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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?
 
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!

setup.jpg


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.
 
I see what you mean golden, great idea ill get right onto that and study this backflow effect, thanks for your help :)
 
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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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.
 
Burn the filter papers down to ash then process the powder in a minimal volume of AR or HCl-Cl.

Steve
 
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
 
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
 
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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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
 
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.
 
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
 
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.
 
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.
 
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.
 
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.
 
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
 
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.
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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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