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quicksilver
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Are there patents? A quick search of "semicarbazide perchlorate" got a 0 return from USPO (but that doesn't mean a thing to me, I got a "0" from a
fuminate search due to dating aspects of the database). Where did you hear of this?
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Rosco Bodine
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Semicarbazide perchlorate is listed with a brief paragraph
in PATR . There is a patent related to its use as a burn rate modifier in solid propellant .
It just occurred to me that it should very likely also have explosive properties , although none are stated for it
in PATR .
It could probably be made via double decomposition of
a semicarbazide salt and a perchlorate salt . Since both
are entirely improvisable from mundane materials ....
this became even more interesting .
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Boomer
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(Also posted on APC, but as some here seemed interested in these mixes...)
Tried a 28mm SC with a cast mix of AN/HDN/UN/NaN/KN/GN/NQ (all the leftovers I had) plus just 10% RDX. Casing was 2.5mm wall steel pipe, 42 degree
copper 0.8mm liner, standoff 1.5 CD. Using 100g explosve (plus 20g RDX-plastique booster), it went through approx. 50mm of steel.
The pic shows the first two plates (20+25mm). To the right is the entrance hole of the top plate, to the left the exit hole of the second plate. I did
not bother to carry the last plate where it got stuck to work:
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quicksilver
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Nice pics, interesting mix too! No reason for a wild "left over" mix like that to not proform well. What -were- those plates? They look lke old USGS
markers or old weight plates from a gym 
I know this is OT but with the Holidays around the corner, I had once found that old X-Mas decorations can make workable SC liners; as some of the
ornaments for x-mas trees are glass, Al, etc. Sawed in half, they form workable SC shapes.
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Boomer
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Weight plates from the gym? No those holes were *not* there before! 
BTW I can go look up the mix, even though it was leftover stuff, all components were weighed. Oh and the liner was hand-rolled around a metal cone,
using four layers of 0.2mm copper sheet and super glue.
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nitro-genes
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Hehe, that's funny....I have got exactly the same steel plates. There was a whole pile of these in all kinds of sizes at some scrapjard where we
bought them. I think the holes in the sides are made to make sure they can't be used again...(for whatever purpose that me be)
If your charge was 28 mm in diameter, I assume you had quite a bit of subcalibration included for 100 grams of explosive? Or did you use a large head
height? Too bad you didn't make a photo of the charge itself...
How did you fill the charge? Pourloading or pressing? Nevertheless, the potential of these eutectics is clearly quite high, especially at larger
diameters...
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Bert
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The discs are the cutout scraps from an automated torch cutting machine. The "T" slot is where the torch makes a first perforation before beginning to
cut out the programmed shape- It starts away from what will be the finished edge to keep any irregularities from the initial pierceing operation in
the scrap piece.
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Boomer
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Thanks for explaining that, it makes sense indeed: They were from the scrap pile of a place specialised in cutting steel to shape. Unfortunatly they
are down now. No more plates buhuuuu. 
No subcalibration was used, and approx. 1.5 CD head height above the cone. Density was 1.5 so do the math yourself. It was melted in a hot (~80C)
water bath, then spooned in and tamped down while cooling.
Oh and the comp was 93g of 40/15/15/10/5/5/10 AN/UN/HDN/NaN/KN/MAN/RDX (formula 50 from above) plus 5g GN + 2g NQ. The latter were added to see if
the m.p. would drop further. In fact it could be hand moulded comfortably, and barely set hard at RT.
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Rosco Bodine
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Here's another interesting melt composition .
Attachment: DE1057514 AN + Ca(NO3)2 + Mg(NO3)2 eutectic + PETN + RDX cast composition.pdf (118kB)
This file has been downloaded 1156 times
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nitro-genes
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Interesting composition Rosco, though a larger quantity of anhydrous Mg(NO3)2 would be rather difficult to aquire, at least not by heating the
hexahydrate. The patent explicitly mentions the anhydrate though as they write that the presence of any water reduces performance and the stability on
storage...
