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Ammonium Perchlorate And Sodium Hydroxide

Author: Subject: Ammonium Perchlorate Synthesis
TitusGabonicus

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Ammonium Perchlorate Synthesis
I thought it interesting, the opinion danger level fastened to the following reaction: {synthesis of AP, from 'Hawley'south Chemical Dictionary'}
Reacting NH4ClO3 with NH4OH and HCL. It has niggling more particular, and for safety, I will aggrandize no more.
I tin see possible reaction mechanisms, producing AP + NH4Cl + NaCL + H2o.
Converting AP to HClO4, using HN03 + HCl, is an extensuion to the question.
If NG is 10 on the synthesis danger scale, how would you rate these reactions?

[Edited on iii-8-2011 by TitusGabonicus]

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hissingnoise

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Quote:
Reacting NH4ClO3 with NH4OH and HCL. It has niggling more than detail, and for prophylactic, I will expand no more.

Just as well, since ammonium chlorate is dangerously sensitive!
hissingnoise

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AP is prepared by two methods - metathesis with NaClO<sub>four</sub> and neutralisation of HClO<sub>4</sub>.
AndersHoveland

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One typically would desire to reduce out any trace of chlorates, using 20%HCl, before they add an ammonium salt to precipitate out the NH4ClO4, then as to avoid formation of any unstable ammonium chlorate.

Only you are asking what would happen if the ammonium chlorate was reacted with the HCl later. Do not really know.
Hydrogen peroxide actually preferentially attacks muriatic acid before it attacks ammonia. But mixing H2O2 and NH4OH volition not result in any firsthand reaction, whereas mixing H2O2 and HCl immediately results in formation of bubbles (vissible if 30% reactant concentrations are used). This demonstrates that nitrogen is a more than "electronegetive" element than chlorine, despite the fact that formation of diatomic nitrogen is oftentimes very favorable. It would not be possible for NH3 to burn in air if not for the formation of the strong N-Northward triple bond. (for comparison, HCl gas cannot burn in air on its own).

The reduction of chloric acrid past H2O2 has a very slow reaction rate unless heated, and then it may be that, if reacting NH4ClO3 with HCl, the ammonium ions will mostly be safety from directly oxidation. The only way to know for sure is to practice the reaction, and see if any (and how much) nitrogen gas results. Of course, the chlorine generated volition and so course some of the dangerous NCl3 with the ammonium ions!

ClO3[-] + (six)HCl --> Cl[-] + (three)H2O + (3)Cl2

The reaction forming nitrogen trichloride is actually an equilibrium reaction:
NCl3 + (4)HCl <==> NH4Cl + (three)Cl2

The formation of NCl3 is just favorable inside a sure pH range. Very low pH will prefer hydrolysis of NCl3. Alternatively, higher pH volition prefer formation of chloramine instead.
If there is any free ammonia in the reaction, nitrogen gas will tend to form rather than NCl3.

So, yes, such a reaction would potentially be very dangerous, considering some NCl3 would probable form in droplets at the bottom. If you practice the reaction, use a plastic container (non drinking glass which can shatter), wear protective middle goggles, and only experiment with very small quantities of reactants. Endeavor to keep your fingers away from the lesser of the container, where the NCl3 could collect, and maybe explode without warning.

[Edited on 3-viii-2011 past AndersHoveland]

I'm not saying let's go kill all the stupid people...I'chiliad just saying lets remove all the warning labels and let the trouble sort itself out.

Rosco Bodine

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Some serious fact checking should exist washed concerning but near every word in the above mail service by Anders Hoveland.
AndersHoveland

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All the to a higher place information has already been posted on this forum with references, simply here is the data again:

Here is the information most the equilibrium of NCl3:
http://books.google.com/books?id=QQkSAAAAIAAJ&pg=PA2178&...

