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quicksilver
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Air pockets are a problem in respect to efficiency.The polymers (Polyester often enough) utilized in many dbsp are best fused with a solvent that
minimizes the air pockets (thereby creating a solid where there once was a compacted group of particulate) - similar to a extremely heavy NC lacquer.
Somewhere there is a list of those DBSP with higher NG content (TiteGroup 37%; BullsEye 40%, Nitro 100 20.5% AA #2 variable @ 20.5-23%,
Cordite/Ballisite 49%, Chinese ball copy WW231 43% & so on). This packaging emulates the percentages on many common energetic dynamites, etc. The
controlling of the burn rate (& thereby it's use as a propellant) was a duel faced agenda of a heat-oriented primer rather than a detonation - and
the design element incorporated in the physical shape of the powder. Burn rate adjustment & DDT in this area is a science w/ a great deal of
research behind it.
However the mp of Picric Acid is rather high & that of TNT low: low enough to be the material of choice when a cast material was called for. So
the physical shape of the powder can be overcome by the use of a solvent & Picric Acid's high mp can be dealt with by the use of a lower melting
addition (ETN, TNT, DNT, etc). Past efforts to melt Picric Acid were fraught with a great deal of danger & uncertainty.
When hot water was used with Picric Acid (water bath / sand bath graduated heating) the material retained bubbles unless the heat was high enough to
come close to a danger point. {See Military Explosives, Weaver, 1905, 1917}
[Edited on 1-6-2010 by quicksilver]
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The WiZard is In
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No doubt I will be chastised because I had previously posted
this in a different thread, however, I work for free.
The Chemical Gazette
London 1859
Some Observations on the Amount of Picric Acid obtained from Botany Bay Resin. By
Prof. BOLLEY.
The so-called Yellow gum, or Botany Bay resin (the resin of Xanthorrlueahaslilis)
[Xanthrorroea saxtilis] , was indicated by Stenhouse, and subsequently by Warington
and Bottger, as the most abundant source of picric acid. - It was said to furnish 50 per
cent, of picric acid, so that notwithstanding its high price, it was the most economical
substance from which to obtain picric acid.
The author has had numerous experiments made on this subject by his pupils in the
Pharmaceutical Laboratory at Zurich. In these the resin was treated with 10 times its
weight of nitric acid in a retort, and the distillate repeatedly poured back. At the
commencement strong effervescence and evolution of nitrous acid took place
without any application of heat; the action was afterwards assisted by heat, and this
was continued with return of the distillate until the mass in the retort was
completely dissolved to a reddishyellow fluid. This treatment furnished-
Experiment 1. 22-5 per cent, of picric acid (somewhat purified by combination with
potash and reprecipitation by muriatic acid).
Experiment 2. 25-6 per cent, of picric acid (obtained by crystallization from the acid
liquid).
Experiment 3. 15 per cent., and therewith a yellowish powder, consisting principally
of woody fibre, partly converted into pyroxyline.
By treating the resin with alcohol until nothing more dissolved, there was found to
be 16-68 per cent, of insoluble matter, of which 2-5 per cent. was ash. The portion
insoluble in alcohol consisted principally of small fragments of wood. In experiments
1 and 2, but little was to be detected in the residue left undissolved by nitric acid.
The difference in the results of these experiments and those made by others, may
rather be attributed to impurities or differences in the composition of the raw
material, than to differences in the mode of preparation. The statement that 50 per
cent, of picric acid may be obtained from the resin, can only be true in rare cases. -
Schweize- rische Polytechn. Zeitschrift, 1858, p. 125.
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pjig
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@quicksilver ...
Thanks again for your input, it's greatly appreciated... 
I wonder if just dbsp powder is used w/o any other energetic material (dissolved in a solvent) would work alone, if cast in to a case as the main base
charge. ...
Also knowing that when the mix dries it could shrink. Could this be anything to fear, if the base charge is allowed to fully dry, before the primary
is pressed?
Also as a side note,and a bit of curiosity, does fine grade aluminium add to the ddt as it does in tnt? I was pondering the though of making a melt of
nm+dbsp+Al to be cast as a plastic in a SC..
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quicksilver
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Albeit this is OT the question re: DBSP gives rise to transportation issues just as water packing Picric Acid does..
The short answer is - yes. DBSP is exactly what people would imagine it is; an explosive. The propellant aspect is a process of "taming" the
materials via a combination of physical structure and a specific type of "primer" that does not act like a ignition cap.
Thus DOT can issue a "propellant" label for it's production & sale.