Another composition that's a really interesting possibility is the eutectic composition of 50%/50% Ethylenedamine dinitrate/AN, forming a clear melt
at 102 deg. C. with good oxygenbalance and less hygroscopicity. it is also less acidic than urea nitrate and more stable than hexamine dinitrate,
mentioned in Boomers eutectic compositions, which can pose some stability problems on storage. Ethylene diamine is not very OTC though, although I
have been able to aquire 250 ml's of it relatively easy...
[Edited on 18-1-2007 by nitro-genes]
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Boomer
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After a closer look, the patent mix contains PE, not PETN! It is added as a fuel and an organic flux.
25% RDX - no wonder it performs well, I used 10% only in the above test.
The second mix (that nitro-genes mentioned) is similar to EAK, but melts higher without the K-nitrate addition. With the abrevations EAK and NEAK
existing, would this be called EA then?
And yes I plan to leave the HDN out, I assume it is the culprit for the stuff gassing while hot, and being springy/spongelike while it hardens (it
tried to squeeze itself out of the casing, I had to put a clamp on until cool). While this gives small cavities to promote det transfer, it also
lowers density. And you never get consistent charges if density depends on colling speed and the time it was molten.
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quicksilver
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I just made a trade for some perchloric acid (techgrade I assume @ 68%) which cost from my side about $30 a gallon....what's the going rate? Was that
a fair deal as the trade material really was worth close to 30 dollars (high grade Ekheart Al).
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Rosco Bodine
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I have some indications and suspicions that possibly the only way of producing anhydrous Mg(NO3)2 is from direct union
of the metal itself and acid , under special conditions , or
some other strategy which involves the formation of the
anhydrous salt bound to or formed in parallel with another
salt . I have some more ideas and references on this
which I am posting in the other thread where salts are being
tested for usefulness in nitrolysis of HDN to RDX .
These eutectic or useful lowered melting point mixtures of nitrates have probably been charted somewhere in the literature and I think it is mentioned
in the patent . We should try to accumulate a list of these mixtures which have
interest and possible usefulness . The matter of low melting
mixtures which involve dehydrating salt(s) which easily lose
their crystal water in combination and form an anhydrous double salt stable in a neutral condition , but will be split by a lowered pH as is present
in a nitration mixture are of interest to me . I saw other eutectics reported while searching for any peculiar in that dehydrating characteristic
and here is one .
80 NH4NO3 / 20 NaNO3 mp. 120C
And here is another
2 Ca(NO3)2 / 54 Mg(NO3)2 / 44 NaNO3 mp. 138C
See US1952849 concerning this tertiary eutectic .
[Edited on 19-1-2007 by Rosco Bodine]
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nitro-genes
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| Quote: | Originally posted by Boomer
The second mix (that nitro-genes mentioned) is similar to EAK, but melts higher without the K-nitrate addition. With the abrevations EAK and NEAK
existing, would this be called EA then? |
Yes, it was mentioned in some los alamos report, the abreviation they used was indeed EA. A slightly lower melting eutectic was also mentioned with
addition of KN, though the VoD was significantly lower with a minor addition of KN compared to the composition without. Something like 6600m/s for EA
and 5300m/s with addition of KN... Very strange...
I noticed the same thing for the compositions containing HDN btw. When you press the composition in it springs back to it's original position. When
you tap the container you can hear by the sound that there is a lot of voidspace in there. I wonder if it could also have something to do with the
high acidity of UN, making the HDN decompose at lower temperatures than it normally would...
[Edited on 19-1-2007 by nitro-genes]
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Rosco Bodine
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@nitrogenes & others fluent in German as my German is
*very* marginal and minimal  ( as if that isn't obvious )
Please look at the reference for eutectics mentioned in that German patent posted above , which relates to E. Janecke , Zeitschrift fur Elektrochemie
1943 , Bd. 48 , S. 453 .
