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quicksilver
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Take your tubing and curve it on the very bottom of the beaker, into the edge and about 120deg. of circumstance. Use a valve OR a clam to allow a
small amount of pressure to escape. There is a "timing issue" here and if you open the valve up you get a whirlpool effect that is VERY gentle. Hard
bubbles appear to be the problem; the idea is to make the movement very gentle and avoiding "hard aeration". Another technique I've sen is to point
the air tube directly down into the flat bottom of the beaker & lighten up the pressure; this creates a "pebble-in-a-pond" effect which is very
effective. The issue is generally TOO MUCH pressure rather than slight amounts. You just want to have the acid move about in a continuum.
If a magnetic unit is used (IMO) it's always best to use those tiny "capsule" sized ones as they just barely move the acid in a gentile swirl (the
same as air if reduced in pressure, etc).
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maxidastier
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Quote: Originally posted by Microtek  | | 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. |
Yes, but bubbling dry air through it can help to convert red fuming HNO3 into white fuming, doesn't it
4 NO2 + O2 + 2 H2O ---> 4 HNO3
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MetalNeko
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Hi, all! This is my first post - although I would like to point out that I've been reading the forums for four to five years and I've nitrated a
handful of different nitric esters as well as some other things along with pyrotechnics. I haven't done much in the past two years in regards to
chemistry, but I've sort of picked up the hobby again.
----end introduction!---
Alright, I'll make this short and sweet: I nitrated some glycerol/glycerin recently using pure NH4NO3 and Clear Line drain opener (which I believe is
around 97% H2SO4). The nitration, crashing and neutralization all went swimmingly and I'm left with a nice little vial sample of the batch. Here's a
photo of it:
[img]http://i176.photobucket.com/albums/w185/devaughn357/NG.jpg?t=1305082383[/img]
In case you cannot view the photo, the nitro is an off-white color, mostly translucent.
I'm posting to ask if anyone knows if those little bubbles are a problem? Thanks in advance.
[Edited on 11-5-2011 by MetalNeko]
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hissingnoise
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Couldn't find the picture, but if bubbles are visible in your nitro then neutralisation isn't complete!
If you're talking about a slight milkiness - that's normal.
The milkiness of freshly prepared nitro is caused by a small quantity of entrained water and it disappears in a few days by evaporation . . .
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MetalNeko
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I crashed in 10 gallons of water, added an icecream container of sodium bicarb water, let it sit for a few days, sucked up the NG with a syringe, then
flushed the container it was in with about 6x the amount of water.
I placed some sodium bicarbonate solution directly into a little drop of NG and observed no reaction, Hmm, is it possible for it to bubble like this
from being too basic?
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hissingnoise
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10 gal seems excessive unless you're doing litre batches . . .
And letting nitro simply sit in water isn't sufficient for washing!
All of the interior of the nitro must be exposed to the washwater by gently swirling it around the bottom of the container for several
minutes.
I'd rewash it in ~10 times its volume of cool water . . .
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albqbrian
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My two cents...
I've just got on this site and it's been eye opening. I'll confess up front; I haven't made NG nor do I plan on it. But there are some obvious safety
things I feel need mentioning.
I have some background in the area: pyro as kid, college chem deg, lots of work in orgo syn & biochem labs, taught explosive use in military, made
hundreds of pounds of composite rocket fuel as a recent hobby, and I lived long enough to have mainly gray hair. I don't want to start out my career
here as an a**hole, but jesus...
Most of you are scary cavalier about this stuff! You're making something where a few ml can permanently f**k you up. And you're using stump remover?
You're worrying about when you're glass rod hits the side of the reaction vessel? Where is any mention of shielding/armor? Of remote control ops (the
air bubble thing certainly sounded like a minimum precaution), etc.
You want to make NG? OK. But let's be clear. In the US anyway you are seriously breaking the law. No if, ands, or buts. Everyone has to make their own
risk/reward calculations here, but be very cognizant of this. You don't want the ATF on your ass. Ask Randy Weaver or those two dozen kids burned
alive in Waco. But that's who does explosive stuff in US LE. You're making NG? You'd better have a serious plan.
Any serious experiment, or cooking for that matter; requires the best ingredients. You need high quality NA? Then buy it (hard granted) or distill it.
