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Author: Subject: nitroglycerin
Zinc
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[*] posted on 16-1-2011 at 12:05


I washed the NG with an another portion of conc. NaCl soln. and transported it with a syringe into a measuring cylinder. Final yield is 23.5 ml, much more than I thought. A few ml were lost during washing, so it is possible that the yield was over 25 ml. Also I doubt that there is acetone left from the neutralization, the NG has a weak smell, I believe if there is some acetone left, the smell would be much stronger.

Almost all of the bubbles were removed by the final washing and during transportation from the jar to the measuring cylinder. Although a small amount of some powder like material remained on the surface of NG, perhaps some salt (a small amount of water could have evaporated from the NaCl soln. causing some NaCl to precipitate), but the quantity is extremely small (I don't think it is more than a few mg).

Also I have tested it again with litmus paper, it is still neutral :D




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[*] posted on 21-1-2011 at 11:04


Sorry for the double post, and if the question is too "practical".

I was thinking about trying NG/DNT mixture (perhaps with some paint grade Al powder), and I know NG mixtures often contain a small amount of CaCO3 to neutralize any acid that may be in the mix.

As I don't have access to pure CaCO3, and don't like the idea to use impure ground rocks, could perhaps NaHCO3 be used instead of it?

I believe that NaHCO3 is a stronger base than CaCO3, and that it can react with AN quite easier than CaCO3 (to form NaNO3 and ammonium bicarbonate, that easily decomposes to NH3 and CO2), so is perhaps that the reason that it isn't used (at least I didn't find any information on it being used)?

As the NG/DNT (perhaps some Al) doesn't contain AN, could NaHCO3 be safely added (perhaps 1-2 %) to the mixture?

And I know that Al can react with bases, but I don't think that NaHCO3 is a strong enough base to penetrate the Al2O3 layer on the surface of the Al (and my Al seems to be coated with some form of resin or "plastic", don't know how much of that is on it) especially if it is so "diluted" with NG and DNT.




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[*] posted on 21-1-2011 at 14:15


Why don't you just make some CaCO3? Surely you must have access to a soluble calcium salt (CaCl2 or maybe Ca(NO3)2). Then just combine the solutions with stirring and if it doesn't precipitate right away (depending on the exact nature of the salts you may get a gel at first) just keep stirring (or boil the mix) until you get a suspension of fine precipitate. Filter, wash, dry.
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[*] posted on 22-1-2011 at 10:32


Honest answer: Is it really so dangerous when I stir with a glass thermometer that it even could explode? :o:(
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[*] posted on 22-1-2011 at 11:16


I've stirred the reactants with a thermometer on a few occasions but I'll not do it again!
When it comes to nitro you can't be too careful . . .

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[*] posted on 22-1-2011 at 12:00


http://img11.imageshack.us/i/15129161.jpg/

http://img812.imageshack.us/i/43034.jpg/

I have no problems with this setup. The “addition funnel” is very handy, because you can mesure the alcohols directly in the syringe.

[Edited on 22-1-2011 by Jimbo Jones]
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[*] posted on 24-1-2011 at 03:24


Yesterday I tried to set off a mix of 40g DNT, 30g NG and 5g paint-grade Al powder and cca. 1g of NaHCO3 (I don't know how safe it is to use NaHCO3 instead of CaCO3, but as the time from mixing to the time of detonation was only around 1.5 h I took the risk). When prepared the mixture is a very dense and viscous shiny liquid.

Unfortunatley, I had no better primary than MEKPAP/AN.

My MEKPAP was contaminated with unreacted acetone/MEK, so it wouldn't DDT alone in a small glass test-tube (volume 5 ml), forcing me to mix it with AN and put it in a small plastic bottle (the bottle is 15 ml, filled with cca. 2.5g of AN and 4 ml of MEKP/AP). Even then it detonated quite weak compared to pure MEKPAP/AN, but I thought that as the mix contains so much NG it would be enough.

