taiwanluthiers Posted December 22, 2012 Posted December 22, 2012 I read you can make silver nitrate by dissolving silver into nitric acid, and from looking around it seems it's the most cost effective way of getting silver nitrate because the stuff costs more than the equivalent amount of silver bullion/coins. The question is, how much nitric acid do I need for a standard troy ounce, and how dangerous is the nitrogen dioxide fume produced (I will be doing the reaction outside)?
Potassiumchlorate Posted December 22, 2012 Posted December 22, 2012 The fumes from concentrated nitric acid are horrible and very dangerous. However, if you go down to 53% it's no that bad at all. Don't know whether it's too diluted for the reaction, though. The theoretical reaction is simply: 2Ag + 2HNO3 ---> 2AgNO3 + H2. That means 37% by weight of 100% nitric acid to 63% by weight of pure silver or 55% of nitric acid by weight if using 65% nitric acid. Someone more skilled might say whether this is also practically possible.
taiwanluthiers Posted December 22, 2012 Author Posted December 22, 2012 normally "concentrated" (as in non fuming) nitric acid is 68% or so, at least the one I got is 68%. It wasn't too expensive either but I figure I can take some silver coin and make silver nitrate with it... The reaction makes NO2 in itself.
Potassiumchlorate Posted December 22, 2012 Posted December 22, 2012 Do it outdoors and/or use a gasmask.
pyrojig Posted December 22, 2012 Posted December 22, 2012 One thing that really helped kick things off was using a hot plate. As I recall, there is a need for water to be present in the Hno3 to make the reaction happen. I used 70% about 100ml in a beaker and one oz of silver. The silver was chopped into slivers with some metal sheers. Once the reaction gets going lots of poison gas is produced. As stated above DO OUTDOORS, or in a proper fume hood. The gas's can kill you if you get a good wiff. Once the reaction gets going the heat needed will decrease, due to the reaction self sustaining heat in the degrading process. Of course , make sure to be in protective gear when attempting the process ..
dave321 Posted December 22, 2012 Posted December 22, 2012 I read you can make silver nitrate by dissolving silver into nitric acid, and from looking around it seems it's the most cost effective way of getting silver nitrate because the stuff costs more than the equivalent amount of silver bullion/coins. The question is, how much nitric acid do I need for a standard troy ounce, and how dangerous is the nitrogen dioxide fume produced (I will be doing the reaction outside)? now why are we making silver nitrate ? are you also using ethanol by any chance dave
psyco_1322 Posted December 22, 2012 Posted December 22, 2012 (edited) And what pyrotechnic use does silver nitrate have? I'd say this is almost in the wrong section of the forums. Looks like Dave beat me to it! Edited December 22, 2012 by psyco_1322
pyrojig Posted December 22, 2012 Posted December 22, 2012 (edited) You mistake its wonderful use : in detecting chlorides in the chlorate purification process . It is great!!LOL you guys are stuck in the HE realm ... Any exploding mirror's in the making . I guess the industry had a few probs with Agno3 and other compounds used in making mirrors going boom during manufacture or upon drying and moving . Edited December 22, 2012 by pyrojig
taiwanluthiers Posted December 23, 2012 Author Posted December 23, 2012 I am not going to make flash with Silver Nitrate... it's going to make the world's most expensive flash. I just need it to determine if chloride is present in the chlorate I make, and I can't think of any other way to do this.
WSM Posted December 23, 2012 Posted December 23, 2012 I just need it to determine if chloride is present in the chlorate I make, and I can't think of any other way to do this. I believe lead nitrate reacts similarly to silver nitrate. I suspect the silver nitrate is more sensitive though, and can accurately detect chloride in very small concentrations. In my Handbook of Chemistry and Physics, under the title of "Laboratory Reagents for General Use", it lists "Silver nitrate, 0.5 M, 0.5 N. Dissolve 85 g of AgNO3 in water. Dilute to 1 liter." A full liter doesn't have to be made, and other concentrations are also useful as indicators (even quite dilute ones). It's important to know the concentration of your indicator solution. Armed with that information, others can follow your work and be certain of the results they observe. Therefore, be certain to clearly mark your container of test reagent with as much information as you have available (or keep an accurate lab book nearby), but at least indicate what the test solution is and it's concentration. WSM
taiwanluthiers Posted December 23, 2012 Author Posted December 23, 2012 I thought of lead nitrate, I wasn't sure if it's sensitive enough and if it will cause confusion (like will other things like lead chlorate also show ppt?) Another thing about lead nitrate is its extreme toxicity... not sure if it's something I want around.
50AE Posted December 24, 2012 Posted December 24, 2012 (edited) Nothing wrong with lead nitrate, just don't swallow it or breathe its powders. If you can't handle lead nitrate properly, you cannot do the same for pyrotechnics mixtures IMHO. The problem is, it isn't sensitive enough for a precise test. If lead chloride precipitates in your solution, it's very chloride contaminated. Just compare the solubilities of lead/silver chlorides and you'll get the picture. Merry Christmas ! Edited December 24, 2012 by 50AE
pdfbq Posted December 25, 2012 Posted December 25, 2012 (edited) Nothing wrong with lead nitrate, just don't swallow it or breathe its powders. If you can't handle lead nitrate properly, you cannot do the same for pyrotechnics mixtures IMHO. Merry Christmas !I do not agree on this. Lead nitrate is very soluable which makes skin contact also something you do not want. Second, lead builds up in your body, you do not get rid of it anymore. But I agree silvernitrate is the way to detect chloride. It is so sensitive though that you need demi water to test with.Tap water immediately goes white with the nitrate. I used i think 1 gram for 100 cc water but probaby 1/2 gram will do to.1 drop of this solution in tap water at my home turns it white. When you want to store your test solution do it in the dark. Edit: i do not say you can not work with the Pb nitrate but do not underestmate it. Edited December 25, 2012 by pdfbq
50AE Posted December 25, 2012 Posted December 25, 2012 Underestimation was not my point. Getting familiar with it its properties and toxicity was. Every chemist or pyro must learn to do that before handling a substance.
