold atoms back electrons), in another chemical reaction, so using too much oxidizer can also make it a little more difficult when we wish to precipitate the gold, when using nitric acid this is more of a problem, so using only the amount of nitric needed becomes important, if you do not wish to spend many hours evaporating solutions, or adding another contaminate to your gold solution, chlorine in solution from using sodium hypochlorite as an oxidizer is much easier to remove as the chlorine gas will not stay long in a hot solution, 

How much bleach to add?
Much depends on how you drive the reaction.
But to get an idea of how much you may need to begin with, read the general reaction list provided on the forum, I believe a recommended recipe is there.


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## superten67 (Dec 9, 2012)

Palladium said:


> I had some gold last week that was almost that same color orange. I filtered and filtered it, i mean like 10 times. Usually once your filter is packed up with gold the fine stuff won't make it through. I kept filtering and would wait about an hour or two later and look at the filtered solution and their was gold settling out as a very, very, fine dust in the bottom of my vacuum flask. Aggravating was what it was. I even triple stacked the filter paper with no luck stopping it. Finally i let it settle, wash it with water, let it settle, poured it off slowly as not to lose very much, and redissolved it. After i precipitated it it was a courser material and i had no problems what so ever. I use a vacuum filter and trap my gold in a buchner funnel the first go around then incinerate the filter and redissolve it again so you might not do it exactly this way but maybe it will help you some. The second go around no gold should be poured into the filter, only left in the beaker for drying.



thanks palladium seems like i need to drop to drop it 2 or 3 times then i think thats what quite a few people on the forum do from what ive read lately.
and thanks again for sticking with me.


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## superten67 (Dec 9, 2012)

butcher said:


> How much oxidizer or bleach to use, I do not go by a recipe, but you can find one on the forum, sorry I cannot answer what is recommended, but maybe this can help.
> 
> Let’s look at how we dissolve gold.
> Nitric acid HNO3 will not dissolve gold alone.
> ...



thanks also to butcher.


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## Palladium (Dec 9, 2012)

Not a problem brother!


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