If you can't successfully distill NA I'd say you shouldn't be making NG. What sort of shield is between you and the reaction vessel? A bit of NG in a
small glass container won't need much, but it needs something. If you're smart enough to make NG aren't you smart enough to find a way to turn/shake
your reaction vessel without holding it in your hand?? Wow, holding something glass in my hand while it has a dangerous quantity of HE and who knows
what impurities. Is that about right? Shiver. What about your dry runs? With colored water or whatever standing in for the chems while you do all the
tasks required of your synthesis. I'd do that at least a couple of times. No way you'll do a complex task exactly correctly the 1st time. If you need
a simple example to convince you; go pick out an unfamiliar recipe (for food) and make it. You'll see.
OK, I'll stop now. I found this thread to be very educational. Certainly as a life long pyro I've always wondered about the nuts and bolts of making
NG. I've learned a lot. But I strongly feel that what I said needed saying. If you want to boot me from here; I'll understand.
In the future I'll post some positive stuff. I don't want you to think I'm just some nasty old a**hole 
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hissingnoise
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| Quote: | | Wow, holding something glass in my hand while it has a dangerous quantity of HE and who knows what impurities. Is that about right? Shiver.
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You've spent time in the army, blowing shit up, and you're this overly paranoid about a substance that has been produced in tonnage quantities since
Nobel's day?
Are you, perhaps, taking the 'Hollywood model' at little too literally?
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albqbrian
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HN...
I don't want get into a pi**ing contest here. But you can't equate industrial production with the methods being discussed here. That's not what this
thread is about. It's about one person, most likely at home, by hand, making a somewhat sensitive HE.
What just jumped out at me was the lack of a big picture, process perspective. The checklist, the practice runs, another person who can save you if
something bad happens, etc. All I saw was is this pure enough, how much of that ingredient. Those things are important; but you need an overall plan
to successfully get you to your objective.
In the Army using explosives was pretty regimented; not always, but mostly. And if you had to do something dangerous; one person did it; while a
rescue crew waited nearby.
I'll leave this topic be now. Thanks for listening.
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hissingnoise
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I wasn't having a go at you albqbrian, but there are tried syntheses of more sensitive and dangerous compounds than nitro on the board . . .
Nitro certainly commands respect but once the synthesis is known any careful amateur can prepare it without incident.
I'd recommend a reading of COPAE; "The Chemistry of Powder and Explosives" by T.L. Davis - it's in the site library.
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quicksilver
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Gentlemen please take a moment and realize that you're closer in your manner of thinking than it may superficially seem.
All too often the printed word cannot convey the undertones that body-language and facial expressions do.
That being said; an individual considering experimenting with nitric esters who does not do substantial background study is obviously opening
themselves up to a serious set of problems. [Baker 1909 US patent] siting the stability-longevity of glycerin when compared to glycol; the choice is
obvious. I believe it was the Nitro-Nobel Corp. offices maintain an original sample which they periodically test and neutralize; yet glycols have met
shelf life stability of decades.
Polyester+ stabilizer pelletized NG in firearm's propellants have (in some cases) maintained stability for close to 100 yrs.
However the common testing batch sizes used by the USBoM maintained at or below 40gr as a standard. Controlling acidity and related issues of
stability in sizes measured in grams is common & achievable.
I was going to set legal issues aside; however there are (written into law) levels of experimental unit sizes of energetic materials that can and do
amount to common research and are not infractions of US Federal law. The popular "Orange Book" is very old at this point & cannot be depended upon
for clarification of Federal statutes in this regard. However they may be infractions of State law & the best thing is to do one's legal research
before anything chemical.
Realistically, there is a difference between "kitchen chemistry" and graduate and post-doc research in energetics. It's not my place to second-guess
what any other individual is doing with physical materials. While any "picture' could just as easily be table salt or mineral oil, any discussions can
be confabulation; I prefer to not assume anything & realize that our dialogs are a 1st Amendment Right and NOT aimed at the "practical
implementation" of energetic materials application. This is NOT the E&W forum.
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hissingnoise
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Apropos of nothing in particular, a dark question I've asked myself more than once is; if when holding a beaker containing, say, nitro, an unscheduled
detonation occurred, would it be preferable that the batch would be the usual quantity, a quantity which would have the energy to pretty well fuck me
up physically for the remainder of my life, or should there be 'enough', the concussion of which would take me out - instantly . . .
I'm fairly certain this 'uncomfortable' question lurks in the recesses of the minds of a few other people interested in HEs, posting here!
[edit] I seem to remember Sidney Alford once saying; "Think of the hospital bills you'd save" . . .
[Edited on 28-5-2011 by hissingnoise]
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quicksilver
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That IS pretty dark.