The reaction between solutions of chloric acid (HClO3) and hydrogen peroxide does non have whatsoever appreciable reaction rate until a temperatures above 70degC. (note that perchlorate is not a reaction production in the decomposition reaction, although information technology may be likely that traces are formed). experiments conducted by Sand, published in Zelt phys. Chem.,50, 465 (year 1904)

A mixture of hydrogen peroxide and ammonium hydroxide (in a 1:three ratio) acts equally a reactive oxidizer, which tin attack organic compounds and elemental carbon. The reaction rate is negligible at room temperature, merely when heated to threescore°C the reaction becomes vigorous and self-sustaining. Such solutions are sometimes known every bit "base of operations piranha". With a 1:one:5 volume ratio of NH4OH, H2O2, and H2O, respectively, the half-life times of peroxide were 4 hours at fifty°C and 40 minutes at 80°C. "Reaction of Ozone and H2O2 in NH4OH Solutions and Their Reaction with Silicon Wafers" Japanese Journal Applied Physics. 43 (2004) pp. 3335-3339.

I'thousand not saying let's become kill all the stupid people...I'one thousand only saying lets remove all the warning labels and allow the trouble sort itself out.

Rosco Bodine

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Using an elevated temperature will be the best precaution against nitrogen trichloride formation and against ammonium chlorate formation Your observations about electronegativity are wrong. There is no appreciable reaction betwixt H2O2 and HCl. Frankly it is difficult to even understand how H2O2 is relevant to the topic. Some fact checking would be in order here because yous seem to exist all over the place with your response that is not really an answer to the question existence asked. The question being asked by the original poster relates to rating the danger of a reaction which does non have place ....therefore the original mail service is based upon a premise that is an oxymoron, to "rate the danger" of a reaction which does not occur.

Given that the reaction which is the premise for the question does not hold true,
then how can any of the answers not pointing that out be considered informed or intelligent answers?

[Edited on four-8-2011 by Rosco Bodine]

AndersHoveland

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Quote: Originally posted past Rosco Bodine
There is no appreciable reaction betwixt H2O2 and HCl. Given that the reaction which is the premise for the question does not hold truthful,
then how tin any of the answers not pointing that out be considered informed or intelligent answers?

Not true.
http://www.sciencemadness.org/talk/viewthread.php?tid=14490

oxidation by H2O2 was used equally a comparing to how acidified chlorate might react, whether it would adopt to oxidize chloride, or ammonium ions.

[Edited on 4-8-2011 by AndersHoveland]

I'm not proverb let'south go kill all the stupid people...I'm just saying lets remove all the warning labels and let the trouble sort itself out.

Rosco Bodine

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Hilarious ......you give yourself as a reference. This is similar answering the question "which came first, the chicken or the egg?" by saying in answer
"It isn't about which came first, but more virtually the number of fertile eggs
appearing simultaneously at the moment of cosmos of laying hens, provided by the Lord as a chore for them to do of sitting on the nest when not pecking corn"

Obviously, God did not want chickens to suffer from colorlessness. :D

Past the way, recompiling my words out of context is a really neat trick .....but it is deceptive in that it obscures the pregnant of what I said. Hey Anders, virtually of us here reside on a planet called Earth. If not too much trouble, could you please join us here and knock off the B.S. with off the cuff misinformation and pseudoscientific jibberish which but keeps getting you caught at every plow? You are too often speaking authoritatively and incorrectly in what you are saying.

[Edited on 4-viii-2011 past Rosco Bodine]

AndersHoveland

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Quote: Originally posted by Rosco Bodine
Hilarious ......you lot give yourself as a reference. This is like answering the question "which came first, the chicken or the egg?"

By the way, recompiling my words out of context is a really bang-up trick .....but information technology is deceptive in that it obscures the meaning of what I said. Hey Anders, could you knock off the B.S. with off the cuff misinformation and pseudoscientific jibberish which just keeps getting y'all caught at every turn?