Is the context for that reference more general as to describe
a charting of many more eutectics than the one mentioned 51 Mg(NO3)2 / 49 NaNO3 ?
If it is a general charting of other nitrate mixture eutectics ,
I am thinking that we should get that chart for any further reference value it
may have .
It seems likely that a bit of urea or glycine and perhaps some other things could be added to further reduce the mp.
of that nitrates mixture described in the German patent .
Perhaps with some added components a very good oxidizing
salts mixture for a melt in fuel type emulsion could evolve from this .
I am also very interested in these mixed nitrate systems
for their possible usefulness in nitrations , and also perhaps
usefulness for improved distillations of HNO3 .....even those
where sulfuric acid is also used . These mixed nitrates may
provide a way to add some finesse to already known reactions ....improving the yields while decreasing the
rigorous and sometimes even extreme conditions which
are otherwise required .
[Edited on 19-1-2007 by Rosco Bodine]
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nitro-genes
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The replacement of the coordinated water by the formation of a double salt is something I hadn't thought about, but seems logic indeed. If I
understand it right, the PE is the fuel component that can also dissolve/emulsificate in the eutectic forming a solution of fuel in eutectic. This is
very interesting, obviously a whole range of alcohols can be added as well, just like amines, because of their high polarity which makes them soluble.
This brings interesting new probabilities, like adding glycerol, mannitol or even sugars, like glucose, sacharose or fructose (although these wouldn't
be as resistant to heat, given their resonant aldehyde group) or even using sodium or potassium oleates as a fuel component in the eutectic...
In this respect it very much resembles emulsion explosives containing AN and some oil as the fuel, the more intimate contact between fuel and AN makes
the VoD go up. When liquified there is an even more intimate mix, making the mixture behave like it was an ideal monomolecular explosive...
I would still like to see some VoD measurements though from these explosives, since I'm still convinced that a large percentage of inert cations like
Ca, Mg or Na will have a reducing effect on the resulting VoD compared to compositions without. The patent stated performance better than TNT in
leadblock expansion tests, though contained a relative large amount of RDX compared to some compositions mentioned in the los alamos works, just like
Boomer said.
[Edited on 19-1-2007 by nitro-genes]
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Rosco Bodine
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Sorbitol might be a good addition .
Sulfur and/or Sulfides too .
Powdered charcoal/lampblack is another possibility .
Ammonium picrate would seem good too .
Ethylene glycol is known to be a solvent fuel
and sensitizing component which lowers the mp
even further of such mixtures , and flake aluminum
is a sensitizer and brisance enhancer .
It really is key to use the *mixed* alkaline earth
nitrates to " break the water of crystallization "
and provide a path to a eutectic of anhydrous salts
having a reasonably low mp which is not just
the nitrates melting in their own water of crystallization ,
but giving it up in preference for the double salt or
eutectic which is anhydrous .
And I think the *Basic* nitrates probably have value in this regard also , particularly in the case of the Magnesium nitrate . One thing I have
thought about
is a possible usefulness of forming the Magnesium nitrate
in part from a reaction of the basic carbonate with
ammonium nitrate in a melt .....where the nascent CO2
evolution would foam and loosen the melt and the escaping CO2 would carry with it much of the water vapor also . Such a lowered density foamed
composition might have easier pulverizing as it solidifies to the anhydrous mixed salt , while still hot , being crumbly
instead of setting up like a cooled glass as some melts
will be certain to do .
[Edited on 19-1-2007 by Rosco Bodine]
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nitro-genes
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I was thinking, reverse emulsion explosives are made by adding an oil with emulsifier dissolved in it to a liquid eutectic mixture of AN/SN/CN or
AN/KN/H2O at melting temperature...