taiwanluthiers Posted December 25, 2012 Author Posted December 25, 2012 Most pyro chemicals except for Lead Tetraoxide (used in dragon eggs) do not bioaccumulate, I say most because there are still some like Paris Green, Dichromate that probably does bioaccumulate. I think the most toxic chemical I have is probably barium nitrate, and if it doesn't kill you it won't bioaccumulate like lead can. At least Lead Tetraoxide is insoluble meaning it won't do as much damage to you in the case of skin contact. I don't know what lead nitrate does to you but the thought of a highly soluble lead compound doesn't sit well with me... But then lead nitrate is also like 10,000 times cheaper than silver nitrate, and even silver itself is cheaper than silver nitrate, although I don't know how much silver nitrate can you yield with one troy ounce of silver.
pdfbq Posted December 26, 2012 Posted December 26, 2012 (edited) I think yield can be 100% so ~31 gram will give you some like 45 grams of AgNO3 and thats a lot. Disolve all in HNO3, get rid of the excess HNO3 (boiling might do the trick) and boil down till syrup. Then dry for 2 weeks with CCl2 or NaOH, thats the way I would try to make it. Edit: nurdrage channel at youtube has some vids about making nitrates, even silver iirc. Edited December 26, 2012 by pdfbq
Mumbles Posted December 27, 2012 Posted December 27, 2012 The equation you're looking for is: Ag + 2 HNO3 ---> AgNO3 + NO2 + H2O You really should be able to figure things out from there on your own. Also, of course silver nitrate is going to be more expensive than straight silver metal. Silver nitrate is very easy to reduce to silver metal, so no one is going to sell it for less that the equivalent silver price.
pyrojig Posted December 27, 2012 Posted December 27, 2012 I believe yield is over 100%. But as Mumbles stated , it is a very simple equation . Just steer clear from the No2 gas.
Mumbles Posted December 27, 2012 Posted December 27, 2012 You should probably also carry out this procedure with a reflux condenser or a watch glass over the beaker. Once the reaction gets going, it's fairly violent, and can spray precious silver solution out if you're not careful. Once the reaction subsides, just rinse the sides of the container and watchglass/condenser down with distilled water.
Potassiumchlorate Posted December 27, 2012 Posted December 27, 2012 Hm, Mumbles is right But why don't you buy silver nitrate from KeteN? He is a son of a bitch, but it's much easier than making it yourself.
pyrojig Posted December 28, 2012 Posted December 28, 2012 I've made it with very good success. It is not a hard procedure. One must be careful , and pay close attention to the details of steering clear of the gas, and making sure the acid is heated to start the reaction then it will go on its own. One thing that I did to control the crazy violent stage was to add small slivers of silver a little at a time( v.s. the whole bar) . This gave me a lot more control , and kept the chance of a violent boil over spill from happening . I find it also helpful to cover your hot plate with foil to catch the splashes if they do happen. It will make for a easier cleanup and a catch for the spills.
taiwanluthiers Posted December 28, 2012 Author Posted December 28, 2012 just how bad is nitrogen dioxide? Is it something that as soon as you smell it you have to go to the hospital right away? I know if you can see the brown its bad, but if its done outside, will it still be bad for you? Wikipedia seems to make it sound as though the gas is worse than cyanide... I plan on doing it outside and starting the reaction with a pot of hot water...
Potassiumchlorate Posted December 28, 2012 Posted December 28, 2012 just how bad is nitrogen dioxide? Is it something that as soon as you smell it you have to go to the hospital right away? I know if you can see the brown its bad, but if its done outside, will it still be bad for you? Wikipedia seems to make it sound as though the gas is worse than cyanide... I plan on doing it outside and starting the reaction with a pot of hot water... You won't die from feeling the smell of it, but accidentally inhaling it may destroy your lungs. It's one of the few compounds that really scare me.
pyrojig Posted December 28, 2012 Posted December 28, 2012 You will know if you got to much in your lungs. It will burn like the worst fire in your throat and lungs. It will cause the lungs severe damage, to the point they fill up with liquid trying to protect them= you drown internally. A slight wiff will only cause your head to rear back from the pungent odor. It is a sharp smell, I have smelt it in small amounts( very diluted in the air). A direct wiff over the beaker will surely cause a trip to the hospital. Indirect dilute gas's are very dangerous still, and may cause you to feel a bit sick ( flu like) , but usually nothing more.
taiwanluthiers Posted December 28, 2012 Author Posted December 28, 2012 I saw the thing on Nurd Rage where they made nitric acid with nested beakers... I think it might not be a bad idea for me to do this when doing the reaction, just so that any NO2 that forms gets absorbed by the water and minimal amount gets into the environment. It will still be done outside, but this time with less NO2 gas escaping.
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