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Ral123
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Excellent acid. With that you can do almost anything in the book. You ask how the runaway happens. Well, you add the hexamine and not much temperature
rise is observed. After a while reacting you stop adding to let it stay at safe temperature and you consider replacing the ice bath. However it still
bubbles and the temperature stays uncomfortably high. You realize you don't have another ice bath prepared. You drop the vessel in a bunch of ice, but
it doesn't sink all the way in the ice lumps. At some point the temperature rises above 30 and it gets more violent by the second. With very little
time to react, you just rush the reaction to a safe place for it to boil off and enjoy a very clean and sterilized floor. Also awful coating on
everything near. The NOx can be seen seeping out the lower part of your apartment door.
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Armistice19
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Hmmm...so it seems one should use vinyl gloves for nitrations.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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golfpro
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It seems One should not think too much for nitration.
Just use gloves, if you do that you're doing good, take them off if you spill acid on them, nitrile is fine.
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Hockeydemon
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I agree with golfpro - if you notice I'm wearing nitril gloves while shooting the video. Though it is possible that I might spill that quantity of
nitric acid on myself it is unlikely. Most of the 'spills' I'm exposed to are drop sized when it comes to them actually touching me. If you get a drop
of nitric acid on nitril gloves it will heat up very noticeably, but I don't know that it would combust like it did in the video - at least not nearly
as quickly. Though if you're so inclined you can buy some more expensive non-disposable lab gloves.
Though I should note I have multiple safety guards in place. For example while I was making the nitric acid (and wearing nitril gloves) I need a water
sources for my condenser which is a bucket of water right next to the distillation apparatus. It would take no time for me to dump my hand in that
water. I also have chemical fire extinguishers in multiple places, and base solution for neutralizing acids nearby at all times. I also wear a lab
coat, goggles, and a respirator.
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Armistice19
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You're probably right, either way I just bought a small pack of disposable vinyl gloves at home depot for the occasion.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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Hockeydemon
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Not that it has any real relevance to anything, but I redid that video with a GoPro so it is a little better quality.
http://youtu.be/mTPgCzwqpJE
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Armistice19
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Alas, I am reminded of how much I wish I had a GoPro.
Here's the deal, I don't think I will be ready with enough NC for July 4th, and the only reason I didn't "go big or go home" with flash powder is
because of its relative instability. So now I ask a new question, how big can I go with flash powder before I am putting myself in danger? I
understand static shock and friction are some things to keep in mind as far as safety goes, but how much really changes the bigger you go? I mean it's
the same stuff, it's just more of it right?
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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chemcam
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When I do a big flash charge I make several small batches (10g each) then dump them in together once I have made enough. Flash powder is safer than
most easy-to-make HE's, and yes, same stuff only more damage if an accident occurs. With HE's that is not always the case, more together means more
sensitive and dangerous i.e. silver fulminate and other primaries. Even with some secondaries bigger quantity makes higher percent chance of having
residual acid or impurities.
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golfpro
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That is so dumb how it's that easy to make a very High Explosive from basic materials (ETN, EGDN, HMTD etc.), but there is almost no way in hell to
make flashpowder no matter how hard you try, KCLO4 -- yeah right, and aluminum powder. Is the govt. more worried about FP? if so why is that?
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killswitch
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Quote: Originally posted by Armistice19  | Yes tannerite is cool, never shot it yet but I've heard alot about it. However I'm really more trying to test myself with actually making something at
this point. I love to create, and watch my creations go boom. I would like to feel proud this year, and go big or go home. In other words, store
bought explosives are out of the question in my mind. Synthesis in and of itself is a joyful experience. Ease of manufacture is important only because
I have a month to obtain materials and begin production. Really, I am much more concerned about how safe the material is to make, and how
stable/insensitive it is after it is complete. I know I am just a beginner, but I would rather try to make something and fail multiple times, than
succeed and blow my hands off.
(Also please no tertiary suggestions at this point, I know I already said ANFO but tertiaries seem a bit too complex at this point)
[Edited on 2-6-2013 by Armistice19]
[Edited on 2-6-2013 by Armistice19] |
If it is as warm as you say it is, peroxides are not a smart idea. They're unlikely to go boom, but since you're not in a clean room I'd say no.
Interestingly enough, nitroform (trinitromethane) can be made solely with dichloromethane, nitric acid, and isopropyl alcohol.
Don't quote me on this, and do your own research, but HNO3 is soluble in dichloromethane, while H2SO4 is not. NaNO3+H2SO4+dichloromethane should make
a clean two-layer separation of nitric acid+DCM and sulfuric acid. Decanting+ pipetting can separate them, though vacuum distillation is still your
best bet. Then on to the nitroform synthesis.
