# Confused about AP



## Moo (May 24, 2012)

Hi forum, have had about 3 kilograms (7lbs) of ceramic cpus bathing in AP with a bubbler for last 4 days when ive been checking the vessels is extremely dark brown however everything appears to be stripping nicely no change in 24 hours so I added some water and it slightly gave off a little bit of smoke so I added a little more acid and peroxide 12 hours later Anxious to save myself some time later on I decided to transfer the vessel into another bucket and clean what foils i had collected already from the bottom of the vessel. However upon collecting the sediment all I got was mainly a black mess of stripped pins and cpu dies not a foil in sight. Am I too inpatient or have I done something wrong here? Aplogies for photo quality its best I could get.


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## goldenchild (May 24, 2012)

Sounds like your black mess is gold. Especially since you saw no foils. The ap probably dissolved your foils and the gold was plated out by the pins base metal(s). Whatever you do don't throw anything away! Make sure you test all your solutions with stannous and filter them extremely well. 

It does sound like you are impatient and AP is for the patient. But there are other ways to get to the end game faster. May I suggest that you separate the pins from the ceramics if possible. Think of how much less solution you'd use for just the pins and how much smaller the reaction vessel would be. There are a bunch of ways other than AP(not that AP is bad). Here are a few ways 

By member Sucho

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=8813&hilit=tall+form(towards bottom of page)

Sucho breaks the cpus up and treats them in HCL. Doing it this way will keep the gold intact without dissolving it.




By member Samuel

The separation method probably wont work for ceramics but it illustrates the point I was making about the seperating the pins from the cpu

Removing pins and processing pins(video on bottom)

http://goldnscrap.com/index.php?opt...fiber-cpu&catid=36:scrap-cpu-a-chips&Itemid=2


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## Geo (May 24, 2012)

if you have a bubbler going, theres no need to add any more H2O2 than the amount you first added to start the reaction. by adding more, you could have dissolved some of the foils in solution. think about this. the bubbler keeps the solution oxygenated and then you add extra oxygen in the form of H2O2, hcl acid will dissolve gold in the presence of excess oxygen. use a magnet and see how much of the material left is magnetic. odds are, its Kovar from incomplete digestion. my advise would be to add all the material back to the solution and proceed with the removal of ALL the base metal before doing anything else.

i would like to add a couple of points. (1) when your digesting CPU's with AP, the P part is unnecessary. i know what you must be thinking. this guy doesnt know AP. the pins on the CPU's is iron based, theres very little copper in a CPU for the AP to work with. hcl when in the presence of oxygen will react with iron and create ferric chloride which is why the color of the solution is off.this is to your benefit because ferric chloride dissolves iron faster than AP anyway.

(2) you would have had better results with a cleaner product and faster if you would have reacted the CPU's in straight hcl on heat. a prolonged boil in hcl would have dissolved the pins in hours instead of days and you wouldnt have had to worry about dissolving your foils.


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## Moo (May 24, 2012)

Thanks golden, point taken about patience  I actually dont mind waiting just got a little inpatient due to the err mishap I just had melting the powder from the first run of fingers I got and having the bowl crack on me  was a porclein bowl and just went pop although i very slowly heated it up to tempreture I was using a mapp torch and after 10 or so pop. so had the urge to recover some losses. A/P is about as far as I want to go I think as playing with Nitric and stuff scares the heck outa me. To separate those pins I think would be near impossible theres so many there, I have filtered several times and just dropped the filtrate with some SMB that contained the rinse water I had a slight reaction and it took on a slight brownish tinge in colour I done this as I haver no stannous atm and no tin to make any. What would be the best way to recover the Gold foil from the reaction solution as present? as far as im aware it should be emerald green, However from the moment I started adding the peroxide to the acid the vessel went brown.
Please forgive my newbiness, I do promise to be more patient and am taking the time to study as much on my own as I can, and thanks again for your help


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## Moo (May 24, 2012)

Thanks Geo the reason I added the cpus as a whole was because I was under the understanding that not being of the fiber type they would contain little iron/kovar I actually have a bunch from fibers I plan on dissolving in acid, I suspect the pins are mainly other metals and have confirmed with a magnet I pulled from a hard drive. Should I proceed to add the sediment back to the reaction vessel and what measures should I now undergo to get the foils back without loss if possible.Remove the bubbler for couple of days? Roughly the soulution would currently consist of 2.4 litres 28% HCL 1.4 Litres Peroxide, I dont think you dont know AP at all I think im silly not having this dawned on me by now after researching this bubbler addition to AP to reduce the need for peroxide the other night.  please forgive me I sometimes make messes of things when I take on to much information at once... lesson learnt.


