Mardec Posted October 26, 2007 Posted October 26, 2007 Hey I recently got some HClO4. 70%. And I made some ammoniumperchlorate with ammonia. 12 %. I made it by slowly mixing and cooling it and then boiling the water off. and when almost dry putting it in an exicator. In total I made 5 grams. But the ammonium perchlorate is pretty crappy. With my finest Mg powder it just sparkles. So now I am wondering, are there soms test to see if the acid is perchloric acid? Basic and simple tests please. And I don't have a lot of HClO4 so I wouldn't want to waste it. The acid it self is viscous and clear. Some what like H2SO4.. Thanks in advance.
WarezWally Posted October 26, 2007 Posted October 26, 2007 You do realise that this is some pretty nasty and dangerous stuff?
Mumbles Posted October 26, 2007 Posted October 26, 2007 Well, I'm glad you could be helpful Wally. Anyway, about the best way to test would be to add a drop to a small sheet of paper or something. If it's nitric, it will probably turn yellow, if it's sulfuric acid, it will probably start charing, but with perchloric acid it will hopefully start on fire. If available, sulfuric acid side by side with the suspected perchloric may help to distinguish them.
DeAdFX Posted October 27, 2007 Posted October 27, 2007 Well you could mix copper or a copper salt, sugar(hexamine whatever) and supposed Ammonium Perchlorate if you get a blue color then you will have ammonium perchlorate. I don't think you should be getting a supper fast combustion reaction with Ammonium Perchlorate and magnesium. Unless you are using really fine chemicals. By any chance could you give us a rough estimate of the particle size of your chemicals.
Voryon Posted October 27, 2007 Posted October 27, 2007 I made NH4ClO4 some time ago, more or less the same way as you did. To see that your Ammonium Perchlorate works as an oxidant simply make a saturated solution of it, soak a piece of paper with the solution and dry it. On ignition it burns like a fuse. It is quite interesting to watch it burn as it looks different than made with sodium-/potassium- chlorate/nitrate. To test your perchloric acid I`d recommend to add a few drops of it into a solution of ~5% KOH. As the forming KClO4 is poorly soluble it`ll precipitate on instant. Potassium Salts of other common acids are much better soluble. Nice Side Effect: You`ll produce KClO4
andyboy Posted February 9, 2009 Posted February 9, 2009 [Andyboy starts making a fool of himself] Hi. I found a nice bottle of Perchloric acid on a shelf (thanks Rooster) by incident. I am thinking about making some Ammonium Perchlorate although I want to use the right amount, have been searching around but decided it's time to show of my complete ignorance. NH3 (aq) + HCLO4 (aq) = NH4CLO4 That should be right, right? Now for the big question, do I take a mole weight each of the Ammonia (17 grams) and the Perchloric acid (~100 grams) and mix it? The Ammonia is 24.5% solution and the Perchloric acid is 70-72% solution, should I calculate it to 100% each to get the right amount without wasting to much material? Say, 69,4 grams of Ammonia solution to 140 grams of Perchloric acid? Would it be best to have an excess of Ammonia or an excess of Perchloric acid, I would prefer the former seeing tha t I only have a limited amount of the latter. I do have a lot of Ammonium Cloride , would that be a better material then Ammonia? [/Andyboy stops making a fool of himself for now]
crazyboy25 Posted February 9, 2009 Posted February 9, 2009 Well I believe the equation is: 4NH3 + 4HClO4 = 4NH4ClO4 so you need 68g ammonia and 400g Perchloric acid. Your ammonia is 25% so its roughly four times as much (272g) and your perchloric acid is 70% so about 1.4 times as much (560g). Perchloric acid is much harder to come by then ammonia so an excess of ammonia might be desirable so I would say about 285g of your 25% ammonia and 400g perchloric acid. (This can be scaled down of course.) BTW the L in Cl isn't capitalized.