In hand-loading (or reloading) there is a phenomenon called "detonation" where too LITTLE powder is placed within a cartridge and the result is a
catastrophic explosion, often resulting in damage to the firearm.
IF the material (dbsp) is altered in shape and form via a solvent, etc and it is initiated by a true primary it will detonate. This has been proven by
various laboratories & experimenters. It also exists in some IED's & documented therein by some military services. I don't have notation of
source listing at hand, but I do know that it exists from various references.
Addition of Al will generally sensitize & generate more heat in a detonation while slowing the VoD to a degree. Heat in an explosion will alter
the overall affect & had been in place for a variety of reasons from anti-personnel to visual observation of an HE round. It's placement in Picric
Acid is not common but it's use with TNT is. The addition to something like DBSP in reference to a DDT is something that has not been professionally
explored. However the detonation modeling (see Davis & Fickett) often used today would show that more generated heat at the time of ignition would
affect detonation in cases where a "borderline ignition exists.
Primers for firearms are often lead stephnate based. in such cases where a primary is "weak" (such as primer composition) powdered aluminum may have a
profound effect in pushing ignition to detonation.
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gnitseretni
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Why make a plastic explosive? Why not mix the NM with a sensitizer (like HNO3 or microballoons) and use it in a SC? Being that it's liquid you'll get
a better uniform density than you'd get with a plastic explosive.
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pjig
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@ Quicksilver, thanks again for your well informed answer..
(AS far as tnp, I dont think Al would be advisable to mix with)
The reason of making a SC out of the dbsp,Al and NM is one, that is not corrosive to metals and safer to handle, and if some where to get on you in
the process. All in All I think it's just the novelty that one can create an OTC explosive ( not that N-acid isn't available ) ,with fairly high
bristance and ease of access to materials.
[Edited on 2-6-2010 by pjig]
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pjig
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@ quicksilver
A quick Q. on compadibility....
I noticed that it was claimed that it may be possible to mix ETN and PA, for reasons of lowering the MP. I was just making sure that there are no
incompadibilities of these( forming dangerous picrate compounds or spontanious reactions ) when mixed in a melt.
I'd imagine that this base charge would form a great compound det. able to initiate most sleepy explosives.
Now as far as a stabilizer for PA would it be needed for storage of the above mix, or would the cast be fairly thermaly insensitive. I'd imagine that
urea may improve the shelf life. It seems both ETN and PA are very sensitive to quite a few different things, I'd hope a melt would stabilize this.(
ETN=heat->deteriorates , PA= dangerous picrates)
One of my fears would be that the PA in the base charge would react with any metals ( electric ematch, squib, or priming comp. ..etc. ) forming a
dangerous cap. One would have to take great care to seal the end of the ematch with wax paper glued on the business end.
PA and NM are used in one patent and shot in a aluminium can by a cap and booster pellet(6g) wrapped in foil....Isn't PA reactive to Aluminium? Pat.
us5140908
I appologise as this is slightly off the main topic...
[Edited on 10-6-2010 by pjig]
[Edited on 10-6-2010 by pjig]
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quicksilver
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Well, all I could add is that patents are not always complete (or totally correct) so take everything you read in a patent w/ a grain of salt.
This is how I would project the issue: you have a nitric ester & a (very) mild acid. Their exposure level to each other would not be for any
lengthy period of time. What's more, I believe that one or more of our senior members has experimented with a eutectic with these materials. frankly,
I have not.
No "red flags" go off when I think about such a combination (ETN/PA).
[Edited on 10-6-2010 by quicksilver]
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Hennig Brand
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Aluminum is one of the things normally considered safe to use with Picric Acid. IIRC the Picrate formed is much less sensitive than the Picric acid it
came from. It will also form very slowly, especially with little moisture and little heat.
I would also like to add that I have been making some Sodium Nitrate from Ammonium nitrate and Baking Soda, and using that in Rosco's TNP synthesis.
It works so much better in all respects than Potassium nitrate that it is well worth it to first synthesis the Sodium Nitrate(I think). I see very
little reason to bother with the Nitric Acid, the results were that much better than with KNO3. The synthesis(TNP) was much less work, and a superior
product.
It takes a while to make the NaNO3 but it is a very simple process, which requires little attention.
Rosco's ratios where I believe 1 g ASA, 4 mL H2SO4, and 1.8 g NaNO3. I found I needed more like 4.5 mL acid to even get all my ASA into solution. I
just did a 50 g batch and will get back with a dry yeild. It looks very good after one recrystalization, better than mine looked after two
recrystalization when using KNO3 I believe. Nice big pale yellow, well formed, clean looking crystals.
