Quince
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Can't open the lid
I put about 30 mL nitroglycerin I in a small caviar jar and forgot it due to the distraction of my hospital stay. Now I can't open the lid. I'm
afraid to force it, since some is probably in the threads, or the jar could break. Any suggestions? I think it's fairly pure, so sensitivity
shouldn't be too bad, but still...
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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The_Davster
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Metal lid right?
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Nerro
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ehm sounds like something I wouldnt have done but now that you're stuck with it it might be best to (carefully!!!) take it out to some remote spot and
detonate it using a small charge.
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DrP
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Hmm.... - when my pots of polymer dispersion get their lids stuck on I BASH them REALLY!!! hard on the desk and that usually loosens them up a bit!
 Try eating some poisonous beans after to make sure!!
But seriously, if it has dried in the threads of the jar as you suspect, could you try soaking the jar for a couple of hours in a solvent for the
material? Hopefully the solvent will work its way in and free up the thread for turning. (???) I've never made nitroglycerin and would probably be
a bit scared too, so I'm really not an authority on this.
[Edited on 17-5-2006 by DrP]
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Bert
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Go to a vacant area. Lay a small fire of quick burning wood, cardboard, etc. Place the jar on top. Light the fire on the down wind side, retire to a
safe distance. Wait for loud whoosh or possibly BOOM! Don't store nitroglycerine or other such materials improperly in the future...
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Quince
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| Quote: | Originally posted by rogue chemist
Metal lid right? |
...
Yep, hot water did the trick. It took a few tries, since the small lid would cool by the time I could get a good grasp.
All this chemistry is making me forget my physics I guess
[Edited on 17-5-2006 by Quince]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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Marvin
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Storing a high explosive in a glass container is a pretty stupid thing to do at the best of times.
Depending on the purity I might have been inclined to put it in the fridge until it froze though. Frozen NG is much less sensitive.
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Chris The Great
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Since the glass get's blown to dust by the detonation, I don't think it matters that much. Also, I'd rather have a glass container and not have to
worry about the HE reacting/dissolving/etc the container, though that's really for liquid explosives. In this case, I'd rather have a glass
container, since nitro might cause degradation of the plastic over time.
The fact that the plastic in the lining seized up is a good indicator that the nitro would degrade plastic over time.
I store my methyl nitrate in a glass jar, but then again, there is over a quarter pound so if it ever did explode I wouldn't be around to care about
the glass fragments imbedded in the small chunks of meat that used to be me spread across my yard. But it doesn't like plastic, so I only use that
for short transportation, in polyethylene bottles which seem to be one of the few things that doesn't get turned too goo.
Anyway, not really stupid in some cases.
Thawing nitro is a lot more dangerous than storing it in a glass jar IMO.
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Marvin
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NG is much safer to handle when frozen and given Quince has a long history of flouting risk it was unlikley he'd simply destroy it (The best option).
Defrosting NG only has a bad reputation in the early literiture due to how it was being done, generally on site just before use and people were
lighting fires to provide the heat. Companies like Nobel were freezing NG for transport and defrosting later for decades without any problems. This
was massivly safer than transporting the liquid. Properly frozen, the glass jar could have been smashed with low risk, depending quite a lot on the
quality of the NG though, so opening the lid should not have been a real problem in this state.
I don't think home made NG is suitable for any long term storage at all, though in many cases use of glass for short periods is unavoidable. Maybe a
teflon coated plastic container might be better for handeling the liquid but storing it frozen is also a much better move.
I have no experience with Methyl Nitrate, nor have I read much about it so I can't really comment but I may start calling you 'Chris the great area'.
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Quince
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Yes, I was worried about using a plastic container as Chris suggested. I don't see how I'm flouting risk.
I am glad I hadn't used acetone to desensitize the NG for storage, as that would have completely dissolved the plastic lining on the lid's underside.
I am intending to gel as soon as I can manage to get a properly nitrated cellulose, which I've always had trouble with whatever method I chose, as the
cotton keeps getting highly nitrated in some spots and not nitrated in others, despite my best efforts at stirring; I am never able to get the proper
moderate nitration for gelling NG.
By the way, adding Al powder as fuel to improve oxygen balance, will the Al be completely unreactive with the NG/NC for some time?
