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PHILOU Zrealone
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[*] posted on 16-11-2015 at 15:41


Quote: Originally posted by dangerous amateur  
Yes I know, until it's neutral.

But how many steps does it usually take for you to get it 100% neutral?

I usually wash it with sodium carbonate solution first, then with additional water.
Then I recristallize it from ethanol.

I cannot find any acid detectable with ph strips.

However, would you recristalize a second time?


The following links are related:

ETN crystalization 1

ETN crystalization 2


[Edited on 16-11-2015 by PHILOU Zrealone]




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[*] posted on 21-11-2015 at 03:37


Are NG and EGDN storage stable for a long time like PETN or RDX ?
Also do NG and EGDN evaporate ?

[Edited on 21-11-2015 by underground]
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[*] posted on 21-11-2015 at 04:26


I think I have heard of people storing pure NG before.
According to COPAE, the inventor of nitroglycerin, Sobrero, stored a sample of nitroglycerin he prepared in 1847 and washed it with bicarb solution and took it to the Nobel factory many years later in 1886.
The pure liquid explosive is never going to be storage and handling stable like PETN and RDX unless you make a dynamite out of it but even then there is the risk of sweating and causing a dangerous to handle product.
In my opinion, you would want to wash it extremely well to make it as free from acid as possible and probably store it in the dark in a cool place. Repeated periodical washings with sodium bicarbonate solution would probably be needed as well. Even better you might be able to store it dissolved in acetone or another solvent that it is miscible with, but I honestly would turn it into dynamite if I wanted to store it and store the sticks.

As for the evaporation question, the high vapour pressure of NG would mean that it does evaporate I am sure.
Correct me anyone if I am wrong.


[Edited on 21-11-2015 by greenlight]




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[*] posted on 21-11-2015 at 07:39


EGDN evaporates but not too quickly, not nearly as fast as water anyway.
In my experience NG evaporates very slowly, to the point of being entirely insignificant for just about purpose.

That would suggest vapor pressure and volatility aren't strictly related which goes against everything I've been taught and understand about the subject.

Are you sure it has a high vapor pressure? High in relation to what?

Edit... I couldn't find the vapor pressure of NG but EGDN is only 0.05 mmhg which is much lower than water.


[Edited on 21-11-2015 by OneEyedPyro]
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PHILOU Zrealone
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[*] posted on 21-11-2015 at 10:25


I have read (info stored in my memory) that a NG sample from one of Sobrero's initial synthesis is stored for more than a century now in Italy.



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[*] posted on 21-11-2015 at 15:22


I was wondering if there is any liquid HE that it is not going to evaporate so we can use it for plasticizer
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[*] posted on 21-11-2015 at 17:39


I think it is better to store NG in a bicarbonate solution. this would automatically remove any acid generation.
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[*] posted on 21-11-2015 at 19:55


Quote: Originally posted by OneEyedPyro  
EGDN evaporates but not too quickly, not nearly as fast as water anyway.
In my experience NG evaporates very slowly, to the point of being entirely insignificant for just about purpose.

That would suggest vapor pressure and volatility aren't strictly related which goes against everything I've been taught and understand about the subject.

Are you sure it has a high vapor pressure? High in relation to what?

Edit... I couldn't find the vapor pressure of NG but EGDN is only 0.05 mmhg which is much lower than water.


1`[Edited on 21-11-2015 by OneEyedPyro]


Yes, it doesn't make sense. I think that I was wrong and NG is sensitive to initiation because of the vapour pressure in the liquid explosive causing the formation of microscopic bubbles. I do not think that it is a high vapour pressure though.
If it had a high vapour pressure it would evaporate quickly and as someone stated, the evaporation rate of nitroglycerin is barely noticeable.

[Edited on 22-11-2015 by greenlight]




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[*] posted on 22-11-2015 at 03:59


Quote: Originally posted by underground  
I was wondering if there is any liquid HE that it is not going to evaporate so we can use it for plasticizer


The evaporation rate of NG is entirely insignificant, even EGDN which is noted for being far more volatile than NG is still nearly 100 times less volatile than water, I'd guess NG is several hundred times less volatile than water.
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[*] posted on 22-11-2015 at 04:12


so why we have headache when we synthesis NG ? I think it is faster than water
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[*] posted on 22-11-2015 at 05:12


Chances are the headache you get from synthesizing nitroglycerin are from accidental skin contact, fumes during the nitration, or washing the glassware afterwards.

[Edited on 22-11-2015 by greenlight]




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[*] posted on 22-11-2015 at 05:16


Quote: Originally posted by greenlight  
Chances are the headache you get from synthesizing nitroglycerin are from accidental skin contact, fumes during the nitration, or washing the glassware afterwards.