Mumbles Posted February 9, 2009 Posted February 9, 2009 Crazyboy, where did you get that reaction formula from? It's 2nd week high school chemistry to put it in the most reduced form. NH3 + HClO4 ---> NH4ClO4 or NH4OH + HClO4 ---> NH4ClO4 + H2O You might want to check what type of % you have. Chances are it's in grams per liter. You should probably also check to see if the ammonia percentage is based on Ammonia, or ammonium hydroxide, as it will change the values. Chances are it is based on ammonia though. MW Ammonia - 17.03MW Perchloric acid - 100.46MW Ammonium Perchlorate - 117.49MW Ammonium Hydroxide - 35.05 So, we need 1 mole of each so 17.03g NH3 + 100.46g HClO4 ---> 117.49g NH4ClO4 Assuming grams per liter, and concentration based on ammonia, and 72% acid this gives: 69.5mL Ammonia soln + 139.5mL perchloric acid I would use a slight excess of ammonia, just to make sure it's all neutralized. You don't want perchloric acid in anything. Say 75-80mL. This hopefully should be enough to account for ammonia loss, and make sure all the acid is neutralized. You may want to dilute everything too. It could be a rather intense reaction. After it's done, you can boil it for a while to remove excess ammonia. Obviously this is an outdoor reaction due to the boiling, and the use of perchloric acid. I'd almost be tempted to do this over bare dirt. The perchloric acid will light up any wood or organics like grass, and will soak into and remain in any concrete. I've heard stories of fume hoods blowing up as the cement tables were being broken apart with hammers 10 years after perchloric acid exposure.
andyboy Posted February 9, 2009 Posted February 9, 2009 Thanks guys. I didn't have it that wrong then, love the excess Ammonia thing. Thought about changing the L to l but that would make your comment look strange.
tentacles Posted February 9, 2009 Posted February 9, 2009 I agree with mumbles here, bare dirt is the way to go... Perchloric acid can be very dangerous stuff indeed. Keep all solvents FAR FAR away from it. Be careful too of what plastics you have near your reaction, as some could catch fire or create perchloric salts.. and most non-alkali perchloric salts are unstable and energetic to say the least.
crazyboy25 Posted February 9, 2009 Posted February 9, 2009 Crazyboy, where did you get that reaction formula from? It's 2nd week high school chemistry to put it in the most reduced form. You're right, I was just balancing it because I thought there might be other products but there aren't and I forgot to put it back into simplified form. 1
Sylar Posted February 10, 2009 Posted February 10, 2009 This may sound more chemist-ish then pyro-ish, but perchloric acid is WAY more valueable then ANY of its salts ... Sell the perchloric acid and buy at least 3 times the qantity of perchlorate from the profits.
andyboy Posted February 10, 2009 Posted February 10, 2009 This may sound more chemist-ish then pyro-ish, but perchloric acid is WAY more valueable then ANY of its salts ... Sell the perchloric acid and buy at least 3 times the qantity of perchlorate from the profits. Who would I sell it to? If I knew someone who would buy it and someone that would sell Ammonium Perchlorate to me I would most definitely go that route. By the way, wanna buy some Platinum Oxide?
Boomer Posted February 10, 2009 Posted February 10, 2009 Mumbles, you sure it's grams per liter for both? It is likely for ammonia since it's a dissolved gas, but for the HClO4 I bet on weight percent. Otherwise better check your bottle of conc. sulfuric, it should have 184%
Mumbles Posted February 10, 2009 Posted February 10, 2009 Maybe my sulfuric acid is just that awesome I'll check in the lab today what the units are on the perchloric acid bottle. You're probably right though. Convert that 139.5mL to 139.5g. I don't offhand know the density of the azeotrope. On a related note, we had a lab safety lecture a few weeks ago. Apparantly KClO4 is like the most dangerous thing ever Little do they know just how much I possess. I also got all the incompatibilities right. Just picked out the pyrotechnic uses for them, chances are that's the incompatibility.