[Edited on 18-5-2006 by Quince]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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enhzflep
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With regards to the production of NC, the most succes I've had in its production, involves the addition of cotton wool in very small increments. I.e
something like 5 or 6 additions per 1gm pad. Nitration is effected in seconds IIRC, so it's just a matter of adding small amounts albeit many more of
them. I used the method specified in Urbanski, though the method of cellulose hexanitrate as found on the PowerLabs site works equally well.
Have never had particullarly good results using phosphoric acid + nitric, nor have I had good results with H2SO4 + any nitrate salt. For best results,
you really need to use concentrated nitric acid. This has been produced succesfully dozens of times using a brand of fertilizer freely available from
supermarkets combined with distilled H2SO4 from discarded car batteries. The distillation equipment could not even be described as primative .
I.e saucepan filled with vegetable oil, glass bottle (I use V or RedBull) with platic lid, along with a section of clear PVC tubing (8mm OD). This
tube runs through a hole in the lid of the reaction vessel into a hole in a second plastic lid 1/2 way screwed onto a second glass bottle submerged
into a large cup filled with ice/water. The receiving flask's cooling water needs to be changed every 10 mins or so. Ensure also that the tube runs to
nearly the bottom of the receiving flask.
While being light-years from optimal, this setup has successfully distilled nitric with a s.g of 1.5 - 1.6 each and every time, albeit with the
replacement of the plastic lids every 5 times or so and replacement of the tubing every time. It goes opaque and begins to crackle
While Al will improve the overall energy output of such a mixture, one would need to use rather a low percentage of NC in order to keep a +ive or 0
O.B, remember that something like 6-7% NC is needed for an OB'd mixture. IIRC its use (Al) will also slow the max VDet, although the practical VDet
may be increased due to the adherence of bubbles to the Al powder.
Failing the use of home-made NC, one may freely use double base shot-gun (or pistol or rifle) powder as the NC source. If as is probably the case,
this is not a viable option, Table tennis balls are entirely serviceable.
Simply dissolve them with minimum acetone first to form a thick gluggy mass. Next add calculated mass of NG, kneed to incorporate bubbles and at the
same time provide heat to drive off acetone and Voila! Blasting gelatin!
Can't say however if the Al would be unreactive. You could try a web search for compositions containing these three if you've not done so already...
[EDIT] The fertilizer sold is less than 50% NH4NO3, which obviously entails purification first. This however is another matter..
[Edited on 18-5-2006 by enhzflep]
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Boomer
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Nitric of density 1.5 - 1.6? You mean like 125% pure? 
Depending on temp, 1.50 - 1.52 is 100%. You *can* get higher densities for a given concentration if NO2 is dissolved, e.g. 1.5 g/ccm but only <90%
pure, with water and NO2 raising it above 1.45.
Oh and NC is *not* fully nitrated in seconds. Leaving it 15-30 minutes, or even some hours gives better results (especially with sulfuric/nitrate). It
also helps to cut it as fine as possible before. I rather spend 10 minutes with scissors than stirr a hard lump an hour. The cut-up stuff is easy to
stir, making a few stirs over an hour sufficient (after initially stiring well for 5 min).
As far as NG and plastic is concerned, all *hard* plastic I tried was OK, just not the rubber-like lining in metal lids. Small med bottles with
plastic lids work fine for me, so do syringes which stand up infinitely as well.
Finally I like to note that home made NG *can* be stored for ages. My two youngest batches are from 2004/5 respectively (I don't use much), and are
still fine, and I even have small samples left from the 1980ies and 90ies! Three days of washing, with a shake every time you walk by does the trick.
Very weak soda solution (<<1%) is sufficient here, you don't want it to hydrolize. The bulk of the acid must be removed beforehand of course,
and the soda and finally the water removed well after.
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nitro-genes
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You can even make NC quite well with a nitrating mix composed of 40 grams AN or 50 grams of KNO3 with 100 ml H2SO4 (96%+). I have used nitrating times
up to 5 days (!) at room temperature with very good results. You have to use very pure, and well rinsed cotton for this else you will end up with a
yellow goo...
