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Author: Subject: Nitric Acid Synthesis
DJF90
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[*] posted on 7-9-2009 at 16:31


That would insult about 80% of the members of this board. Think before you speak. And you fall far short of a chemist.
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entropy51
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[*] posted on 7-9-2009 at 16:32


Quote: Originally posted by Picric-A  


Im a chemist- i prefer to buy Reagent grade 98% sulphuric acid or 69% Nitric acid if i want it, not crappy 'drain opener' like you probably do!


If you can buy nitric (or sulfuric) then why on earth are you trying to decompose fertilizer (is that reagent grade too)?

And of course with your official police sanctioned research lab license you are allowed to possess "any chemical you desire".

If you're a chemist, why are you buying obsolete Rotovaps that don't even have half the parts?

If you're a chemist, why didn't you know the answer to this?


Quote: Originally posted by Picric-A  
can ammoniium nitrate be used to make nitric acid via H2SO4 + nitrate salt method?
Picric a

If you're a chemist I wonder why most of your posts read like they were written by a 14 year old kewl?

[Edited on 8-9-2009 by entropy51]

[Edited on 8-9-2009 by entropy51]

[Edited on 8-9-2009 by entropy51]

[Edited on 8-9-2009 by entropy51]
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panziandi
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[*] posted on 7-9-2009 at 16:37


Wait a minute there!

Quote: Originally posted by Picric-A  
If you have easy acess to conc sulphuric this reaction works extremly well.
Simply add pices of copper to a flask followed by conc sulphuric acid and simlpy heat to produce a steady stream of SO2, quite dry. This method works well when you have plenty of drain opener. Of cours it is pointless when using it to make sulphuric acid via contact process... :P


This was posted by you Picric-A on 30-8-2008 at 10:33 AM, http://www.sciencemadness.org/talk/viewthread.php?tid=11101#... now then you imply using cheap drain unblocker over lab grade due to cost, that is EXACTLY what Entropy is suggesting by using a cheaper "OTC" grade of sulphuric acid to generate your own cheap nitric acid.




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DJF90
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[*] posted on 7-9-2009 at 16:40


There is nothing wrong with drain cleaner quality sulfuric acid. If one has the determination and patience, and suitable apparatus it can be cleaned to an equal specification as 98% reagent grade, and even higher if necessary. For many things, it will suffice where concentrated sulfuric acid is needed.
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entropy51
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[*] posted on 7-9-2009 at 16:42


A real chemist would know that some things don't require reagent grade chemicals, wouldn't he?

I save my ACS reagent grade chemicals for the purposes that require them.

And if one knows what he's buying, not all drain cleaners are crappy. Some are 96% and "technical" grade.

[Edited on 8-9-2009 by entropy51]
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DJF90
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[*] posted on 7-9-2009 at 16:43


A real chemist would know alot of things...
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[*] posted on 7-9-2009 at 16:47


The continuing conflict between several members and Picric A and his derivatives is degrading the quality of this forum. I think all who participate should at try to hold back on the comments a bit, though it is damn hard I'm sure.

Picric A, want to help drop your conflicts between members, by not replying to what you might believe are personal attacks? I can see how your post above was provoked, but why do you choose to keep it going? Please stop for the sake of the forum.

As for the others, it would also be a good thing to stop this BS. Seriously, how many threads have derailed and ended with discussing the quality of Picric A?






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panziandi
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[*] posted on 7-9-2009 at 16:53


My Picric acid is ACS reagent grade...



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entropy51
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[*] posted on 7-9-2009 at 17:00


OK, here you used a "roaring bunsen flame"
Quote: Originally posted by Picric-A  
i used roaring bunsen flame which proceeded to completion (on 2g scale)


But here you say you heated it with nichrome wire:

Quote: Originally posted by Picric-A  

how does it work?? well you could not be lazy and read the thread, but i guess i could tell you. I heated a copper tube full of Ca(NO3))2 beads with Nichrome wire then passed the evolved gasses through a series of bubblers.


Not only are you a liar Picric/Saber/Labxyz, but you are not even a good liar. It's beyond me why you haven't been banned for crapping up our forum with your fairy tales.
Quote: Originally posted by Picric-A  
If you had read what i wrote carefully you would note that.

Note- The hint is when i said on 2g scale and 'full of nitrate beads'
If you did write carefully (and you certainly don't) we wouldn't need hints to decipher what you claim to have done.

[Edited on 8-9-2009 by entropy51]
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Picric-A
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[*] posted on 8-9-2009 at 01:13


Roaring bunsen on test tube scale and nichrome on copper tube scale. If you had read what i wrote carefully you would note that.