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Rosco Bodine
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The composite of picric acid and ETN offers nothing as it is damned near impossible to completely detonate and probably isn't storage stable because
of the acidity of the picric acid adversely affecting the ETN stability. What happens is the matrix of melt cast ETN detonates and vaporizes the
particles of picric acid into a dye cloud without the picric acid being detonated. Picric acid is so insensitive to initiation that it requires the
adiabatic heating provided by the compression of occluded air between the crystals to augment the detonation wave, and filling the microscopic voids
with cast ETN doesn't do the trick. It barely even works with PETN crystals as the filler and is ten times harder to initiate than a compressed
particulate composition. Anyway test it if you like and you will have proof positive just how damn hard it is to detonate picric acid under anything
but very deliberately specific optimized conditions which would unlikely be encountered just by chance. Picric acid will detonate brisantly in a
specifically optimized configuration of loading density and crystalline form. And it will do well in combination with various other materials, but
ETN isn't one of them. The testing of a melt cast ETN / picric acid composite is an experiment which caused me to be further convinced of what I
already knew from other similar experiments, and that is that picric acid is like TNT, not a sensitive explosive at all and is actually quite
difficult to cause to detonate accidentally, and not even all that easily caused to detonate deliberately. That is no impediment however to its
practical use, because under very specific conditions it will go high order very reliably.
[Edited on 11-6-2010 by Rosco Bodine]
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pjig
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| Quote: |
What happens is the matrix of melt cast ETN detonates and vaporizes the particles of picric acid into a dye cloud without the picric acid being
detonated
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That sucks... Thought I might have been on to something here.
Makes sense though, ETN being sensitive to the acidy conditions eventually breaking it down.
The patent posted in my last text was showing the improvement of picric in NM . Seems like a worthy material, probably close to Nitric A and NM. I
guess thats why they used a 6g booster pellet to ddt it.
Do you supose any incapability's are in a DBSP/ TNP mix then..?
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Rosco Bodine
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Yes there is incompatability there for the same reason, acidity attacking the ester.
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Hennig Brand
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OK, for my 50g ASA batch I used about 750mL of boiling water to put the crude product into solution. This was all done in a glass whistling kettle (I
have about 8 of these kettles now, made in Germany, borosilicate, $6 on sale).
I put cloth pot holders under it and several layers of towels around it, and covered the top to prevent cooling due to evaporation. I left it to cool
all night. I have almost exactly 43g after the first recrystalization, which is not the best I guess but it seems like very nice pure stuff.
Once I retrieve what is in the crystalization water I will probably have about 50g Picric Acid total.
I only kept the temperature at 100-110C for ~45 minutes at the end, and I didn't have magnetic stirring for the last stage of heating(I only have
stirrer, not stirrer-hotplate). No doubt there are refinements that I can make to increase yield.
By the way, I have been using 0.4g Lead Azide with my TNP in compound caps. I have been just pressing it right on top of the TNP. Any reason why I
shouldn't do this? I think Rosco indicated that this combination is very compatible and storage stable a while back(I think).
[Edited on 11-6-2010 by Hennig Brand]
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Rosco Bodine
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The older members are keenly aware of the inhalation hazards attendant to nitrations, but we are in receipt recently of a lot of postings from a
younger crowd who evidently from their postings haven't done a thorough study of earlier writings and are likely to be complacent about the dread and
insidious dangers of "oxides of nitrogen", particularly in settings where formal lab equipment and procedure is not being used. For the bold and
careless experimenters who dismiss the inhalation hazard, I would recommend putting your affairs in order before experimenting, including of course
pre-writing your obituary so that surviving family will be spared the anguish of retrospective biography to publish to those still living on earth,
some description of who you were when you formerly lived and breathed in the same world. It would be thoughtful and considerate of others to do these
things as advance arrangements, and such kindness may even help you to get your wings and harp while on your way to join the heavenly choir.
http://www.youtube.com/watch?v=3sgD2JXk4XQ&fmt=18 How Shall I Sing That Majesty ?
[Edited on 11-6-2010 by Rosco Bodine]
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Hennig Brand
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Interesting. I didn't have a proper fume hood, but I was outside with a rather large and powerful fan with cowling sucking away fumes as they came out
of the top of the beaker. Just being outside is more than half the battle usually I think, especially if you are mindful and use the wind ( if any) to
your advantage it can be very effective at limiting your exposure to fumes. I left out most of the details of my experiment, the main reason being
anyone following along in this thread knows exactly what the score is. Also I am not as quick to pad all sharp corners, or remove all danger, just to
make it completely safe for all the dumb-asses out there. All that said I do agree that with Picric Acid the poison gas is by far the biggest risk
factor, and should be always kept in mind when experimenting.