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## Geo (May 24, 2012)

if you have dissolved any gold, it will be in the fines left over after all the other material is dissolved. if you have any magnetic material in the bottom of the bucket, place all the material back in the solution and let it proceed with the dissolution of the base metal. after a week has gone by, it is safe to assume that everything that is going to dissolve is already dissolved. when you decant the solution, leave the last few inches of liquid and safely tilt the bucket on the edge (i place a brick under one side) this will concentrate all the solids to one side. siphon the remainder of the liquid off or use Butchers method of using a turkey baster bulb and draw the fluid down that way. be sure to leave all solids whether its foils or powder. rinse the final inch or so of solution containing all solids into a glass container and let it all settle. decant slowly down to the solids and add more water. repeat this rinse until water stays clear. next, rinse with hot hcl as many times as it takes until solution remains clear (not much is needed, just enough to cover material). then follow with the water rinses, again until water stays clear. now you can dissolve the solids and filter.


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## Moo (May 24, 2012)

Thankyou for your time Geo,

As im am still a tad confuzzled  confused and puzzled. To clarify. Could you please confirm.
Leave bubbler going?
1.Add Sediment back into centre bucket.
2.Decant after another 3 and a half days which will total a week. From when I have started
3. ??? Gold left is solids? im under the impression just let it dissolve and then drop with SMB after filtering and washing the solids from the solution several times with water.


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## Geo (May 24, 2012)

leave the bubbler going.

(1) yes, add everything back to the reaction.
(2) yes, one week in all. if three more days make a week, then three days it is.
(3)any gold that was dissolved cemented out as a black powder on any solid iron or copper as soon as all the excess oxygen was used up. no SMB needed. if you want assurance you can test the solution with stannous chloride. be mindful of false positives.


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## qst42know (May 24, 2012)

Test that solution for disolved gold.

What strength of peroxide?


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## Moo (May 24, 2012)

3% my friend will test and be mindful of false positives.


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## tek4g63 (May 25, 2012)

Geo, thanks for that great tip about propping the bucket up at an angle with a brick to concentrate the solids in the corner! Its the simple little solutions that are right in your face that are so easily over looked. I will defiantly be using that trick from now on! Once again I have to say, geo you are the man!


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## Geo (May 25, 2012)

thanks Thad. i dont profess to know much but everyones welcome to everything i know.


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## nickvc (May 25, 2012)

Geo said:


> thanks Thad. i dont profess to know much but everyones welcome to everything i know.



Modesty, proof of an experienced and skilful refiner who knows his trade in this case 8)


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## Moo (May 25, 2012)

So basically Geo apart from the fact u is a wiz 
as soon as all the pins and base metals dissolve the powder will drop to the bottom of the bucket, What do I do if all the pins and base metals aren't dissolved withing a week will the powder still drop? I had a peep in the vessel today and there still appears to be quiet a few pins there to dissolve. I considered putting the bubbler in the centre bucket of the vessel to speed things up in dissolution would this help?


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## Geo (May 25, 2012)

placement of the air source doesnt effect the speed of the dissolution, but heat does. i know its hard to heat liquid in a plastic bucket. one member suggested using a metal tub to set the bucket in and add water to the tub and use a fish tank heater in the tub to warm the water thus warming the liquid in the bucket. since there is still quite a bit of material left, instead of rushing it and keeping on disturbing the process, i would suggest letting the chemicals do their work and try to concentrate on something else for a few more days. the process you decided to try is a set and forget type of process. every time you stop the air or remove the solution to check on it means it has to start the reaction over and over prolonging the wait time. trust me, its not going anywhere. if you let it sit there and bubble for a month, it will not hurt any of the gold or other PM's. if you need it in a hurry for a fast turn around, you really should have picked a different process. switching gears now would probably cause you more problems than just having patience and letting it be.

by the way, as long as you have solid base metal and you dont add more H2O2, you will not have to worry about gold being in solution. any gold that may have dissolved is now a fine powder either free floating in the solution or on the bottom of the bucket or still stuck to the base metal it cemented out on.