[Edited on 22-11-2015 by greenlight]

not true , from wiki :


Quote:

Industrial exposure[edit]
Infrequent exposure to high doses of nitroglycerin can cause severe headaches known as "NG head" or "bang head". These headaches can be severe enough to incapacitate some people; however, humans develop a tolerance to and dependence on nitroglycerin after long-term exposure. Withdrawal can (rarely) be fatal;[27] withdrawal symptoms include chest pain and heart problems and if unacceptable may be treated with re-exposure to nitroglycerin or other suitable organic nitrates.[28]
For workers in nitroglycerin (NTG) manufacturing facilities, the effects of withdrawal sometimes include a "Sunday Heart Attacks" in those experiencing regular nitroglycerin exposure in the workplace, leading to the development of tolerance for the vasodilating effects. Over the weekend, the workers lose the tolerance and, when they are re-exposed on Monday, the drastic vasodilation produces a fast heart rate, dizziness, and a headache, this is referred to as "Monday Disease."[29][30]
People can be exposed to nitroglycerin in the workplace by breathing it in, skin absorption, swallowing it, or eye contact. The Occupational Safety and Health Administration (OSHA) has set the legal limit (permissible exposure limit) for nitroglycerin exposure in the workplace as 0.2 ppm (2 mg/m3) skin exposure over an 8-hour workday. The National Institute for Occupational Safety and Health (NIOSH) has set a recommended exposure limit (REL) of 0.1 mg/m3 skin exposure over an 8-hour workday. At levels of 75 mg/m3, nitroglycerin is immediately dangerous to life and health.[31]
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[*] posted on 22-11-2015 at 05:29


It says that "people can be exposed to nitroglycerin in the workplace by breathing it in (fumes during nitration or washing glassware in hot water from steam), skin absorbtion (accidental skin contact), swallowing it or eye contact (slightly more unusual)".
So the nitro headache would be caused during synthesis.
It does have to touch the skin, eyes or be breathed in or ingested.

[Edited on 22-11-2015 by greenlight]




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[*] posted on 22-11-2015 at 05:33


:D you are correct greenlight
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[*] posted on 22-11-2015 at 05:36


:)haha I was wondering what you meant.



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[*] posted on 22-11-2015 at 16:48


Does actually exist any liquid HE that is not going to evaporate as i said befor ?
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[*] posted on 23-11-2015 at 01:09


What about nitration of glucose
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[*] posted on 23-11-2015 at 05:08


After tracking down a vapor pressure of NG and double checking my math I take back what I said.

EGDN is 350 times less volatile than water and NG is 437 times less volatile than water.
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[*] posted on 23-11-2015 at 10:34


EGDN and NG are not strictly speaking volatile... just a little; otherwise, cold under reduced pressure evapo-condensation would be an option to purify those.

The presence of microbubbles doesn't come from the liquid itself, but from dissolved gases (or volatiles fluids) that expel themselves from the liquid as the temperature increases.
Depending on the affinity of the two compounds for each other, if one is more volatile and has no strong affinity for the major phase, the major phase tends to gather it and to push it out (see lowering of the boiling point).

The main problem with EGDN and NG (and of other nitrous or nitric esters) is that their effect on blood pressure is very strong even at very low doses...so even if the volatility (evaporation or fog dispersion of micro-dropplets) is low the effect is immediate on the human body...

Some liquids HE are absolutely non-volatile (just note that like for unsolubility - nothing is really unsoluble and as a slight solubility; so everything is volatile to some extend ... even cold iron at ambiant T° ;)).
--> Hint do a search on ionic liquids...

Nitration of glucose...has been discussed a few times on this forum... search with the search engine eventually with the keywords "glucose or suggar nitration, nitrosuggar, nitro-suggar, nitroglucose" ;)

[Edited on 23-11-2015 by PHILOU Zrealone]




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[*] posted on 23-11-2015 at 12:15


PHILOU Zrealone can you just name some of those absolutely non-volatile HEs ?

[Edited on 23-11-2015 by underground]
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[*] posted on 23-11-2015 at 15:08


Quote: Originally posted by underground  
PHILOU Zrealone can you just name some of those absolutely non-volatile HEs ?

[Edited on 23-11-2015 by underground]

Google Search --> Ionic Liquid Explosives
--> Link
p 17
AMT-ONT
1-AMTN --> US Patent 7,645,883

This is just the spirit of it once you understand what is an ionic liquid, you understand why it will not be volatile!




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[*] posted on 24-11-2015 at 06:19


Can nitration of erythritol be done by mixing it with AN and slowly add the H2SO4 ?
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[*] posted on 24-11-2015 at 07:30


Quote: Originally posted by underground  
Can nitration of erythritol be done by mixing it with AN and slowly add the H2SO4 ?


it work but avoid it.
you will have a lot of heat generated and you will not be able to control it easily.

H2SO4 + AN => generate heat
Nitric acid + Erythirtol => generate heat.

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[*] posted on 24-11-2015 at 07:37


Quote: Originally posted by underground  
Can nitration of erythritol be done by mixing it with AN and slowly add the H2SO4 ?


That would make temp control impossible almost regardless of how slowly you do the addition since the acid and AN would liberate lots of heat on contact without much mass to absorb it or rather without an efficient way for that heat to be dispersed throughout the mass.

You can dissolve erythritol in the acid then slowly add AN with stirring being careful to maintain the temperature. This is actually a very good method since it allows you to easily keep the mixture at the desired temp.


[Edited on 24-11-2015 by OneEyedPyro]
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[*] posted on 24-11-2015 at 10:36


The dissolved erythritol into acid (sulfuric or nitric acid) can be storage stable over time at room temp ? I am trying of making a semi-automatic setup for nitration.
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