What are you talking about? Yes, the link refered to one of my prior posts, but references were given in that postal service for the reaction of H2O2+HCl.
(Livingston and Bray, J. American Chem. Order, Book 47, p2069 (1925) and "Oxidation of Hydrogen chloride with hydrogen peroxide in aqueous solution" V.I. Skudaev, A.B. Solomonov)

It can be seen on the Pauling electronegativity calibration that nitrogen (value of iii.04) has almost the aforementioned value every bit chlorine (3.xvi). http://www.tutor-homework.com/Chemistry_Help/electronegativi...
Of course, these values to practise non correlate to how the elements will behave in all reactions, or what their chemical reactivities at ordinary temperatures are, but it is at least somewhat indicative.

From two of the above mentioned reactions, it would seem that hydrogen peroxide more readily oxidizes hydrochloric acid than ammonia. But of course, the chlorine which forms gets reduced back every bit fast as information technology forms.

References accept been provided for all the reactions that were mentioned. If in that location are any other reactions that you would like to have references for, but ask.

Certainly was not trying to be deceptive or misquote yous. How do yous fifty-fifty perceive that?

[Edited on five-8-2011 past AndersHoveland]

I'k not saying let'due south go kill all the stupid people...I'm merely maxim lets remove all the alert labels and permit the trouble sort itself out.

Rosco Bodine

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You recompiled my words to misquote me as if H2O2 was the issue instead
of an original post that was most a reaction which isn't a reaction.

You are yet beating the dead horse H2O2 aspect which is irrelevant.
And I did non say there was no reaction.....I said at that place was no appreciable reaction, every bit in no significant reaction ratewise or otherwise readily apparent.
You lot are non speaking in terms of applied reaction schemes or rates as
would be applicable to a realistic process, if the presumed reaction of the original post was valid and relevant ....which it is not.

Everything that follows and derives from that incorrect premise is revealing.

If y'all think you elevate yourself to post a hate blog confronting me have at it,
if you desire to descend to a new low. You accept come here to a forum where intelligent people try to bear on intelligent discussions which are based in real science fact, and yous take a cavalier tone towards readers of this forum as if you were somehow the knowledgeable professor, but what y'all say is not of a quality which bears out the presumption you conspicuously have almost the vastness of your own knowledge. Consequently y'all often state things that are just apartment wrong and it is unscientific and certainly unprofessional. If y'all read a periodical commodity with some comprehension, you lot then accept behemothic leaps in estimating the telescopic of your own knowledge and information technology plainly shows. I don't want to argue with
you. I would just inquire that y'all stop posting a lot of things that you lot don't know just only call up without any differentiation between the two. The decorum around here is not rigid with regards to discussion, only this is a scientific discipline forum not an annihilation that can be imagined should be posted for fact kind of weblog, where information technology then becomes the task of the residue to scratch their heads and wonder how much is truth or fiction.

AndersHoveland

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Question for TitusGabonicus,
just to analyze, did the entry in 'Hawley's Chemical Dictionary' specifically say that reacting NH4ClO3 with NH4OH and HCL would make ammonium perchlorate?

It does not seem like any perchlorate would be formed, but cannot exist completely sure.

[Edited on 5-eight-2011 by AndersHoveland]

I'yard not saying permit'due south go kill all the stupid people...I'm just proverb lets remove all the warning labels and let the trouble sort itself out.

Rosco Bodine

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Exactly.
TitusGabonicus

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The 'Hawley edition' of 35 years ago, reads equally does its11th..edition.(1984)
Derivation: (Re. NH4ClO4): Interaction of ammonium hydroxide, hydrochloric acid and sodium chlorate. Recovery by crystallizatuion.
Sounds scary, its true. I therefore am questioning the accuracy of this procedure. Information technology may be an fault? Thus, I placed it to yous, to evaluate its validity. Thank you.
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Quote: Originally posted by TitusGabonicus
The 'Hawley edition' of 35 years ago, reads as does its11th..edition.(1984)
Derivation: (Re. NH4ClO4): Interaction of ammonium hydroxide, hydrochloric acid and sodium chlorate. Recovery past crystallizatuion.
Sounds scary, its true. I therefore am questioning the accurateness of this procedure. It may exist an error? Thus, I placed it to you, to evaluate its validity. Thank you.