And yeah, NG that is neautralized and stabilized is very storage stable, in fact the 6 grams that was used for my last shaped charge was from 10 ml of
NG stored for over a year in a safe place. Just gave it another wash before using it, just to be sure. To know what unstable NG looks like I've stored
1 ml quantaties also that were only bicarb neutralized for a day, without stabilizer and these samples went from very faintly yellow, to almost orange
in about a month. If NG is still very faintly yellow and clear, I think it is safe to say that there is very little decomposition and it won't be
terribly more sensitive...
I'm glad to hear NG is compatible with hard plastics, I've noticed indeed that there is no problem of using NG with PVC, unfortunately though PVC
adhesive does get dissolved... Polyethylene or polypropylene, (Greiner tubes and
eppendorf tubes  ) are no problem. Hard polystyrene however looks very much like
these plastics, and becomes weak very fast...
[Edited on 18-5-2006 by nitro-genes]
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Quince
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nitro-genes, what do you mean stabilized? What additives do you use? And I didn't know a liquid explosive could be used for a shaped charge.
As for my cotton, I usually use cotton balls from the drug store which I boil in water and dry before nitration.
I never tried cutting them up, since already much of the cotton after nitration is just floating about in small particles and I've no idea how to
separate it from the liquid, since the acid mixture would eat away any filter.
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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Chris The Great
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| Quote: | Originally posted by enhzflep
While Al will improve the overall energy output of such a mixture, one would need to use rather a low percentage of NC in order to keep a +ive or 0
O.B, remember that something like 6-7% NC is needed for an OB'd mixture. IIRC its use (Al) will also slow the max VDet, although the practical VDet
may be increased due to the adherence of bubbles to the Al powder. |
Nearly doubles it by weight by my calculations
Who cares if it 0% OB, you're still going to be getting a butload of energy. IIRC I calculated that with 32% Al powder by weight for the nitro/NC of
93/7.
Thank you so much for that tip nitro-genes for NC! I've tried it with NC before, it gelled stuff, but it was not fully nitrated and burned very
slowly. I will try your method from now on. Off topic I know, but thank you!
Marvin- methyl nitrate has a drop test of 40cm (vs. 20cm for EGDN) but is apparently friction sensitive. My two month old first batch, after
it turned yellow, could not be set off with repeated hammer blows on the anvil, even when absorbed into paper. Still, I treat it with respect, a 240%
TNT brisance makes one tread carefully.
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Swany
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Well, whatever you do, make sure it doesn't spill in your bedroom if you attempt to open it... I'm sure Boomer could enlighten you with the downside
of this if he so chooses to.
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enhzflep
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Yup, thats right. Itwas RFNA - not WFNA. Should have mentioned that. sorry.
If I'm in no particular hurry it's pale yellow, but generally without a vacuum and with correspondingly higher temps and short reaction time - its
rather red.
I never bother with urea unless I'm doing NG, and can't be bothered looking up the literature now, (the NO2 may well have an effect on the nitrating
abilities of the mixture)but the cotton shrinks immediately upon contact with said acid mixture.
Yeah, I guess zero OB is not too important, I just preffer low light emmisions and a good sharp crack rather than a BOOM - personal preference..
For what its worth Quince, if your cotton doesn't stay stuck together in clump at the bottom of the reaction vessel, you may just pour the mixture
through a plastic strainer as found in a supermarket, failing that - just tip the acid out slowly and recycle as desired..
I use cotton pads as opposed to balls since the packet was unmarked and I thought I was getting a 'brick' - (like we use for polishing the inside of
gold rings with.
However, this form of cotton wool in pads has proven to be very satisfactory. Each pad may be pulled apart into about 8 layers of reasonably uniform
thickness. I have been more successfull with the cotton
in this form than in cut-up form too, btw. Since each layer is about 2mm thick and like a cyclone fence in compactness - i.e free access for the acid.
The longest I generally nitrate for is 1/2 hour (room-temp to slightly warm acid mix) - 15mins after last addition, after which time a sample is flame
tested from each of the strata. (The cotton doesn't stick together too much at all..) I don't have scales acurate to 1/100s or 1/1000s of a gm, but
the amount of ash left behind is on a par with smokeless powder. - Though admittedly there is a rather nitric smelling emmision of gas upon burning,
due to obviously insufficient neutralizing. Boiled in bicarb for around 10mins.
