Sciencemadness Discussion Board

Improving process of someone

plante1999 - 2-2-2013 at 11:59

Lately I did a fast experiment. The objective was to keep the use of the chemicals used in nurdrage video, but get higher yield. And hopefully purer product. I did a process to improve his potassium nitrate at home video, and I got a quantitative yield based on KCl, and 93% based on NH4NO3. My product is non-contaminated by any volatile impurity. This process may be quite dangerous, but the yield is very high. Also it might be good to know that I did this to use my remaining ammonium nitrate.

His video:
http://www.youtube.com/watch?v=xOjtlIxYYbs

My page
http://hclo3.weebly.com/make-potassium-nitrate-kno3.html

[Edited on 2-2-2013 by plante1999]

kavu - 2-2-2013 at 12:38

Quote: Originally posted by plante1999  
I got 100% yield based on KCl


There is no such thing as a 100% yield. Given your experimental error you could state that the yield is quantitative but not 100%. Also you have to determine your yield according to the amount of limiting reagent (in this case that would be the chloride). This is a general consideration in all synthetic publishing.

How did you determine the purity of the final product, the burning test itself is not very efficent. It would be nice to check the product with AgNO3 for chloride contaminants. Ammonium ion could be checked with ammonia tests.

[Edited on 2-2-2013 by kavu]

plante1999 - 2-2-2013 at 12:46

Quote: Originally posted by kavu  
Quote: Originally posted by plante1999  
I got 100% yield based on KCl


There is no such thing as a 100% yield. Given your experimental error you could state that the yield is quantitative but not 100%. This is a general consideration in all synthetic publishing. How did you determine the purity of the final product, the burning test itself is not very efficent. It would be nice to check the product with AgNO3 for chloride contaminants.

[Edited on 2-2-2013 by kavu]


Chloride test would be really important, I will test the soonest possible. I only have a gram of AgNO3 tough. I fixed the 100% in the first post, it may take longer to fix on the website.
I did test for ammonium using tincture of iodine solution of mercury. The test was negative for ammonium.


[Edited on 2-2-2013 by plante1999]

blogfast25 - 2-2-2013 at 14:54

One of the best and cheapest tests for ammonia is... your nose! Take a significant pinch of your product and mix it with KOH or NaOH and a little water, in a test tube. Strongly heat and carefully assess for NH3 fumes.

For Cl-, Pb nitrate is fairly sensitive and AgNO3 may be a bit too sensitive, as you'll find traces of chlorides in a lot of things...

plante1999 - 2-2-2013 at 15:22

I would test with Pb nitrate, but my supplier forgot it in the package! If the tincture of mercury do not test it, I would not sniff it. I tested my reagent with a so dilute ammonia solution, that I was not able to smell anything, and yet, the test was clear.

Mailinmypocket - 2-2-2013 at 15:32

Just wondering... What is a tincture of iodine solution of mercury?

plante1999 - 2-2-2013 at 15:50

http://en.wikipedia.org/wiki/Potassium_tetraiodomercurate(II)

A very interesting reagent.

Lambda-Eyde - 2-2-2013 at 15:50

Quote: Originally posted by Mailinmypocket  
Just wondering... What is a tincture of iodine solution of mercury?

It's more commonly known as [url=http://en.wikipedia.org/wiki/Nessler's_reagent]Nessler's reagent[/url] or potassium tetraiodomercurate(II).


Edit: Why the FUCK won't that BBCode work? Please don't tell me that it freaks out from URL's with apostrophes in them........

[Edited on 2-2-2013 by Lambda-Eyde]

Mailinmypocket - 2-2-2013 at 15:54

Quote: Originally posted by Lambda-Eyde  
Quote: Originally posted by Mailinmypocket  
Just wondering... What is a tincture of iodine solution of mercury?

It's more commonly known as [url=http://en.wikipedia.org/wiki/Nessler's_reagent]Nessler's reagent[/url] or potassium tetraiodomercurate(II).


Edit: Why the FUCK won't that BBCode work? Please don't tell me that it freaks out from URL's with apostrophes in them........

[Edited on 2-2-2013 by Lambda-Eyde]


Ahhh yes, okay gotcha. I had just never heard that term before and when I searched all I was finding were results for mercurochrome. I think I had a bottle of nesslers reagent in an ammonia test kit for aquariums a long time ago.

watson.fawkes - 12-2-2013 at 10:09

Quote: Originally posted by Lambda-Eyde  
It's more commonly known as [url=http://en.wikipedia.org/wiki/Nessler's_reagent]Nessler's reagent[/url] or potassium tetraiodomercurate(II).