Welcome. Overnice first post. I'm glad you used documented source & it is a question many would have, were they to read the synthesis as presented.
Would yous happen to have a scan or copy of the exact synthesis? {Are yous sure of the typed example?} Did the material mention temperature(s) command of the process? And / or control of reactions w/ hydroxide?

I recollect we're all on the same page in so far as the unsafe nature of ammonium chlorate (in situ or non) during this synthesis only did the author delve into methods to control the reaction, or caveats regarding manipulation so as to place a level of control therein? Was any further background given? Occasionally broadly expressed methods are used as ways of learning inapplicable bug & not as synthesis practicum.

NOTE: Often material available in the Great britain is tough to find in the USA, particularly if yous're looking at classroom text.

dann2

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Information technology'southward simply an error in the volume. Jade Ledgard mush have been reading it too............

http://oxidizing.110mb.com/chlorate/further/cep1957/cep1957....
http://oxidizing.110mb.com/chlorate/further/cep1961/cep1961....

Ammomium Hydroxide + HCl gives Ammonium Chloride + water.
Ammonium Chloride + Sodium Perchlorate (non Chlorate!) gives NaCl + Ammonium Perchlorate (all in water solution)
Crops of Ammonium Perk, must be crystallized out of the solution. Crops of NaCl will also exist taken out at the proper times (continous product).

Dann2

[Edited on 16-viii-2011 by dann2]

AndersHoveland

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Yes, information technology is to be strongly suspected that the book made a error. Ammonium chlorate is more than probable to result from this procedure, assuming excess HCl is not used.

I'm not saying allow's go kill all the stupid people...I'm just saying lets remove all the warning labels and allow the problem sort itself out.

TitusGabonicus

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I likewise, think it is an error.
Hawley has been i of my 'desert island books', for many years.
Information technology is a marvellous text, only yous could still lose fingers, lest you lot triplecheck reactions from ANY source. To the lowest degree of all when dealing with (per)chlorates.
My thanks to those who contributed.
If 'Hawley' has any comment, I'm sure it would be well received.
Hennig Make

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This is from the same website that dann2 linked to, very adept website. It has a method for making ammonium perchlorate starting with the commonly bachelor potassium perchlorate. Information technology seems similar information technology would work, and not be all that hard either. Ammonium sulfate is a very common/cheap fertilizer which is easily obtained.

I made 500g of potassium perchlorate with the help of that website over a twelvemonth ago. I like that website.

Attachment: Ammonium Perchlorate from Potassium Perchlorate.docx (15kB)

This file has been downloaded 1740 times

Edit:
After reading the thread a bit more than carefully I realize I am non really on topic. I will leave it anyway, as I call up it is interesting.

[Edited on 21-8-2011 by Hennig Brand]

dann2

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@HB
Terminate, stop you making me chroma FFS!!!!!!!!!
Hennig Brand

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Sad about that. Y'all blush easily do you?:D

And then that is your website then. I was never 100% sure, simply I did get the impression that you were somehow continued to it. Well, if it makes you uncomfortable I'll lay off the compliments, simply it still is a nice collection of data on the topic.

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It would be a practiced topic for my next coursework. I'll learn more than about it and will get-go to write with some service'southward aid.
Laboratory of Liptakov

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NH4ClO4
Ammonium Perchlorate from Potassium Perchlorate.docx ( 15kB) Ane from best data about NH4ClO4 preparation always. Genious method.

Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015, inventor CHP and Lithex

Ammonium Perchlorate And Sodium Hydroxide,

Source: https://www.sciencemadness.org/talk/viewthread.php?tid=17185

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