The only success I've had in making reasonably good NG - read no discoloration after at least 6months, is to use 98% H2SO4 from chem supplier, along
with 70% Nitric, dried with same sulphuric, over the course of about 3hours- and without the use of pvc tubing. Think along the lines of small mouthed
glass bottle inserted into larger mouthed glass jar/bottle - It just allows more gases to escape, for the sake of usually unnessecary purity. Which,
when using store bought Nitric is rather galling due to it's rather high price when only buying 2.5L at a time, considering that 15L may be had for
just over twice the price as 2.5!
Hence my most common use of fertilizer + distilled car-battery acid. Heating gas is very cheap, car-batteries are about $1.50 worth of petrol for 6
or 7 at a local car workshop, and the fertilizer is also very cheap - labour is free
There is a saying in computer programming that also applies to much of life. The final 20% of the job takes 80% of the time.
If the results gained in the final 20% are not necessary then why use 80% of the time on them? Hence quick 'n dirty production techniques for material
to be consumed within 24 hours. SO LONG AS the first 80% of the job will be safe.
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Quince
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I'm still wondering what stabilization of NG nitro-genes was talking about.
[Edited on 19-5-2006 by Quince]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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quicksilver
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| Quote: | Originally posted by Quince
nitro-genes, what do you mean stabilized? What additives do you use? And I didn't know a liquid explosive could be used for a shaped charge.
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The stabilization of nitric esters like NG (or ETN / PETN) may be accomplished by the use of Diphenylamine. That is the route commercial production
utilizes. It's a nice little tool as it also turns a blue colour if there are exposures to impurities or any break down of the product. So it gives
you a warning to re-purify. Betain may be used as well. Roscoe turned me on to that technique (Betain is a vitamine B material).
To stabilize a nitric ester is perhaps one of the most important things one can do IMO when even thinking of storage due to the fluxuations in temp
and contact with impuriies all stored materials may face.
Diphenylamine is commercially available, inexpensive, and lasts a long time as one uses just a wee bit of it for stabilaization purposes. It even has
an energetic material made directly from it! (See COPAE). The blue colour issue is very useful and has a great deal of documentation regarding it's
use in explos mfg.
There are also stabilization proceedures with Urea but their long term benefit is not nearly what Diphenylamine provides.
Du Pont's Diphenylamine is a biege colour rhobic platlets, the reagent grade is white needles and is available from most suppliers. It's cost is
reather high but a 100gr bottle will last for years.
[Edited on 19-5-2006 by quicksilver]
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Quince
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Crap, I can't find any seller of diphenylamine that would sell to me.
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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Boomer
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Have I read somewhere that diphenylamine in *not* good for liquid nitric esters, in that it decomposes them faster than what would happen to neutral
stuff without it? That it is only used for NC/NS, something else for PETN/MHN and a third substance for NG/EGDN?
I may be totally wrong here but it somehow rang a bell.
My NG has no stabilizer and stores a decade or two, so before this is cleared up I will leave it that way.
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nitro-genes
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| Quote: | Originally posted by Boomer
Have I read somewhere that diphenylamine in *not* good for liquid nitric esters, in that it decomposes them faster than what would happen to neutral
stuff without it? That it is only used for NC/NS, something else for PETN/MHN and a third substance for NG/EGDN? |
Could be true, but I thought diphenylamine was still in use as a stabilizer in many double based gunpowders and also in high percentage (40-50%) NG
containing solid propellants. But this could be mainly a stabilizer for the NC indeed...
Todays stabilzers for NG, the centralites, have only replaced diphenylamine since centralites make slightly more effective stabilizers, not because of
incompatibility IIRC...
But ok, thoroughly washed it stores for quite some time indeed. I believe it was on this board that I read about one of the first bottles of NG made
by Sobrero himself that is only washed with bicarb. solution every year. Don't know if this is true though...
[Edited on 22-5-2006 by nitro-genes]
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quicksilver
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Actually that was started by a web site that made that claim IIRC. Someone brought it up on a discussion board and the web site which was a commercial
outlet for explos did indeed state that directly. But it had been a standard in DBSP for many decades and is still in use. (?) One has but to read a
can of powder to see that it's still used.
I quote from an ALLIANT label:
NC
NG
diphenylamine
ethyl centralite
rosin
polyester
Can is 5 months old and smells great! Same great smell as an old Hercules can that 15yrs old +.... Seems to work quite well for DuPont as well (see
IMR powders).
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