Reminds me of a WWII concept wherein the Allies were using booby-traps in field telephone made from one (single) blasting cap in the ear-piece of the
phone. Result was generally instantly lethal due to placement.
It's a lot like realty and home sales...."Location, location, location".
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hissingnoise
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And the Wehrmacht, of course, weren't exactly slouches when it came to thinking up methods to produce this type of nasty little, er, 'surprise'!
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nitromethano
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Hi, I'm new to the forum, I had all kinds of explosives usually high order for about 5 years, I'm from Argentina, do not speak good English, so I use
a translator, I hope you understand.
My concern is: I always spoil nitroglycerin, in a short time. My NG fresh, is translucent, practically colorless (very similar to EGDN), its
sencibilidad is correct, its viscosity, and pH.
After completing the chemical reaction, wash it 5 times, with big quantity, solution of sodium bicarbonate (2 liters of saturated solution of
bicarbonate to 20 ml of NG). Then dried.
In this NG, is translucent, colorless, with a faint odor, slightly oily, and is supposed to be neutral. PURE NG
After a month, begins to turn yellow-green, as the weeks go more green, at 3 months and is green with some small bubbles.
As the months pass, it becomes dark green and some small crystals are formed on the shore.
After a year and some months, take this photo, where liquid is transparent, with jelly crystals. ¡¡¡¿¿??!!!
[Edited on 30-9-2011 by nitromethano]
[Edited on 30-9-2011 by nitromethano]
[Edited on 30-9-2011 by nitromethano]
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bonelesss
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I am a bit confused why You store such a volatile explosive so long period? Are You making some kind of test? I would not even stand near that.
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hissingnoise
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| Quote: | | My concern is: I always spoil nitroglycerin, in a short time. |
For starters, the neutralising wash should contain no more than a few per cent bicarbonate and and all traces of the salt should be washed from NGl by
two or three further clean-water washes!
Properly stored, purified NGl should remain unchanged indefinitely . . .
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quicksilver
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Hay muchas cosas que son muy imporante!
* - Sabía usted tome una lectura de pH después de neualization?
* - El "lavado de carbonato" se debe a totalmente en la solución por lo tanto, sólo necesita una pequeña cantidad de "carbonato" a un mayor volumen
de agua.
Usted debe leer litererature de la ciencia antes de hacer esto para que sepa de todas las técnicas de laboratorio apropiadas y peligros. Muchas
personas se han visto afectados por no leer lo suficiente la calidad de la ciencia (the chemistry) libros sobre explosivos. Almacenamiento no es una
buena idea para el "nitric ester". There are different tipos o "diseños de productos químicos (de explosivo). And they have different "REQUISITOS"
(sp?) in the storage. First you must understand those requirements.
Obtener el libro de "Química de la Pólvora y Explosivos", escrito por "Tenny Davis". Sí, es en Inglés, pero se puede traducir y la síntesis de
explosivos de la ciencia - no solo la discusión. It is free: you can download it here in the "Los Alamos" book section at the start of the Forum.
Esto es muy peligroso. Hacer sus preguntas en español, está bien. Pero LEER y estudiar los libros de ciencia alidad. Usted recibirá respuestas
sólidas aquí, pero cualquiera puede cometer un error Y con este tema, esta actividad, un error y usted perderá sus ojos y manos.
[Edited on 1-10-2011 by quicksilver]
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hissingnoise
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Looks interesting, but I'm too old to start learning Spanish . . . any chance of a translation, QS?
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quicksilver
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Of course.
I asked if he had tested his pH ( at his point of completion of neutralization - so that he knew from the outset that it had moved from being
acidic.)
I mentioned (as you did) that a small amount of anti-acid [properly in solution] was the best way to create a means of dealing w/ acidic nitric
esters.
I attempted to communicate the requirements (requisitos - I'm not sure if that's the correct spelling) of nitric esters in shelf life
Then I addressed the importance of obtaining source material and pitched Davis' book. And that - although it was in English he could work with it just
as he was dealing with the language issue here (& elsewhere) bit by bit. I also mentioned cautionary elements (especially with esters) and how
it's all to easy to loose your eyes and hands. Basically, I reiterated the need to "READ" before proceeding with energetic chemistry; to study the
science of chemistry. That's about it.
