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Author: Subject: Alternative Methods of Deacidification of Nitric Esters
freedompyro
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[*] posted on 15-7-2011 at 13:13
Alternative Methods of Deacidification of Nitric Esters


This is really starting to annoy me... I ran 50g NG with 2000ml 5% Sodium Bicarbonate solution starting at 40C for three hours with a water stirring setup. (Flat paddles running at 3RPS on top of the water.) With a drop of soap to prevent floaties. The NG would stay swirling at the bottom only reaching an inch and a half from the bottom.

It turns out that didn't deacidify it... Trying again the exact same way except starting with 90C water and remotely activating the stirring setup. Other details that might be important... NG was synthesized with 95% HNO3 slightly RFNA (Around 1% oxides) and Rooto. That might be the problem... Maybe soda ash is better than bicarbonate...

Is there any other ways to do this? Will sodium carbonate or sodium bicarbonate dissolve in acetone so that you can just dissolve it all in acetone and instantly neutralize it that way... Then evaporate.

If not I'm just going to leave it in the water with the agitator running for like three days... See if that does it!

[Edited on 15-7-2011 by freedompyro]
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[*] posted on 15-7-2011 at 13:48


Realistically 3 hours may simply not be enough time to achieve neutralization. But there may be another reason if you see NO diminishment of pH.

The issue MAY be involved with surfactant inhibitions where the base (anti-acid) is not reaching the ester. Your surfactant is the soap obviously.
A surfactant or surface active agent is a substance that, when dissolved in water, gives a product the ability to remove dirt from surfaces such as the human skin, textiles, and other solids. However surfactant models might prevent contact with the ester. Ordinarily a saturated solution of both saline and an anti-acid is exposed to the material. The salt prevents the ester from absorbing water, while the anti-acid does it's work & neutralizes.

It is a possible that this is an issue of surfactant chemistry. Honestly I am not up on that issue. However exposure to the bicarbonate should neutralize the material. It would not make a great deal of difference what the base is, a carbonate, bicarbonate, etc. Something may be preventing contact. The surfactant may also be absorbing the anti-acid, rather than preventing it from contact. Hopefully someone with a bit of background in this area of chemistry will chime in because, frankly, that is odd. If you see no alteration of pH in 24 hours then the likelihood is that it's not going to neutralize.


Disclaimer:
I am simply drinking coffee and guessing at this. Ordinarily I would put a solid 5% as low but provided the anti-acid is in solution, 5% should show some marginal neutralization. Are you using a method of accurately displaying the alteration of pH? IF this is a digital meter - yes I would say it's fairly odd as you should see some alteration. but if this is a case of test strips and the color difference is slight then you need to give this some time.
Surfactant chemistry is very interesting & I wish I knew more. It would be a very useful area to study. Generally in a neutralization it's a more productive thing to use a saturated solution of the base but if 5% is all that would go into solution, so be it. There are more soluble bases that bicarb.



[Edited on 15-7-2011 by quicksilver]




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freedompyro
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[*] posted on 15-7-2011 at 14:24


It was only one drop of soap. It was suggested to me a while back to break surface tension and prevent floating NG droplets.

There was a reduction in PH over the first three hour run, however litmus still turned red when dipped in NG... Also, after placing a few grams in a jar with a desiccant suspended over it the smell was horrible after a day confirming the acidity breaking down the NG. However the NG was still clear to slightly yellowish.

Was thinking there was something wrong with my PH test strips and had to confirm, but nope... They are accurate. LoL! (They are tongue PH test strips for checking your own acid balance.)
http://www.swansonvitamins.com/SWB001/ItemDetail

Edit: Update... After the 90C solution with the NG cooled down over an hour the NG now very slightly darkens the color of the yellow litmus toward green. The solution itself turns the paper vivid dark blue.

I'm not exactly sure how safe and sensitizing that temperature is on NG...

The maximum concentration of bicarbonate that is practical is 9% around room temperature according to Wikipedia. Can I just dissolve as much as possible and will that prevent the NG from absorbing water or does it need salt dissolved in it too?

[Edited on 15-7-2011 by freedompyro]
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[*] posted on 15-7-2011 at 20:17


I discovered that I can convert sodium bicarbonate to sodium carbonate through heating and that I can make a 21% solution at room temperature of sodium carbonate in water.

Would this 21% sodium carbonate solution be twice as effective at deacidification as the 9% sodium bicarbonate solution or is carbonate a weaker base?

Sodium Carbonate > Basicity (pKb) 3.67

Sodium Bicarbonate > Basicity (pKb) 3.671

Oh... Interesting... Converted Sodium Bicarbonate pKa to pKb and it's the same as Carbonate... It seems carbonate is THAT much better!

I wonder if Sodium Hydroxide would be a suitable neutralizer... Enough of it sure dissolves in water... LoL!

[Edited on 16-7-2011 by freedompyro]
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[*] posted on 16-7-2011 at 03:03


checking meglomanias instructions he recommends first washing it several times with sodium carbonate, and then letting it sit a day in a concentrated sodium chloride solution. Maybey that will help a bit.
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[*] posted on 16-7-2011 at 08:20


Quote: Originally posted by freedompyro  


I wonder if Sodium Hydroxide would be a suitable neutralizer... Enough of it sure dissolves in water... LoL!


Theses are exactly the experiments that should be documented as best you can. You need not utilize several grams of energetics per se' for such a thing. You could work with a one gram unit per test design. The example of sodium hydroxide solution could be made relativity safe & fascinating simply by percentage solution exposure, understanding the initiation issues and reducing the energetic to a sub-gram level w/ shielding, etc

Example of notes (title, data, & so forth:


Experimental: Neutralization of liquid nitric ester via exposure to varied basic solutions.

Nitric Ester format: NG (starting pH level: )

Base Type / Exposure time tables:

Solution sodium carbonate 5% .

Sodium carbonate saturated solution (percentage water),

Ammonium hydroxyde 10%

{Cont'd on with what you would use.}


Time of exposure:Hours:

Results in Start / End pH level:


Comments:
_____________



Notes such as those get to be worth your time as you professionalize your experiments. Without notes, you really won't remember a great deal of chemistry years down the road. The fact that energetic chemistry is also a serious safety issue allows those notes to maintain certain safety / exposure issues that are also very easily forgotten 5-10 years later. (You can also encrypt them) I have large volume of notes from roughly 15-20 years ago that have some fairly interesting things. It's a very important habit to get into. Actually, I have some material that eventually became very rewarding.



[Edited on 16-7-2011 by quicksilver]




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