Edit: Why the FUCK won't that BBCode work? Please don't tell me that it freaks out from URL's with apostrophes in them.
I won't tell you that the board software freaks out, because I don't believe it has emotions, much less sentience, but it does fail on them. Replace the apostrophe character with its URL-escape code, %27, as such: http://en.wikipedia.org/wiki/Nessler%27s_reagent. Ironically for the complaint, the Wikipedia page redirects to a page with a punctuation-free title.

Random - 12-2-2013 at 12:41

Quote: Originally posted by blogfast25  
One of the best and cheapest tests for ammonia is... your nose! Take a significant pinch of your product and mix it with KOH or NaOH and a little water, in a test tube. Strongly heat and carefully assess for NH3 fumes.

For Cl-, Pb nitrate is fairly sensitive and AgNO3 may be a bit too sensitive, as you'll find traces of chlorides in a lot of things...


every time when i heated urea in test tube my eyes started watering and i had no sense of smell

Meakanesis - 18-3-2013 at 09:55

Quote: Originally posted by Random  
Quote: Originally posted by blogfast25  
One of the best and cheapest tests for ammonia is... your nose! Take a significant pinch of your product and mix it with KOH or NaOH and a little water, in a test tube. Strongly heat and carefully assess for NH3 fumes.

For Cl-, Pb nitrate is fairly sensitive and AgNO3 may be a bit too sensitive, as you'll find traces of chlorides in a lot of things...


every time when i heated urea in test tube my eyes started watering and i had no sense of smell


Nice to know :P, personally wouldn't sniff a vigorously heated tube filled with anything+naoh my experience with lye is great and to be frank i hate it, it makes me paranoid and i have to say vinegar is my best friend when dealing with it. Nice thread though even if i have nothing but a safety complaint to add.

woelen - 19-3-2013 at 00:07

Why would you want to make KNO3 this way? If you have NH4NO3 then you can also use K2CO3 or KOH in aqueous solution and simply evaporate the water. You drive off ammonia (and CO2 if you use K2CO3) and what remains behind is KNO3. Use a slight excess of NH4NO3. A single recrystallization allows you to make very pure KNO3, becauseiIn cold water, KNO3 is much less soluble than NH4NO3.

plante1999 - 19-3-2013 at 00:12

You didn't understood the idea, I was improving the process of someone, using the same reagent as he did.

AndersHoveland - 19-3-2013 at 01:36

Why try to improve what already works?

There are plenty of other theoretical reactions proposed by various members (cough, cough) that no one has ever tried.

plante1999 - 19-3-2013 at 03:48

Quote: Originally posted by AndersHoveland  
Why try to improve what already works?

There are plenty of other theoretical reactions proposed by various members (cough, cough) that no one has ever tried.


To make it work better! That's how I think, and it is probably the required thinking for an indutrial chemist like I want to be.

And I already got permanent chemistry scars, it is well enough if the other member can understand.

woelen - 19-3-2013 at 04:31

Quote: Originally posted by plante1999  
You didn't understood the idea, I was improving the process of someone, using the same reagent as he did.
Yep, I understand. Sometimes it is fun to make or try something, using a specific process or to improve a specific process. For the same reason I have made certain chemicals, just for the fun of making them and being able to make a nice picture of these chemicals (e.g. K3CrO8, CsBr3, SeBr4).

AndersHoveland - 19-3-2013 at 14:10

See if you can get this reaction to work:
Quote:

"Also, nitrosyl chloride is produced by the action of chlorine on sodium nitrate...

NaNO3 + Cl2 --> ClNO + NaClO2

Handbook of Inorganic Chemicals, Pradyot Patnaik
http://site.iugaza.edu.ps/bqeshta/files/2010/02/94398_16.pdf

I am not sure if it is true, or how reliable the source is. I suppose it could be possible, but my intuition tells me it is probably not so easy. At the very least, I am sure the NaNO3 solution would have to be completely saturated with chlorine for the reaction to be able to proceed.

gasapparatus.jpg - 214kB

(chlorine could be made by reacting bleach + hydrochloric acid)

[Edited on 19-3-2013 by AndersHoveland]

madscientist - 28-3-2013 at 05:12

Quote: Originally posted by AndersHoveland  
Why try to improve what already works?

There are plenty of other theoretical reactions proposed by various members (cough, cough) that no one has ever tried.


I assume you're talking about your own ones - if so, I'm sure glad they haven't.