If it's fun you want, get some nitromethane from an online dragster fuel outlet, non-PVC plastic pipe, an empty plastic water cooler tank, and some
black powder and fuse. Add nitromethane to the container (no more than 20% full, and probably less), then insert a plastic pipe with one end sealed
tight, stuffed with black powder.
You see where I'm going with this.
Make sure the nitromethane is airtight, so that none of it actually comes in contact with the powder or leaks from the nexk. Light the fuse and hurl
it from a slingshot, or run away. The confined black powder makes an impressive bang, and an instant later the fire touches the nitromethane fumes and
makes a nice fuel-air-explosion. It ought to look just like a Hollywood-style fireball.
[Edited on 26-6-2013 by killswitch]
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killswitch
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| Quote: Originally posted by golfpro | Holy COW!!!!
I bet you get a firm knock on your door/kicked down instead of these things ever being delivered. Good luck. |
LOL I have ordered a liter of acetic anhydride from eBay and had near-next-day delivery. Been over a week. No Federalés yet.
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killswitch
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| Quote: Originally posted by chemcam | | Quote: Originally posted by Hockeydemon |
What are the potential dangers (serious question) in PETN & RDX synthesis? Up until I nitrate them there is no real danger (explosive danger), and
aren't these two particular explosives relatively insensitive? I'm intrigued about it, but I'm not going to just jump into making explosives.
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When you say "up until I nitrate them" I have to assume you mean the precursors, pentaerythritol and hexamine? There is no explosive hazard from them
before nitration unless you have a certain percentage of the dust in the air but that is 99% unlikely the flash point of pentaerythritol is 200.1 °C, hexamine is flammable but that is the only danger. As long as you pay close
attention to the temperature, continuous stirring and don't leave unattended you should be okay. There is always a risk for a runaway but if you're
aware it shouldn't happen.
RDX has fairly low sensitivity but honestly I only know that from talking with others I have no experience with it. If you are using reagent grade
acids it will be much safer than industrial grade. Impurities always have an effect on the sensitivity.
PETN is actually easy to detonate, I would say it is marginally less sensitive than ETN but I do not have proof of this. I mean both of them are much
less sensitive than primaries but you should treat them all the same, very carefully. You do sound a little too relaxed when talking about these
things but at least you are only in the knowledge acquiring phase. Have you read through this thread? Life after Detonation
Like I have said many times before the first nitration should be cellulose to get the feel for it. |
Not true. I spent several hours drying and grinding up hexamine and spent the next three weeks trying to convince my girlfriend I wasn't cheating on
her. Smell my finger indeed.
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killswitch
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If you wish to look less suspicious in the future, ordering HCl and H3PO4 along with nitric and sulfuric gives the impression you are just buying
mineral acids.
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chemcam
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| Quote: Originally posted by killswitch |
Not true. I spent several hours drying and grinding up hexamine and spent the next three weeks trying to convince my girlfriend I wasn't cheating on
her. Smell my finger indeed. |
Ahahaha! That was a nice comment to wake up to. You're right though hexamine smells like fish or dirty *****.
Be aware of the ones that smell like fish...It's not normal. Lol
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Armistice19
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| Quote: Originally posted by chemcam | | When I do a big flash charge I make several small batches (10g each) then dump them in together once I have made enough. |
10g each?!?! I have made 300g batches before, and shaken them violently in a Ziplock container sprayed with "static guard". Perhaps this was
inherently stupid? I have already decided to attach myself to an electrical ground at the wrist if I were to use flash powder again this year.
Honestly I have enough KClO4 left to make a Key and a half of flash, and I was seriously considering putting it all in one tube with a long fuse.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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Armistice19
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| Quote: Originally posted by killswitch | | If you wish to look less suspicious in the future, ordering HCl and H3PO4 along with nitric and sulfuric gives the impression you are just buying
mineral acids. |
What would I use the H3PO4 for? I don't want to spend money on extra stuff that I won't use.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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hyfalcon
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| Quote: Originally posted by Armistice19 |
10g each?!?! I have made 300g batches before, and shaken them violently in a Ziplock container sprayed with "static guard". Perhaps this was
inherently stupid? I have already decided to attach myself to an electrical ground at the wrist if I were to use flash powder again this year.
Honestly I have enough KClO4 left to make a Key and a half of flash, and I was seriously considering putting it all in one tube with a long fuse.
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You are lucky to still have your arm or life. If that much flash had gone off that close to your body you more than likely wouldn't be here today.
When 50g is confined, it is scary enough, much more than that you start breaking windows.