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## Moo (May 25, 2012)

I will be more patient and leave alone I have some lids here so ill go start on preparing for that and do it properly this time. I was just worried was all. thanks again for settling my nerves. I do really appreciate your time and efforts to help me.


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## Moo (May 27, 2012)

Decanted solution today and most pins are dissolved however some still remain, no powder at bottom of bucet. what to do? I going to go and get some solder to make some stannous and test the solution for gold, if it returns positive shall I drop a ball of copper in? or just leave sit for few more days?


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## Geo (May 27, 2012)

the fact that you still have solid pins would exclude the possibility of gold being in the solution. just re-use the solution for the next batch. you can reclaim the floating foils now, but they will be contaminated. the very tip of the pin could still be in the hollow tube. if you collect the foils now, wash with HOT hcl before dissolving in hcl and bleach. keep in mind, the solution will still be green from the copper and will need to be refined again.


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## Moo (May 27, 2012)

errm ok Geo thanks but theres no foils in sight nothing. <EDIT> After leaving solution sit for a few hours I just checked and now have a black powder will wash thouroughly and add bubbler to solution to rejuvenate,


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## Geo (May 27, 2012)

its amazing and somewhat disappointing that what looks like a lot of foils makes such a small amount of gold powder. thats how gold gets lost in the process. when you dissolve gold foils by accident, the resulting gold powder that cements can be hidden under a very small amount of (undissolved pins, solder mask, copper chloride crystals, trash, loose components) just to mention a few. gold is heavy and will migrate to the bottom of the pile. some will still be stuck to what ever metal it cemented out on. in your case, you need to continue the dissolution of all the pins and collect all the powder. there will be more stuck to any undissolved pins.


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## Moo (May 28, 2012)

OK well I just got to recovering some of the powder, Im assuming leave that in its place for now. Ill restart this bubbler and leave go for few more days. Should I add fresh acid to help?


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## Geo (May 28, 2012)

it certainly wouldnt hurt. just dont add water, it could produce copper chloride crystals making it harder to reclaim any powders.

by the way, this is from CPU's? have you reclaimed any gold from this or are you still trying to get the first bit from it?


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## Moo (May 28, 2012)

errrm ok think im gonna need a bigger bucket, ive added water before so funny you should mention that.  

here is what I have recovered as brownish black powder


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## Moo (May 28, 2012)

Sorry yes from ceramic cpus


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## Moo (May 28, 2012)

Geo I have been doing some more study on the forum and I am now assuming most of my base metals are still cememnted to the cpus and pins had a look at a pentium pro that was in there and its black as mud If the solution tests negative forAu HCL I shall proceed to rejuvenate the solution and dissolve the rest of the base metals and all shall be fine.
Does this sound correct? I think im finally starting to get the basics .


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## Geo (May 28, 2012)

normally, the way ceramic CPU's are processed, is to remove the gold plated lids. they are heavy pieces of base metal that can not be processed in AP. they are an alloy of copper and tungsten with gold plating. the brazing that welds them down contains a large percentage of the gold in a CPU. aside from the lids and legs, theres very little base metal in a CPU. you will have to process the lids with either nitric acid to remove the copper or AR to dissolve the whole lid (which takes longer). the legs are iron based so its a slow go in AP to dissolve the legs. then theres gold plated directly to the ceramic body, AP will not effect this at all and will have to be dissolved with AR. 

this is why ceramic CPU's are processed in AR to begin with. honestly, what you are doing is wasting time and chemicals. in this endeavor i will help you to the best of my ability because even a failure is a plus when your learning. when you finally give up on AP as a way to process these CPU's i will also try to help you process them the right way. 

i didnt try to stop you because if i had, you would have tried anyway and maybe hurt yourself or made a mess of it that you may not have been able to straighten out.

now i have to give you some hard advise. decant the solution you have now and store it in a plastic container with a label so you what it is. take all the material you have from this, everything, and place it in a container with a lid and set it aside. look up "poor man's AR". this is the process that you will need to follow if you hope to recover the gold from your CPU's. 

if you want to proceed with AP to see how far you can go with it, put everything back in the reaction container and start the process again. the legs will eventually dissolve but thats about as far as your going to get with AP.