But what if you would add only the emulsifier as the fuel, like sodiumoleate, sorbitanoleate (a commonly used emulsifier for emulsion explosives) or
sulfonated benzene detergents to make the mixture oxygenbalanced? Then add 10%-50% RDX or PETN to increase sensitivity and VoD and decrease critical
diameter. These emulsifiers are commonly available as detergents for all kind of things, making a very cheap and storage stable high brisance
explosive. Ethylene glycol and glycerol (higher boiling point) would also be very interesting fuel components...
I expect performance to be lower than EA, or EAK, but it would still be a very interesting possibility...
[Edit] Performance using glycerol would probably be less than using these detergents as half the mass of the glycerol is made up by the oxygen from
the hydroxyl groups. Just like the inert cations like K+, Na+ etc, it would take up a lot of the energy from the shockwave, slowing it down. You would
need to add about 6-7% of the detergent as a fuel compared to an estimated 15% for glycerol, so that would mean more than 7% inerts in your mix when
using only ethylene glycol or glycerol as a fuel. I could however be useful for lowering the melting temperature of the initial eutectic just like
water can do with only 2-3% added...
[Edited on 20-1-2007 by nitro-genes]
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Rosco Bodine
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Lanolin is the most common emulsifier that can also
function as the fuel . And a percentage of Ca(NO3)2
tends to act as a dispersant of sorts for other mixed salts , and facilitates the dispersion of sulfur and other materials as well .
There actually have been produced sensitive and powerful emulsions which are so effective at having an inherent tendency to form a stable and
homogenous dispersion , that no more mixing is required than simply pouring the warm ingredients together in a bucket and
stirring by hand for a minute or two with a paddle .
The mixture self-emulsifies without any high shear mixing and then gels and sets up on cooling . The only cap sensitive composition which I have
seen reporting this used a highly specific emulsifier which had been developed precisely for this use and it was a patented formulation . But there
are probably small booster sensitive emulsions which are possible from OTC materials . And these are brisant explosives more powerful than TNT
....generally something like 75%
blasting gelatine in power but much safer , cheaper and easier to make . It is these emulsions which are used for hard rock blasting operations ,
mostly as a substitute for the original NG base dynamites . Some water gels
are probably equivalents also .
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Rosco Bodine
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This thread seems to be the proper place to continue to post any eutectics or other interesting mixtures of nitrates which are found reported in the
literature .....
( even though the thread title is
*perchlorate compositions* )
it probably is a good sneaky way to shield the thread from
all the predictable and superfluous AN + fuel composition discussion which would miss the point concerning the unusual fusible and or reactive
mixtures whose discussion has found a sanctuary here .
Anyway , here's another eutectic from Urbanski .
66.5 NH4NO3 / 21 NaNO3 / 12.5 KNO3 fp. 118.5C
And I found an old patent regarding the use of a carbonate
of an alkaline earth metal in reaction with a low water melt
of NH4NO3 , which concurrently produces the nitrate of the
alkaline earth by double decomposition , with the expulsion
of water lost to the evolution of byproduct ammonia and
CO2 at the heat of the reaction .....so that a crumbling product more easily broken up on stirring while cooling
is the result . This patent relates purely to the Calcium
salt .....but it may possibly also apply to the Magnesium
salt or a mixed dolomitic system as well .
[Edited on 20-1-2007 by Rosco Bodine]
Attachment: GB383663 Carbonate of Alkaline earth reacted with AN to form granular product.pdf (168kB)
This file has been downloaded 701 times
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Rosco Bodine
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Zinc can form a diammine zinc nitrate from similar reaction if the temperature is limited , but at a bit higher temperature
the diammine zinc will lose its ammonia and the anhydrous nitrate will remain
This is of interest by itself ...but also in relation to Magnesium nitrate which is most difficult to be gotten in a low hydration condition
......since there is a combination
of Zinc and Magneium nitrates which forms a eutectic
that is more easily dehydrated .