[Edited on 28-6-2013 by hyfalcon]
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chemcam
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Wow, 300g?! To me that sounds as risky as using a 10mm long fuse. I am usually on the safer side of things though, I think 2g of flash confined could
easily remove a finger or two, 300g would blow you to pieces.
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Ral123
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It's not like there's much difference if you blow yourself with 30g or 300g energetic. You're screwed anyway. I try to use sub 10g and keep distance
from the charge. If I'll blow up more, I try to use stable compounds. I don't understand flash well and I don't trust it much.
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Armistice19
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I had no idea that flash powder was THAT sensitive. I will certainly never do this again. I was under the impression that you could hit this stuff
with a hammer and you still probably wouldnt set it off. I am also confused about the sensitivity after confinement. Theoretically if i made a key and
a half of flash powder 10g at a time and poured it loosley in a sealed container, it would be safer than it would as a free powder? I mean otherwise
why do they make M1000s in eastern countries and sell them? It just doesn't make sense.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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chemcam
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You have gotten the wrong idea from all this, flash powder is not all that sensitive when it is fresh, here I am talking about KClO4 and Al. If using
KClO3 and Al it is ever so slightly more sensitive to friction and impact. However, if KClO3 gets into contact with sulfur for instance in BP you will
be in much danger. The finer the aluminum powder the more sensitive it will be. I have 1-3 micron Al and then also sub-micron Al, the latter is always
easier to set off during testing.
When flash is confined it will explode, when as a loose powder it deflagrates up to a certain amount, 300g of powder would probably explode that's why
you do 10g amounts at a time because the chances of it exploding loose is very slim. I don't even use a bag to mix it, I put it on paper and fold it
then break the clumps up slowly.
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I know you didn't ask this or even mention this but I wanted to say as a safety thing since the forth is less than a week away. I once saw somebody
hot-gluing an end cap on a full 2g flash charge and it exploded, luckily it was in a bench vice and not his hand. If using hot glue I suggest to
unplug the gun and let it cool a bit before it comes into contact with the charge. I didn't think flash could go off without flame or spark but it
happened by just a hot surface, I believe, perhaps it was actually static.
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Armistice19
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Understood, if something WERE to go wrong I'd be dead/armless instead of severely burned.
Even though I did not get to make Nitrocellulose this year, my America Day went well anyway using flash instead. Unfortunately my scale was a rip off,
and was completely malfunctional. I should have known better trying to buy a precision balance for $95 (it is now being returned). Anyway, I noticed
from previous years that my usual 7/3 by weight was visibly close to 5/5 by volume, so I thought I would try a little experimentation. Using a 10mL
graduated cylinder (sprayed with static-guard) I measured 2mL of each component and then diapered. The flash was poured into 3/4" cardboard tubing,
and plugged on both ends with slices from a 3/4" dowel rod, before being wrapped in electrical tape for insulation (anti-static). Surprisingly, for
whatever reason I got a much louder report than I am used to. After making my first test charge I did a quick hammer test, which did very well, having
to slam the hammer down very hard in order to get a detonation. The fuse burn rate was then tested with X2 10" lengths of fuse, and averaged at about
2.8 seconds per inch. 11 charges were made with 12.6 second fuses, and many books, electronics, and aerosol cans were destroyed. Each charge was
successful and repeated the same results as the previous.
[Edited on 5-7-2013 by Armistice19]
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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Armistice19
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Just made my first mini batch of NC. You ever decide to do something, and then halfway through you realize you were completely unprepared? I need
pipettes, funnels, a nice sunny day, and some practice with neatness. I spilled constantly, I thought the fan in the window of my basement would be
enough, but it wasn't, I didn't make nearly enough 1M bicarbonate to neutralize everything, and I didn't even nitrate long enough. This was a scary
learning experience. I need to do this outdoors with a few more pieces of equipment. I even contaminated my sulfuric acid with a little bit of nitric
because I used the same graduated cylinder and then poured the excess back into the container. I'm a total noob with nitrations 
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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golfpro
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You have to think through the play-by-play of the whole procedure in your mind before you do something like that or it'll turn into a big mess.
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Armistice19
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Looks like the final product was still okay on the first batch, even though it was a mess. Second attempt was the best so far. I did it outdoors and
made a very small amount. I had plenty of bicarbonate, and the final product was superb. My third batch I decided to go with and ice bath and a bigger
batch (5 cotton swabs in 125mL bath with about 5mL excess sulfuric). Turns out I created nice thick lumps of plastic with some fuzz on the outside. I
obviously did something wrong. The final product on the third attempt would burn medium fast, but would leave behind sticky slow burning residue.
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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