Note- The hint is when i said on 2g scale and 'full of nitrate beads'

[Edited on 8-9-2009 by Picric-A]
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[*] posted on 8-9-2009 at 21:04


Quote: Originally posted by kclo4  
The continuing conflict between several members and Picric A and his derivatives is degrading the quality of this forum. I think all who participate should at try to hold back on the comments a bit, though it is damn hard I'm sure.

Picric A, want to help drop your conflicts between members, by not replying to what you might believe are personal attacks? I can see how your post above was provoked, but why do you choose to keep it going? Please stop for the sake of the forum.

As for the others, it would also be a good thing to stop this BS. Seriously, how many threads have derailed and ended with discussing the quality of Picric A?



Ive got to agree.Thre kid is trying to impress with his obvious flights of fancy and fails to understand that it seriously impedes his ability to benefit from the knowledge of seasoned members and real chemists.
However sustained derisory commentary from those that completely overwhelm the young Walter Mitty both academically and rhetorically is painful to witness.

[Edited on 9-9-2009 by starman]

[Edited on 9-9-2009 by starman]

[Edited on 9-9-2009 by starman]




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[*] posted on 9-9-2009 at 11:03


Eloquently put.
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[*] posted on 9-9-2009 at 20:21


Somebody ban that f*ckin...

I think he's on bombshock rubbing his cock all over the threads.
"Lol, y wud u waste all dis munney makin nitric when you can by it soo easy?"

That aside, I'm 14, and I don't act like that faggot.
Why did we even bother with this stupid decomp of nitrates for HNO3? Its dirty, annoying, with low yields and general faggotry. I would think that the bigger questions aren't being answered on this thread, but it seems people has plenty of time to argue wit that noob.

Would you guys think that a magnetic stirrer would be worth making to prevent bumpin on reduced pressure nitric distillations? Will bumping even occur at like 20-30 torr?
I know that a stirrer will increase how fast the nitric will evaporate, but is that worth integrating it into your home made heating mantle?

Oh, and I'd assume that if I manage to hook up two aspirators in series then I could increase the vacuum? I saw this on the other threads, but does anyone know by how much? i.e. two aspirators in series both capable for 29.5torr

Cheers
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[*] posted on 10-9-2009 at 04:33


Quote: Originally posted by panziandi  
OR saturated calcium nitrate solution and add sulphuric acid (fairly strong if not concentrated) that would ppt CaSO4 and leave with a fairly storng nitric acid solution which could be filtered and distilled.


I think CaSO4 is pretty soluble in concentrated nitric acid, so this would only work form making dilute acid.
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[*] posted on 10-9-2009 at 11:16


Quote: Originally posted by uchiacon  

Oh, and I'd assume that if I manage to hook up two aspirators in series then I could increase the vacuum? I saw this on the other threads, but does anyone know by how much? i.e. two aspirators in series both capable for 29.5torr


That would not be a correct assumption. The ultimate vacuum is set by the vapor pressure of the water. You should reach that with a good aspirator, and hooking two in series will not give a better vacuum than one by itself.

I would never vacuum distill without stirring on account of the likely bumping. Sometimes they bump even WITH stirring.

You sure your aspirator is only pulling 29.5 torr? Right now my aspirator is pulling 15 torr (read off a Hg manometer) at a water temperature of 24 C (which is not very cold at all.) Did you buy the aspirator new? Plastic (and to a lesser extent) metal aspirators do wear out and don't pull as low. Glass aspirators last forever (unless you break them.)

[Edited on 10-9-2009 by entropy51]

[Edited on 10-9-2009 by entropy51]




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[*] posted on 10-9-2009 at 21:02


Well I just looked at the aspirator and it said 29.5 torr max... couldn't find many glass aspirators either. But wouldn't a metal aspirator be just as good as a glass one? They're both pretty darn hard.

This is one of the only glass aspirators I found, and it looks like it has that old style aspirator make. are these ones as affective as the normal ones?
www.onlinesciencemall.com/Shop/Control/Product/fp/vpid/17874...

And one from sigma aldrich, somehow at a crazy 150USD.
www.sigmaaldrich.com/catalog/ProductDetail.do?D7=0&N5=SE...

If you has any other sources for a normal looking glass aspirator do tell.

Cheers
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[*] posted on 11-9-2009 at 05:54


I think the metal aspirators may not hold up in the long run if you distill a lot of HNO3 with them. HCl fumes probably won't do them any good either. Occasional use with acids may be OK, though.