Well it wasn't and the mix went low-order. I know that the VOD at wich NG detonates is very dependent on the strenght of the detonator, but as I didn't have anything else, and didn't want to store the NG/DNT/Al mix I used what I have.




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[*] posted on 25-1-2011 at 10:18



Quote:

I've stirred the reactants with a thermometer on a few occasions but I'll not do it again! When it comes to nitro you can't be too careful . . .


Again, glyceryl trinitrate is quite sensitive, no doubt, compared to PETN oder RDX.
But I insist it will never detonate when a glass rod hits the beaker...
And I've also NEVER read about that so far in any reliable sources, but you still should bear in mind proper safety precautions.

But you can still convince me with data about what energy releases a glass rod hitting a beaker and if that is enough to detonate NG regarding to the given sensitivity data.



[Edited on 25-1-2011 by maxidastier]
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[*] posted on 25-1-2011 at 11:53


Quote:
But I insist it will never detonate when a glass rod hits the beaker...

You're making a very dangerous assumption here, maxidastier!
It's the kind of attitude anyone handling these compounds should guard against . . .
Much better to err wildly on the side of safety at all times!


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[*] posted on 26-1-2011 at 06:15


You are right. But I just can't believe that something like a little "cling" from a glass rod can make NG to explode. If that's the point, I would never handle with it again. :(
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[*] posted on 26-1-2011 at 09:35


Very interesting! Maybe a remote controlled old kitchen mixer and some big ass stirring rod will solve the problem. This is impossible for me, but anyone with nice place for tests is wellcome. Some things like the NG sensitivity in acid suspensions and the temperature are very interesting to me, because in the beginning I heavily used the thermometer for stirring rod. Then I totally switched to the magnetic stirrer & teflon bar combo. So, can “a little "cling" from a glass rod make NG to explode”. It’s time for some mythbusting…….

[Edited on 26-1-2011 by Jimbo Jones]
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[*] posted on 26-1-2011 at 11:14


Veery funny!
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[*] posted on 27-1-2011 at 02:10


Yes I also think this should be tested because I am also of the opinion that NG wont detonate from a glass rod hitting the wall of a flask.
Neither will a stirrbar detonate NG.

If you see how much force is needed with a hammer to detonate NG when it is placed on an anvil....
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[*] posted on 27-1-2011 at 08:55


I would have thought that I would NEVER have to consider saying this but we are talking about safety and ethics so.....

It's NOT just the impact of glass to glass but friction as well.; what's more there can be issues of hot-spots sensitizing minute droplets moving about the acid bath w/ it's possible temp fluctuations. We are also speaking to the phenomenon of the "expls TRAIN" concept where in a small pop sets off the rest. MY GOD! There is no correlation between an active nitration and a competed synthesis and during any nitration that has consistently provided documented proof a hideous disasters from what is termed a "run-a-way", if that phenomenon were to be examined it would be clear to some who has low levels of knowledge in chemistry that NG (as an example) has certain anomalies that can render it hyper-sensitive. The level and amount of unintended explosions has been documented to such a degree that if ANYONE wanted to venture into this with an open mind they would find EVERY reason to employ EVERY safety precaution available.

Anyone who has professional level chemical training does not dismiss safety issues with a "first person all encompassing statement". Just because something had not happened to you yet, does not mean it cannot occur. First hand single level experiences are just that: experiences. That is NOT science.

There is a great difference between a product that is in the process of nitration and one that has been completed, washed, stabilized, cooled, neutralized, & isolated. The correlation of an actively nitrated material's impact sensitivity and one that is currently being nitrated is dissimilar.

The warning of "glass to glass" impact during NG synthesis is VERY old and has been the course of many tragedies. (I actually can't believe I'm writing this.....)
One of the MAJOR rules of energetic synthesis is that you 1st minimize the possible sources of ignition stimulation. Hasn't ANYONE EVER STUDIED THIS? There is NEVER any valid reason for testing the limits of safety.