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## Moo (May 28, 2012)

Thankyou Geo,

Initially I did plan on doing this with HCL to remove the base metals, and then adding it to a solution of nitric and slowly adding HCL, but the idea scares the hell out of me and Ive been hoping to not go there because like just one breath of that stuff and your a goner, and ill have to go bush to do that anyway as im in close proximity to neighbours etc. I was thinking about setting up a distillation apparatus to eliminate the possibility of any fumes, then I might feel a little more comfortable about the whole idea If I have to follow this path, But if its gonna take 2 hours or so to do this are there going to be fumes for 2 hours? what im trying to say is if I set up a distallation apparatus to counter this how large is tfhe recieving vessel going to have to be anyway? Aside from that even if that is a possiblity to eliminate the fumes im going to have to go say hello to that beaker when all is said and done anyway.

The hard advice and your willingness to help is appreciated


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## Geo (May 28, 2012)

yes, you can set up a small apparatus to scrub the fumes from a small reaction with little problem. you would need to do it outside and maybe at night so as to not draw attention. you can use an Erlenmeyer flask with a glass nipple (like the kind used for vacuum filtering) a stopper (i have used rubber, but it must be wound with several layers of teflon tape tightly on all surfaces) nitric acid and rubber doesnt mix well, some chemical resistant tubing and a receiving vessel.

you will need a hotplate to warm the solution and a plastic catch basin large enough for the hot plate to sit in and be far enough from the edge as to not melt it.

you will need hcl (muriatic acid), nitrate (sodium nitrate if you cant source nitric acid), sodium hydroxide (lye, caustic soda). 

the reaction between the hcl and the nitrate will produce nitrogen dioxide gas and will need to be neutralized. the Erlenmeyer flask will be the reaction vessel. connect a piece of tubing to the nipple and cut the length needed to reach the bottom of the receiving vessel with a few inches to spare. the receiving vessel with contain sodium hydroxide solution in water and should be a graduated cylinder or a fruit jar if you cant find one. if you use a fruit jar, be sure the depth of the solution is an inch or so from the top.

this is the basics. read this and find some references on the forum. check out samuel-a's website on how to process CPU's and chips http://www.goldnscrap.com

when you get caught up to here, i will give you more instructions.


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## Moo (May 28, 2012)

Okay Geo heres what I have can quiet easily get nitric or sodium nitrate but if I use nitric acid its going to react straight away right? thus giving me about 2 secs at most to seal the reaction vessel, heres how I am thinking of setting up. 

http://www.youtube.com/watch?v=3JlIPnyrZMw

Apart from the need to use grease I cannot see any problems that jump out at me at least can you? The rubber stopper shouldnt be an issue because glass ones are available.


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## Geo (May 28, 2012)

great. but be warned, unless you already have all the equipment, buying all this will make for one expensive hobby. if you plan on doing a lot of CPU's, then it would be a great investment. 

OK, thats not exactly the setup i would choose. the setup you need is not a distillation rig but a scrubber. there are other devices to cut down on NOx emissions, like a reflux apparatus. it looks like a condenser for distilling, but it mounts vertical instead of horizontal. its open at the top and as fumes are emitted, the NOx fumes condense on the cooled sides and return to the reaction vessel. its not 100% but it does drastically reduce the NOx emissions.

what i described before can be used with lab equipment and some members use it regularly. caustic soda will remove the fumes as the gas is bubbled through it. again, it may not be 100%, but it will drastically reduce the NOx fumes emitted.


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## Moo (May 28, 2012)

Geo I am considering taking this up as a Job and retiring from my old one, but I want to be sure 100% thats its safe and fumes wont be a problem so I dont mind spending whats required to do so im su with time and experience it will soon pay for itself anyway. You mentioned I need to scrub the fumes with water and you could achieve this by using reflux, probaly dont need to ask this but just for assurance is this appropriate?