Rosco, do you use any kind of barrier between TNP and Lead Azide in your experimental caps?
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Hennig Brand
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Sorry for the lousy picture, but I am just starting to get the hang of this picture thing. It does kind of show the crystal structure, but the color
is off(it is actually very pale yellow).
43g TNP
[Edited on 12-6-2010 by Hennig Brand]
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Rosco Bodine
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Quote: Originally posted by Hennig Brand  | | I do agree that with Picric Acid the poison gas is by far the biggest risk factor, and should be always kept in mind when experimenting.
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You are not a novice. My message was more directed to all the energetics hatchling newbees out there, as a serious warning deliberately meant to scare
the "bee jeezus" out of them about the "oxides of nitrogen" which can never be dismissed or ignored as a trifling matter.
| Quote: |
Rosco, do you use any kind of barrier between TNP and Lead Azide in your experimental caps? |
No, but I normally do not store any assembled components for any significant length of time.
Truly pure and dry picric acid is very pale colored, and at a low pH may not even significantly stain a paper filter but slightly in spots. That
looks like a nice sample. The slightest moisture even from the air causes it to darken and the color to deepen to distinct pastel yellow or canary
yellow.
[Edited on 12-6-2010 by Rosco Bodine]
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Hennig Brand
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Sometimes it is hard to tell when someone is giving you the gears a little bit, anyway no harm done. Sometimes I am already "primed" if you no what I
mean, especially if 2 or 3 other people already gave me the gears that day.
Thanks for the reply. I also boiled down my crystallization water to between 1/3-1/4 of its original volume and cooled. I wasn't as careful with slow
cooling(no insulation), but it still look very good. The crystals are fluffier of course but still look mostly like good, clean, pure crystals. I had
absolutely no resinous products, or at least non that collected during the boil-down. After drying well it looks even a little lighter yellow than the
main crop, but of course the main crop has much larger, denser crystals. It must be a little less pure, so if I want to purify it more, it should
probably go into the next batches recrystallization.
I obtained about 6.7g from this, so I came very close to 50g TNP from 50g ASA.
Using NaNO3 in place of KNO3 just making this synthesis so much more enjoyable, as well as making it much easier to produce a superior product.
Of course I had to test a little. A little in aluminum foil, a large ball peen hammer, and a small anvil. On the third or fourth wack with the hammer
I got a good bang out of it.
By the way, during the nitration I kept the temperature around 75-80C, using just the exotherm of the reaction to control the heat. I had very
vigorous magnetic stirring for this. After NaNO3 was all added, I gradually heated it up to a final temp of ~115C, with manual stirring for this.
[Edited on 12-6-2010 by Hennig Brand]
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quicksilver
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Notice the collection of crystalline shapes, needles, spires: a whole collection. That would make a pretty nice slide. Fisher Labs had a reagent grade
sample that was packed 30% water and as yellow as I'd seen. we dried some and it still maintained a VERY light yellow (dyed most likely) but was SO
light as to be clear at 100x. My belief is that at the point of bearing all TNP you'll see the clarity but any DNP (aside from the moisture issue)
what-so-ever and you'll never get that transparency.
There's a fantastic book that is available mostly only in the UK called "Fuels, Explosives, & Dyestuffs" - Tooley.
It explained various benzene-ring materials & their idiosyncrasies. A great experiment is to nitrate aniline. The colors, when exposed to other
materials can vary to such a degree that it almost seems unnatural.
I would love to save up for a digital camera for a microscope (especially one with a size gradation). - Good job on that TNP!
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Rosco Bodine
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Any leftover solutions can be treated with KNO3 and left standing to evaporate and reduce in volume. You will recover any significant still dissolved
picric acid in the wastewater as potassium picrate which slowly crystallizes out.
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grndpndr
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| Quote: Originally posted by gnitseretni | | Why make a plastic explosive? Why not mix the NM with a sensitizer (like HNO3 or microballoons) and use it in a SC? Being that it's liquid you'll get
a better uniform density than you'd get with a plastic explosive. |
or a 6/1-6/1.25 IIRC.NM/ 325mesh AL preferably coated w/stearic acid.The patent #US6960267,'05' 'Multi component Liquid exp.comp.+method.Would make a
nice
rel high vis liquid high brisance HE w/o the density /brisance lowering microballoons.If more viscositys needed a small amt(few%by wieght)fumed silica
IIRC Hope I havent made a mistake vis a vis silica viscosity enhance.)#8 cap
The AL will stay in suspension for 24 hrs according to the patent
As its a essentially binary HE its easily mixed in the field from basically 2components the stearic acid can always be added to the AL if its
uncoated.Seems the AL has more requirements than anything,325 mesh,%stearic acid.Abstract claims a small/ med bore HE suitable for
CSC's,EFP's,demolition,breaching,about anything a 7000mps plus high brisance HE can accomplish.