I believe my glass aspirators were made by Kimble, but they look very much like the one in the Aldrich link above. Yes, they look old fashioned, but my glass aspirators wotk better than the metal and plastic aspirators that I've used. The vacuum is as good or better and it seems to me that the glass aspirators use less water, although I haven't measured the water consumption.

But if the one you have works for you then what more can you ask?




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[*] posted on 11-9-2009 at 07:54


Introduction of a tiny amount of air below the surface of the pot liquid will prevent bumping. I do this with a piece of glass tubing drawn to a pipette end. On the other end of the tube is a piece of rubber tubing with a screwed pinch clamp for adjusting the air flow rate. The tube is held in place with a thermometer adapter in a Claisen adapter. This is the method recommended in my organic chemistry lab manual. It works well.

If requested I can post a picture of this "ebulliator."

[Edited on 11-9-2009 by Magpie]




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entropy51
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[*] posted on 11-9-2009 at 09:06


Magpie, I'll bet you and I are the only ones hereabouts who've used an ebulliator.

Gatterman would be proud of you!

I'm old school but I gave them up when I got a magnetic stirrer. They do work - unless solid forms in the pot and then I didn't find them as helpful.




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[*] posted on 11-9-2009 at 10:22



Will a few boiling chips not help here? Some pieces of red flowerpots sounds good.
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[*] posted on 11-9-2009 at 10:34


Boiling chips seem to lose their effectiveness under vacuum, although some people do use them. And bumping tends to be worse under vacuum. Boiling chips work fine for distillation at atmospheric pressure.



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[*] posted on 12-9-2009 at 00:35


The metal aspirators are made out of brass with a laquer coating.
So not just plain metal.

Also tried out my 68% nitric today on some copper plating stripped off gouging rods, made tons of NO2. Lucky I did it outside, and then I reduced the copper nitrate to copper bits with zinc battery casings. Wish we could do that at school..

Can you give me a link for your kimble glass aspirator? Or any other links for a glass aspirator? And do the different designs make a difference?

Cheers
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[*] posted on 12-9-2009 at 01:38


Quote:
Can you give me a link for your kimble glass aspirator? Or any other links for a glass aspirator?


http://208.72.236.210/html/pg-924000.html

http://www.onlinesciencemall.com/Shop/Control/Product/fp/vpi...

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mad.gif posted on 12-9-2009 at 05:28


Quote: Originally posted by uchiacon  

Lucky I did it outside, and then I reduced the copper nitrate to copper bits with zinc battery casings. Wish we could do that at school.
Cheers

Man you MUST be joking I took highschool chemistry in 1990 and copper in nitric acid was an essential lab to demonstrate metal chemistry. We put copper in nitric acid in a fume hood, went home and then returned the next day and add water if needed and added sodium hydroxide to make copper hydroxide gell(loved that):D and then heated the gell to form black Copper oxide. After decantation 6M HCl was added to form clear green solution and an aluminum wire was dropped in. Went home and came back next day to find clear solution and salmon colored copper deposits with a little debris from the aluminum.

I suppose you are now going to tell me they no longer do the sugar in sulfuric acid trick or the lead iodide gold trick.




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[*] posted on 12-9-2009 at 11:50


Quote: Originally posted by chloric1  
Man you MUST be joking I took highschool chemistry in 1990 and copper in nitric acid was an essential lab to demonstrate metal chemistry. We put copper in nitric acid in a fume hood, went home and then returned the next day and add water if needed and added sodium hydroxide to make copper hydroxide gell(loved that):D and then heated the gell to form black Copper oxide. After decantation 6M HCl was added to form clear green solution and an aluminum wire was dropped in. Went home and came back next day to find clear solution and salmon colored copper deposits with a little debris from the aluminum.

I suppose you are now going to tell me they no longer do the sugar in sulfuric acid trick or the lead iodide gold trick.


I took HS chem last year. We did none of those things! I wish we would have! I didn't like the teacher though; most of the class was bookwork and we hardly ever did labs. The most "dangerous" thing we ever did was titration of HCl with NaOH (and we did that within the first two weeks of AP Bio this year!). No nitric or sulfuric at all; even the teacher didn't demonstrate anything with them. We did maybe one metathesis, and it wasn't nearly as cool as the lead(II) iodide precipitation. Didn't even cover redox in the class. The worst part was that my school didn't have AP Chem, so I couldn't take a decent chem class!

Even so, thats what a home lab is for!

[Edited on 12-9-2009 by bilcksneatff]

[Edited on 12-9-2009 by bilcksneatff]

[Edited on 12-9-2009 by bilcksneatff]
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