The two major areas wherein tragedies have happen were when someone "forgot" a simple procedure (i.e. grounding oneself and related areas to minimize static) and when they IGNORED those safety precautions ("I've done this all the times I've made it and it never........")

Let's just cut right to the chase here. Let's stop the bullshit. If anyone wants to CUT DOWN on their safety precautions (for whatever reason) make a sworn promise with yourself that you WILL come back and post what had happened when you had a tragedy! Remember.....it's NOT an "accident" it's negligence: as you have been amply warned about impact, friction, static, & other forms of stimulus. Not some post that I did this and nothing happened; but when you went to the Emergency Room!
I have heard too many of these things. I have confidence in one thing; unpredictability if formats of consistent precautions in the face of potential injury are ignored. It may not happen for 3x or 100x but eventually, if a person works with energetic materials CUTS DOWN on their safety procedures, they will eventually pay a price.

Ask yourself WHY even manual stir rods are coated with Teflon? Then ask yourself what is the pay off for LIMITING safety precautions rather than tightening them? Then ask yourself how many times you are willing to experiment with the possible loss of sight and limbs, finger, tendon tissue, etc?

Frankly I am very surprised & disheartened to read this thread. I had thought with so MANY years of history of tragedies behind it, that energetic synthesis would have simply been a standard [example of] EVERY lab precaution possible. And to find I was WRONG on that point makes me VERY leery of ever contributing an active, workable synthesis to this section of the Forum again. I would be willing to bet I am NOT alone in this thinking as well!
If what I have just written doesn't make sense to someone or someone wants to "debate" the issue; I simply won't go there but I will leave one statement of fact that should be considered ASIDE from the loss of eyes,, limbs, & flesh. The very idea of REDUCING safety measures when working with energetic materials would actually get you FIRED from most every vocational position dealing with any aspect of this subject.

Some folks wants to diminish their safety precautions: be my guest! I am VERY curious how many would be man enough to come back and speak to typing w/ one hand, or loosing their depth perception AND ESPECIALLY - HOW THEY WERE DEAD WRONG in not taking advise on the side of safety!

I say this with such emphasis because rationalization & intellectualism have caused SO much harm.....there IS NO getting through that emotional defense mechanism. Logic DOESN'T HELP.......So go for it.



[Edited on 27-1-2011 by quicksilver]




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[*] posted on 27-1-2011 at 09:12


I'm sry.
Will it be ok then, when I wrapp my glass thermometer with some Teflon coil? Will it give valid temperatures?
Can I also use a magnet stirrer with PTFE rods?
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[*] posted on 27-1-2011 at 09:29


The use of a thermometer is generally to be a stationary tool. Your best readings are made when it consistently it set up to encompass the fluid, gas etc; it's movement may cause more poor readings than anything else. It is NOT designed to BE a stirring utensil.

The common method of stirring NG both in plant-level and lab was with the use of air. There was a VERY good reason for that. It disbursed the material for better nitration and it made no contact of surface to surface agenda. I had already written that however. So I suppose I'm repeating myself.

[Edited on 27-1-2011 by quicksilver]




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[*] posted on 27-1-2011 at 09:52


But since I'm not the owner of a pump to blow air trough the mix, what can I do?
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[*] posted on 27-1-2011 at 10:20


Quote: Originally posted by quicksilver  

The warning of "glass to glass" impact during NG synthesis is VERY old and has been the course of many tragedies. (I actually can't believe I'm writing this.....)
One of the MAJOR rules of energetic synthesis is that you 1st minimize the possible sources of ignition stimulation. Hasn't ANYONE EVER STUDIED THIS? There is NEVER any valid reason for testing the limits of safety.