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## Geo (May 29, 2012)

yes, that is an example of a refluxing apparatus. the longer the condenser, the longer the fumes will be in contact with the cool glass, the more nitric acid is returned to the reaction chamber. you can also incorporate a small scrubber to collect the slight amount of NO2 fumes that make it through the reflux.like i said before, a solution of caustic soda and water will scrub corrosive vapors from the fumes.most scrubbers use some form of vacuum to pull the fumes into the neutralizing environment but if the reaction is kept small enough and you are very mindful of what you are doing, a simple hose run to a vessel with the tip submerged in the liquid may be all you will need. you can smell NO2 fumes in a concentration as small as 1 PPM. it has a very distinctive smell and can be avoided. no canister type filter can filter out NO2 fumes. you should build some sort of fume control devise in case of a container failure or spill.


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## Moo (May 29, 2012)

So what your saying and forgive me if im wrong, is I need to connect some form of tubing to the top of the condenser and have it running into a solution of Naoh to knock out any fumes that make emit themselves out of the water before they get to the outlet? How do Noxx fumes fare with plastic I was thinking along the lines of connecting a plastic duct to the top kind of like you see on some pc cases designed to suck air in through the side to aid c ooling the cpu heatsink and having that connect to a filtration flask with a nipple on each end with the solution in it plugging the top with a glass stopper and on the other nipple connecting that to a vacuum pump and maintaining a small amount of suction with it. <EDIT> Tring to reinvent the wheel here lol
need time to check this out properly


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## Moo (May 29, 2012)

Might I propose 
figure 4 chapter 5 about halfway down page, 
http://www.sas.upenn.edu/~dbalmer/chem502/Labs/lab4_dielsalder/balmerexp4.pdf
have the tube coming from the gas trap to the flask containing sodium hydroxide.


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## Geo (May 29, 2012)

exactly, you can buy chemical resistant tubing at Lowes or Home-Depot. normal plastic and rubber will spontaneously ignite or even explode in the presence of hot nitric acid.nitric acid and cellophane is two of the ingredients in nitro glycerin.

too the tube in the receiving vessel needs to extend into the solution. 

before you do any process with this type of arrangement, check out some of the post on "suck back". when you have a sealed vessel and a condenser with a tube run into liquid, as long as there is solution in the reactor vessel creating fumes or even steam, you have a positive pressure. but should you remove the heat or the reactor runs dry, a vacuum will form in the reaction chamber due to the cooling effect and suck cool liquid into the reaction chamber and at the least fouling the reaction and at the worst causing the reaction vessel to burst.


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## Moo (May 29, 2012)

Great the more I solve the more complicated you make it for me  but its good complication am learning alot, till I get this sorted however I wouldd like to try and get what gold I can back from my AP solution I have been decanting throughout the day and letting sit for a while and so forth getting little bits of black powder is there any way I can get it all in one swoop if I drop the solution with copper? I just want to recover what I can from it now and make sure theres nothing dissolved in that solution. Then ill be content about putting the cpus aside and running them through AR with the other few kilo I have when I get this set up properly.


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## goldenchild (May 29, 2012)

Geo said:


> yes, that is an example of a refluxing apparatus. the longer the condenser, the longer the fumes will be in contact with the cool glass, the more nitric acid is returned to the reaction chamber. you can also incorporate a small scrubber to collect the slight amount of NO2 fumes that make it through the reflux.



Alternatively (and probably more practical in this case) Moo could use a fractional setup. Instead of cooling a reflux column he could replace it with a fractionating column and cool a condenser (liebig or graham) instead. This way he could collect the nitric in pure* form. I think this would be more practical because the nitric will have to be removed from solution eventually anyway. Of course the chemical resistant tubing still needs to be used to collect the escaping nitric coming out of the joint connecting the condenser and collector. Just a thought.


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## Moo (May 29, 2012)

Thanks Golden for the suggestion, I am a newb by all stretches of the imagination but may I ask why you feel it is probaly more practical in my case to do this via freactional distallation? I can manage backflow Just want this to be as good as possible without possibility for messing things up


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## Moo (May 30, 2012)

If a solution of AP is saturated with dissolved metals can this cause a negative charge of electrons and thus be recharged via adding more metals in any form? and causing the solution to drop the dissolved solids?