It's been my belief that many people naturally believe that the more experience; the greater the learning. We know that in this agenda it's
potentially a serious danger to use experience as a guide alone without a background of prior study: more toward lab technique, safety issues, &
potential "red flags" in a synthesis. I also think it's natural to some degree for an individual to assume that reading about a subject is less
instructive than actively engaging in it. Some people especially with natural analytic, athletic or mechanical backgrounds often enjoy an active
engagement in a subject. Some may believe that reading about it is somewhat "arm-chair experience" & wouldn't apply the same to other hobbies or
areas of interest. Many, if not most people like a "hands-on" approach. But in this area it could end up being a hands off tragedy.
I push Davis' book a lot because it's available, proven, & easily understood. It also has well understood sections that could be translated with
little problem. One difficulty with some of the more expensive & in-depth texts are that they are scanned as a graphic. That does not allow a "cut
& paste" to use in Google's translator or a non-English dictionary conversion program.
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hissingnoise
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| Quote: | | Basically, I reiterated the need to "READ" before proceeding with energetic chemistry; to study the science of chemistry. That's about it.
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Thanks QS --- yes the 'need to read' would seem to be self-evident but apparently it isn't clear to all.
Let's just hope he takes the message on board while he's still in one piece . . .
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Ral123
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I haven't made NG and I'm kinda wandering would I ever http://www.youtube.com/watch?v=5tlvDTPxwEY&feature=relat...
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quicksilver
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Utube is great for getting guitar lessons.....but that was enough NG to tear the upper part of the individual's body apart. The best favor anyone
could do is leave the videos alone for information regarding a subject such as that. Nitric esters need to be totally acid free and in many instances,
re-evaluated for spoilage. In many instances a stabilizer could provide some help or warnings (diphenylamine turning blue in response to nitrus, etc)
but purity in synthesis is not a kitchen chemistry issue.
If I am correct some of the original nitroglycerin on display at Dynamit-Nobel is periodically checked for purity. many esters have long shelf lives
but a great deal of knowledge and research was put into that agenda. Putting 250ml+ in a screw top jar is not a good sign for longevity.....
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Ral123
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That is NG. And I'm supposed to handle such a thing in a beaker till I wash it? How you guys do it? I feel stupid for being afraid of nicely washed,
neutralised egdn at home.
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quicksilver
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First of all a mid-size jar of NG open on a table would give a new user a nitro headache he would not soon forget. That generally needs to be
remembered as the adrenaline rises and your head is pounding....And one of the reasons to work with a tiny amount as well. But there are methods.....
Once NG is synthesized many people retain it under water that has been deeply saturated with common salt (Na or KClO2) and an anti-acid such as
Calcium Carbonate or even baking soda. This is a simple method of drying the NG and freeing it from any remaining acids. The introduction of water
ALSO keeps the head-ache factor at bay. Nitro head-aches can be very nasty and can disturb concentration. After about 3-5days of working with nitro
(glycerin or glycol) the body gets "used to" the extreme vaso-dilation and the headaches go away. In fact some people have a strange reaction AFTER
they have worked with NG for a long period and get head-aches once again when the NG is REMOVED!
NG can be a serious toxin for some and the proper protective gear should be worn at all times when working with NG. notice in the uTube video the
young person had nothing to protect himself from a glass jar of about 250ml+ of nitro. If that blows up the wave would most likely kill him outright.
but if he had some distance the room would be filled with a great deal of fast moving projectiles. NG is still one of the "kings" of seriously
powerful explosives: substantially faster than TNT, TNP, most all primaries, etc.
NG is difficult to contain as a screw-top jar is really a stupid place to store it. Anything with friction or grinding is to be avoided. That was one
of the basic reasons why dynamite was developed. If one MUST work with liquid NG, keep the levels low (in the single gram(s) level) & don't use
glass if you don't have to.Many stores with perfume have sample bottles that contain about one gram and have a polymer seal top. This may be coated
with wax on the top contact of the polymer top and lower friction to a moderate level. A single gram may still have the strength to knock a finger off
but you would live if something unfortunate occurred.
AND -=DON'T=- FEEL STUPID about being apprehensive over potentially dangerous materials. Trepidation, anxiety, fear, and apprehension are emotions we
have that provide self preservation. Poisonous snakes are often handled with a snake-stick for a REASON - and the finest Herpetologists in the world
don't let their samples slither around their homes. We have these emotions for a damn good reason.
Edit:
Nauom wrote some of the best materials you can get for exploring some testing - Book was titled "Nitroglycerin & Nitroglycerin Explosives". Old
but interesting and a fast read. Modern dynamites however (when used) generally use glycol - less sensitive but the headache is fairly serious. Many
nitric ester are now used for heart conditions, even PETN.
[Edited on 10-2-2012 by quicksilver]
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