Yankie Posted February 10, 2009 Posted February 10, 2009 (edited) On a related note, we had a lab safety lecture a few weeks ago. Apparantly KClO4 is like the most dangerous thing ever Little do they know just how much I possess. I also got all the incompatibilities right. Just picked out the pyrotechnic uses for them, chances are that's the incompatibility. Ha, you think thats bad, my chem teacher was saying how dangerous Al powder is, it was atomized I think, and she put it in the fume cupboard so she could add some water to it to see what happens. I had one of the students come up to me and give me a lecture how dangerous it is, when I told them I have used about a kilo of different meshes and sizes all in comps wetted with water they considered me "lucky" that I am not dead yet. You wonder why pyro is frowned upon, the chem teacher would probably not want to open the jar of KClO4 for fear of it exploding her hands if she touched it. Oh and to add insult to injury, she then started using potassium dichromate with no protection! I am going to write a 2000 word essay on how the media has effected the publics view on pyro, that should be a good way to vent. Speaking of which this is probably more apropriate in the Venting Room. Something a bit more on topic... Theres a guy in Adelaide near me that sells HClO4, I had the tinyest consideration to buy some, but hearing how dangerous it can be I dont think I will bother. Edited February 10, 2009 by Yankie
WarezWally Posted February 11, 2009 Posted February 11, 2009 Perchloric acid 60% AR 500ml $43.50 I can buy that right now and have it on my doorstep in a few days If I wanted to, I one of those items I would love to have but don't want to take the risk. I'm surprised he is able to ship it under dangerous goods
andyboy Posted February 15, 2009 Posted February 15, 2009 (edited) Ok, so I poured up 140 grams of Perchloric acid (70-72%) and 80 grams of Ammonia (25%). This was mixed in a large heat-resistant glass vessel, slowly so as to avoid any spattering. Excess Ammonia was used until no further reaction was taking place. The Ammonium Perchlorate formed immediately and the mix was heated to drive of the very slight excess of Ammonia. The Ammonium Perchlorate was cooled to ~+5C° and filtered. After drying I ended up with 198 grams of Ammonium Perchlorate. Doesn't that seem like a lot? Edited February 15, 2009 by andyboy
Swede Posted February 15, 2009 Posted February 15, 2009 Looks good to me. I'm lazy - what would the theoretical yield be? And is it 100% dry? I've had salts shed water for days after I thought they were "dry".
Mumbles Posted February 15, 2009 Posted February 15, 2009 Yes, that does seem rather high. Quantitative should have been around 120g. There may be some water trapped in there. You could also try washing it with alcohol to try to get some of the water out of there(assuming that is what it is), and helping it to dry faster. It's sparingly soluble in alcohol. Heating in a glass dish in the oven for a few hours should probably do the trick. I'd personally recrystallize it first though. I wouldn't want to put anything potentially with traces of ammonia or perchloric acid in the oven.
andyboy Posted February 15, 2009 Posted February 15, 2009 (edited) I'll try it again since I might have been confused when measuring, I might have taken ml's instead of grams . It wasn't completely dry when weighing it but over 70 grams of retained water sounds like a lot to me, although I don't know if the Ammonium Perchlorate suffers from water inclusions in the crystal lattice when formed so fast. Anyway, I used it to make stars with this formula: Ammonium Perchlorate 82Copper Benzoate 18Dextrin +5 It is a spectacular blue colour. I just love it. Edit: Here is a link to the stars in a ground test: Edited February 16, 2009 by andyboy
TheSidewinder Posted February 16, 2009 Posted February 16, 2009 That sure was a nice deep blue. Good job.
Mumbles Posted February 16, 2009 Posted February 16, 2009 Yes, 70g of water is very high. 70g of anything is a lot really. Thats like 25-30% excess. The density of perchloric acid is 1.67g/mL, and the ammonia .912g/mL. That'd make it 234g perchloric acid. This should still mostly be washed away though.
andyboy Posted February 16, 2009 Posted February 16, 2009 Yes, 70g of water is very high. 70g of anything is a lot really. Thats like 25-30% excess. The density of perchloric acid is 1.67g/mL, and the ammonia .912g/mL. That'd make it 234g perchloric acid. This should still mostly be washed away though. Well, in any case I would have noticed that I would have to use a lot more ammonia then 80 ml's if I would have taken almost 100 grams extra Perchloric acid so that is out of the question. Has to be something else, to bad I can't figure out what.
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