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## goldenchild (May 30, 2012)

Moo said:


> Thanks Golden for the suggestion, I am a newb by all stretches of the imagination but may I ask why you feel it is probaly more practical in my case to do this via freactional distallation? I can manage backflow Just want this to be as good as possible without possibility for messing things up



Sure. It sounds like you want to set up a closed glass system of some sort so I feel that with a few more pieces added to the setup you could kill a few birds with one stone. With fractional distillation you would be ridding the digestive solution of nitric which must be achieved no matter which way you decide to process your material. Also, with a condenser and collector you will be able to reuse a significant portion of your nitric acid.

But honestly... I think a glass closed system would be over complicating things. Especially if you are just getting started. When you have a firm understanding of recovery/refining I think you could do just as well if not better with a hotplate and a few beakers. But ultimately you will decide how you want to go about things.


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## Moo (May 30, 2012)

I see your point golden and agree I could use a distallation set up well also killing a few birds in one stone, you are suggesting then that simply by using a graham condenser because it is coiled it would take longer for the fumes to get through to the top and by then they would have condensed and return to the flask and I also could use it for such purposes as distilling water and purifying vapours etc as my knowledge and needs grew? Sounds like a great idea to me.. I have been looking for a magnetic hotplate also to improve things and speed processes up a little and have came up with this. But ultimatly if I have to deal with 
http://www.heidolph-instruments.com/fileadmin/media/3._Support/Betriebsanleitungen/Magnetruehrer/BAL_MR_Hei-End_01-005-004-59-1_05Sep2011.pdf

Its the MR Hei End specs on page 45 looks like it could help me tremendously especially for processing fingers in AP a beaker that a little heat and auto stir would be magnificent 

Sure its expensive all this glassware etc but the way I look at it is how valuable is your life?

What are your thoughts?


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## goldenchild (May 30, 2012)

I think maybe I can best explain with a picture I found on ebay. The vigruex column is simply a column in which the nitric vapors will pass through. The main difference between the column in this picture and the one that you provided is the refluxing. If you notice the vigruex column in NOT water cooled therefore much less of the nitric will go back into the reaction vessel. The cooling is done at the condenser. In this case the setup is using a liebig condenser. Since the cooled condenser is on a downward slant the condensed nitric won't go back into the reaction vessel but to the collection vessel. This is what I was saying about collecting your used nitric and using it again. If you notice there is a spout on the elbow that connects the condenser to the collection vessel. This is where you would hook up the tubing to deal with the small amount of nitric vapor that gets past the condenser. Here is where you would put the tubing into your hydroxide solution. Back pressure would have to be accounted for or your neutralizing solution will go into your nitric!





As far as the hotplate. In my opinion the magnetic stirrers/hotplates have too many limitations. As you have already found they are very expensive. Since you are just starting out you will almost definitely have boil overs until you get a better grasp of the chemical reactions and trying to keep them under control. You will be very unhappy spilling the concentrated acids we use on an expensive hotplate. I personally use a double burner hotplate that costs under $30 from walmart and is pretty much a throw away if need be. One of our veteran members GSP uses a skillet which can be gotten for even less. He has been doing this for much longer than I so it can't be wrong. Then there is the surface area of your heating element. The magnetic stirrer hotplates tend to have a very small surface area for heating beakers and seem to get much more expensive by the inch. On the hotplate I use I can easily heat 4000ml beakers with room to spare. I'd imagine that with a skillet you could heat any size beaker you can find. So the only plus I can see for magnetic stirrer hotplates is the stirring feature. But if you are planning on processing fingers I don’t think this feature will work well. Besides, you could use a bubbler if agitation is what you're looking for.