Back on topic this thread keeps getting better as far as Im concerned.Im not sure the DBSP hasnt been discussed before but perhaps that was a
mekp/DBSP composition. Stretching TNP/ETN supplys is no new idea as far as the arts concerned or myself.Ive searched for whats been used in the past
seems limited.Trimonite or TNP/Mononitronapthalene 80/20.Not an answer to bulking the HE but a useful /safe (i assume) eutectic.
And really IMHO only a primary DNP/TNP for use in a composite cap
Ive seen some mention of TNP/AN recently and in older Books.
ETN/AN also sounds worthwhile as a composite/matrix concerned.But If a person has to do more nitrations for a suitable eutectic for SC/efps I would
seriously consider the NM/AL compositions.Particularly where a watertight device suitable for a cast eutectic is used,far simpler possibly superior
results over pressed crystaline HE's.If TNP/AN could be used as just a composition assuming the brisance VOD were similar to amatol 80/20-60/40 with a
room/fridge temp shelf life of 3-6months.Same for
ETN the hope and search for a suitable energetic material to stretch the few ozs I could concievably make per batch were I so inclined.Cleaned up a
4lb sack of Hi yield 16-0-0 Na of Soda as its been my normal nitrate until I began to experience failures,only change was bonide 15-0-0 used prior w/o
problem.Purified HiYield by sedimentation/ decantation followed by several filterings and finally recrystalization to get decently clean Na Nitrate
crystals that were soluble w/o clay etc.Strangely enough the prills appeared relatively white and clean?SUPRISE!!
Problem as carefully as I carried out this process out of 4lbs I ended up w/2lb 2oz of useable NaNO3!.Id be better off buying a 25lb pail of tech
grade even w /hazmat.Half the (inexpensive)LOL, Na Nitrate I assumed
Nice batch Hennig! I see Im not alone in using coffee filters.Ive gone a step further at least for me.I bought a ss wire mesh bowl shaped kitchen
device w/handle, large enough to handle the largest coffee filter,paper towel or cheesecloth,nice because it supports the filters can be placed on
the beaker or jar intended to catch the mother liqour w/ both hands used to pour, also got the next smaller size. Wire Kitchen strainer?!Lots of
useful stuff in kitchen ware! FWIW
@ Roscoe,If the TNP were nitrated w/KNO3 would the saved mother liqour also produce some pottassium Picrate from sedimentation? Thanks!!
[Edited on 14-6-2010 by grndpndr]
[Edited on 14-6-2010 by grndpndr]
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Rosco Bodine
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Ummmm, lemme think, okay.... yes it will
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pjig
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| Quote: Originally posted by Rosco Bodine | Any leftover solutions can be treated with KNO3 and left standing to evaporate and reduce in volume. You will recover any significant still dissolved
picric acid in the wastewater as potassium picrate which slowly crystallizes out.
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I like your conservative view, in making the best use out of all the materials. I hate wasting the leftover solutions, as they can usually be re-used
in the next batch. It make's a lot of sense to recover the picrate out of the waste, as it has it's uses too..
[Edited on 14-6-2010 by pjig]
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grndpndr
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Is NH4NO3 a suitable bulking material for TNP for the short term (<2wks)
in a composite.Perhaps in similar ratios 80/20-60/40.
I recently tried KNO3 after using NaNO3 almost exclusively
synthesising TNP.There is quite a difference.
[Edited on 16-6-2010 by grndpndr]
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Hennig Brand
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I've been gone for most of the last 2 weeks.
Thanks for the compliments Quicksilver and Grndpndr, and thanks Rosco for the insight.
One quick insight. When using KNO3 in place of NaNO3 in a Picric Acid synthesis, the outcome seems far worse everything else being equal. The thinner
nitration solution(with NaNO3) greatly facilitates effective mixing which is crutial to efficient nitration and preventing oxidation. A related issue
is the Potassium Bisulphate(?) impurity also being a much more difficult impurity to rid one's self of when purifying. I could be a bit biased now,
but with NaNO3 this nitration seemed perfectly smooth by comparison, and gave a much superior product to boot. This may all seem pretty obvious to
most, but for me the extent of difference between the two was quite surprising.
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