Let's just cut right to the chase here. Let's stop the bullshit. If anyone wants to CUT DOWN on their safety precautions (for whatever reason) make a sworn promise with yourself that you WILL come back and post what had happened when you had a tragedy! Remember.....it's NOT an "accident" it's negligence: as you have been amply warned about impact, friction, static, & other forms of stimulus. Not some post that I did this and nothing happened; but when you went to the Emergency Room!
I have heard too many of these things. I have confidence in one thing; unpredictability if formats of consistent precautions in the face of potential injury are ignored. It may not happen for 3x or 100x but eventually, if a person works with energetic materials CUTS DOWN on their safety procedures, they will eventually pay a price.


If you are not going to boil anything ... use plastic. Preferable
soft plastic. If you can find them for powders ... conductive
rubber containers.
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[*] posted on 27-1-2011 at 10:22


You could use methods designed to not require stirring, merely swirling the reaction vessel.

With appologies to Boomer, who posted this for another kid who was going to do it anyhow...

==================================================

OK, I cannot stop you anyway, so here is a very safe method: Your ratios were not bad, I mix 75ml of 96% sulphuric acid with 50g AN and put it in the deep freezer set to max. power (-25C) overnight. During the next morning, I add 11ml of glycerine in four portions with good swirling, and put it back for 1-2 hours each time. Even if you SHOULD add ONE portion very fast, the temp will only shoot from –25C to –10C each time, that’s why it is safe (thermal mass cannot jump to 30C). Of course you WILL add them SLOWLY and WATCH THE TEMP to get a feeling for the process. You have a thermometer, ehh?
I give it a few good shakings over the afternoon (putting it back in the freezer each time), and in the evening pour it into a litre of cold water. The NG settles at the bottom and can be sucked out, washed again with water, with bicarb, with water… look the process up on the above sites again before you start.
The reason you only saw a few drops is that most is suspended in the thick liquid. Yield for this method is around 50% of theory or 10ml of neutralised NG.

And SCALE IT DOWN the first time, please!




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[*] posted on 27-1-2011 at 11:18


Thanks for the method, but yield is rather bad. Anyway, is magnetic stirrer also to dangerous?

"If you are not going to boil anything ... use plastic"

I thought nitric acid and plastic don't work together? What specific sort of plastic do you suggest apart from "soft plastic"?
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[*] posted on 27-1-2011 at 12:00


http://www.tpp.ch/technical_information/raw_materials/Resist...
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[*] posted on 29-1-2011 at 01:25


Well, but where can you get a stirring rod made of PE oder PP???
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[*] posted on 29-1-2011 at 02:14



Adequate air volume should be available from an aquarium air pump.Mine was free from a friend who no longer owned an aquarium.Even new I cant imagine there an awful lot of $ given the increased piece of mind.The aquarium pump really agitates a 500ml beaker full of mildly viscuous fluid.As I dont yet own an overhead stirrer or mag stirrer/hotplate its very useful for relieving tired arms while still keeping the synthesis well stirred.

Im not sure if in high humidity climes it might be wise to try to use air coming off a source of dry heat,electric heater!?

[Edited on 29-1-2011 by grndpndr]

[Edited on 29-1-2011 by grndpndr]
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[*] posted on 29-1-2011 at 08:55


Quote: Originally posted by maxidastier  
Well, but where can you get a stirring rod made of PE oder PP???


There are PE and PTFE (Teflon) stirring rods and small spatulas available.

http://www.labsafety.com/search/HDPE+stir+rod/24550628/

That took 10 seconds to find. Google...

Quote: Originally posted by grndpndr  


Im not sure if in high humidity climes it might be wise to try to use air coming off a source of dry heat,electric heater!?



Heating air only lowers the relative humidity, it doesn't REMOVE any water vapor.



[Edited on 29-1-2011 by Bert]




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3. Mention anything you have learned from your target.
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[*] posted on 30-1-2011 at 10:57


I have always found that air agitation stripped off too much of the nitric, giving huge clouds of fumes. For this reason I have used swirling or magnetic stirring. If anyone has a method that reduces stripping, I'd like to hear it.
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