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## Moo (Jun 1, 2012)

I see what you mean golden, great idea ill get right onto that and study this backflow effect, thanks for your help


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## Moo (Jun 1, 2012)

having ants in my pants and nothing much to do but wait for my stannous to arrive. I have been trying to get my gold from the ferric chloride solution anyway after removing all the pins and cpus I put them in a fresh batch of a/p for a couple of days and to my delight most of the remaining gold dissolved I added this to my original very greenish black almost solution of what was a/p but which I had essentially turned into ferric chloride by adding too much peroxide and having a bubbler added, yesterday I noticed that the solution was now much more like a dark yellow very much if not exactly like auric chloride and having no copper in the form of a bar to cement it out of soulution I decided to just use some SMB So I divided the solution into two buckets and added some SMB to one this morning upon decanting into the other bucket yay I had some black powder although very hard to decant even slowly it was very fine, my filter papers arrived yay (Fisherman brand No 1) yes I know No2 is prefered but all I could find at the time, anyway :mrgreen: so I spent the day filtering all of the solution I definitly after the entire day filtering ended up with black stuff alright but its more like thick mud and not powder. What is going on here? And what is the best way to get this off my paper and back into some fresh acid for refining  I was thinking of just dropping it in there paper and all, tried a scraper but the mud is to thick.


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## tek4g63 (Jun 1, 2012)

I can't give you all the help you have asked for but I can suggest a way to possibly get you powder back into a reaction chamber. I use a water spray bottle to gently wash it off the filter. Just be patient and gentle. The little bit of water you wash down with it will not hurt anything. Good luck.


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## lazersteve (Jun 1, 2012)

Burn the filter papers down to ash then process the powder in a minimal volume of AR or HCl-Cl.

Steve


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## Moo (Jun 1, 2012)

thanks guys for the help, I will place papers in a a container and set attack with mapp torch then dissolve the remains in HCL/Bleach


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## Geo (Jun 1, 2012)

i agree with steve. incinerate to be sure you get it all.


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## Moo (Jun 3, 2012)

Anyone care to comment on this column? not exactly like the one Golden presented so not sure, http://www.ebay.com.au/itm/VIGRUEX-COLUMN-/160645487180?pt=AU_Business_Industrial_Medical_Scientific_Equipment2&hash=item2567379a4c#ht_3099wt_714


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## goldenchild (Jun 3, 2012)

That actually is the same type of column. It's a vigreux column. For a 300mm column $91 is WAAAAAY too expensive. For a little more you could get an entire distillation setup. If you're still dead set on using a closed glass setup check this out.

http://www.ebay.com/itm/New-1000ml-...718?pt=LH_DefaultDomain_0&hash=item2ebbc619b6

To find more use "distillation kit" in the ebay search.


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## Moo (Jun 3, 2012)

Thanks golden I have no idea on prices of this stuff very good of you to inform me of that. 
I do insist on a closed system because id like to do this at home if possible and those fumes are extremly toxic just scares the heck outa me, I have been avoiding this using AP for everything but know thats not posssible now,
I have been doing some research and have found a different kind of setup which addresses the problem of backflow as well. any thoughts? the only problem I can for see is the stopcock at 9 being plastic maybe? and if backflow were to occur with the valve closed could possibly create enough pressure to break the glass.


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## lazersteve (Jun 3, 2012)

Dean stark traps are designed to pull water or other solvent out of a reaction as it forms. This would result in the acid peroxide solution becoming dehydrated and forming salts. Not a good idea.

I would recommend you focus your energy on building a good scrubber set up for the reaciton vessel and preform the reaction in a safe environment. The problem I see with any reflux reaction is that in the event of a failure or glass breakage, you will still need secondary containment around the reaction to protect yourself and others. 

I don't recommend running any of the reactions laid out on the forum inside of a home. You need a dedicated work shop or garage at the very least. A good fume hood with scrubber and proper safety gear are also a must. At the bare minium work outside away from pets and people with good air circulation.

Steve


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## Moo (Jun 3, 2012)

Steve, sorry for the confusion its actually for running AR reactions and scrubbing the fumes by dripping it off into solution of NaOh I originally started this thread because of AP problems with cpus ande upon taking Geos advice am trying tocome up with something I can set up outside for it normally I just do my AP outside in a bucket following the method you have on your videos.


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## lazersteve (Jun 4, 2012)

For AR solutions you want to reflux your fumes/liquid directly back into the reaction vessel so as to get the most life out of your nitric acid before it becomes neutralized. This technique also sends any pregnant solution that makes it's way into the condensor, via spray and spatter, back into the reaction vessel. This setup will not only extend the life of your nitric it will also requrie fewer glassware components saving you money on both counts.

Any fumes that make it through your reflux condenser are then scrubbed further down the line. Typically the fumes that make it past the condenser are mostly gases and need to be bubbled through the scrubber solution. These fumes are further scrubbed after exiting the bubbler liquid with a high surface area media wetted with the scrubbing solution in the form of a mist sprayed down from the top of the scrubbing tower.

Steve


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## Moo (Jun 4, 2012)

Wow ok Steve thanks, So what your saying is I should go with this apparatus then and there shouldnt be any problems? A few people have mentioned heat causing the borosilicate to break so am starting to think perhaps I should go in another direction. But I cant afford a fumehood/scrubber and im not the handiest person when it comes to building things.


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## Geo (Jun 4, 2012)

no glass is fracture proof but borosilica glass is made for heating. thats one reason its used for lab glass.honestly you take a chance every time you do a process of something going wrong. but if you do the best you can with what you have to minimize the danger, if and when an accident does occur, the effects will be minimal. if you never take the chance you have failed. personally, i feel its better to try and fail then to never try at all.sure, its very daunting, working with known harmful chemicals and glass and heat. thats the dangers we face to do what we do.some do it just to be able to say they did it while others make it into a career.whatever your motivation, whether its to refine your own gold to horde or to make extra cash or even a full time job if you spend too much time worrying about what could go wrong and not enough about how to make it go right, you will be doomed to failure.


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## Moo (Jun 4, 2012)

Geo Please dont take this the wrong way but I think its one hell of a danger you breathe that stuff in mate its all over red rover so Im just making sure nothing should go wrong is all I think that will calm me down when I hear so and rather then just go get something without the knowledge of someone more educated in this manner then I would be a bit stooopid methinks. So is steve saying this is a good way to go or???
Thanks again.


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## Geo (Jun 4, 2012)

i know the dangers of nitrogen dioxide fumes very well. i suffer with COPD every day and have never smoked a cigarette. of coarse be safe, there is never a question of skimping on safety. there are some members on the forum that have refined for decades and probably are more healthy than me. i did it to myself and would never recommend someone do something i thought would be harmful. if you go back through the post, you will find where i recommended a form of fume control in case of an accident. a fume hood is a form of fume control that anyone that is serious should be using.i certainly didnt mean to throw caution to the wind.

good luck and happy refining.


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## lazersteve (Jun 4, 2012)

The dean stark apparatus is *not the way *to go. A simple reflux condensor is a better choice.

As for taking a chance to learn, we all have to take some chances to a certain degree, but remember :

*Chance favors the prepared.* 

So be prepared for the problems (at least the ones you can think of) and things will go a lot smoother, even if you have a 'meltdown'.

My main point in the post above was to be sure you are not relying on this glass reactor as your sole protection of insuring your health (and your families if performing indoors). Two layers of safety are much better than one. Being prepared for an accident makes you that much more ready to deal with it in a timely manner. Some accidents occur quickly and there is little time for running away or containing the problem.

Steve


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## goldenchild (Jun 4, 2012)

Moo said:


> Wow ok Steve thanks, So what your saying is I should go with this apparatus then and there shouldn’t be any problems? A few people have mentioned heat causing the borosilicate to break so am starting to think perhaps I should go in another direction. But I can’t afford a fumehood/scrubber and I’m not the handiest person when it comes to building things.



I think Steve is actually suggesting the opposite. I am definitely suggesting the opposite. Trying to do this stuff inside the home is a very bad idea. As Steve said it's best to have a dedicated work area outside the home or at least work outside away from other life forms. I know that fumehood and scrubber systems can be quite expensive and it’s sucky just how expensive they are but there is a way to get around that. You can make these systems or possibly have someone else make one for you. I made a fumehood system rather inexpensively so that I could work indoors (my detached garage), albeit a direct vent system without a scrubber. It’s the same as working outside. If you aren't able to come up with a plan of this sort then you gotta ask yourself if it's feasible to be refining at this point in time. :|


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## Moo (Jun 4, 2012)

Errm I never planned on doing this inside guys  always outside for sure, anyway looks like im going to have to make up my mind now if I wanna do a simple reflux set up and do it out bush in the case it breaks or build a scrubber thanks very much for the help.


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