The inference is that some concurrent and/or sequential reaction of the carbonates , basic carbonates and/or oxides
of both Zinc and Magnesium with a low water or anhydrous
eutectic melt which is largely NH4NO3 ....may result in a
nearly anhydrous mixture of the Zinc and Magnesium nitrates
which has the crumbly physical nature as would make it useful for being able to be added and dispersed as a
dehydrant in a nitration mixture . A minor percentage
of Calcium might be useful also in such a mixture , as could
some basic nitrates , which may not as tenaciously hold onto
any water in the mixture where they are formed , but would
be converted to the normal nitrate in a nitration mixture whereupon their dehydrating value would manifest .
Attachment: US5071630 Zinc diammine Nitrate.pdf (485kB)
This file has been downloaded 770 times
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Boomer
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The eutectics mentioned above, using only AN plus an (earth)alkali metal nitrate, all have melting points around 115-120C. To make it pourable without
having it solidify instantly when it touches the container wall, you have to go approx. 20C above the mp, which gives 135-140C as the working temp.
Apart from having to use a stinky/messy oil bath instead of a water bath, these temps are too high for my taste to add any RDX, let alone a nitrate
ester.
Using an emulsifier or flux as a fuel is something I did not think of before. Instead, I tried to get zero OB with nitrates only, namely organic
nitrates which all have negative OB. In fact, all mixes I tried have slightly negative OB, between -2% and -15% mostly. This was partly caused by the
use of HDN with its bad OB compared to e.g. UN. Since I want to get rid of it anyway, what more stable nitrates would you people think best, GN,
EDDN... (I am not gonna use ALL together again, no way - it was just a test, plus a disposal of leftovers)?
BTW I tried AP, but it did not seem to work well. At least I had the impression it did not dissolve well below 110C, no surprise being a picrate, not
a nitrate. Plus, it is incredibly messy, staining everything including the chemist yellow
Most inportantly, the compatibility with metals goes from bad (corrosion with very slow decomposition) to worse (possible generation of primary
explosives in situ)! 
[Edited on 20-1-2007 by Boomer]
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DeAdFX
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You could use nitrates of amino acid. Like glycine, creatine, agrinine and histdine. In my limited time of using glycine nitrate it did not seem to
be overly hydroscopic[using NH4NO3 as a comparison]. I have not tried the other amino acids. Amino acids are a little more pricier in comparison
to urea/hexamine/guanidine nitrate/ but are probably easier to acquire. All the listed amino acids except for glycine are going to throw off the OB
of your current explosive eutectics into the far negative.
[Edited on 20-1-2007 by DeAdFX]
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Rosco Bodine
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To some extent you may view any of the eutectics
as intermediates to facilitate mixing with other
reactive materials whose reaction products result in
a different final composition .
For example suppose you are reacting other materials with ammonium nitrate which would be the most common means of producing a nitrate by double
decomposition , using an oxide , hydroxide , carbonate ,
or basic carbonate of the alkaline earth desired to
be converted to its nitrate ......it can be useful to use
a lowered melting point mixture of what is predominately
ammonium nitrate , as opposed to pure ammonium nitrate and water .....if a more anhydrous product is
desired at the end .
A specific example would be the case of the Zinc diammine nitrate above .....which could likely be made
from the reaction of Zinc Oxide with the tertiary eutectic
of 66.5 NH4NO3 / 21 NaNO3 / 12.5 KNO3 fp. 118.5C being used as the source of NH4NO3 instead of a 95%
solution of the NH4NO3 in water . Not only could
the quaternary system resulting be anhydrous .....
but it could also have a much lowered melting point
than the unreated mixture of the four components ,
if you follow the logic which applies . So it is not
so much the importance of any specific eutectic ,
as is what may be the end result of utilizing that
eutectic as an intermediate in the process of forming
some product beyond that eutectic ......as could
even occur from a blending of two different eutectic systems . There are even possible supercooled melts
of different nitrates which will stubbornly remain liquid
at room temperature and will set up only after days
time , or upon seeding with crystals . These peculiar
systems are very interesting .
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nitro-genes
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| Quote: | Originally posted by Boomer
The eutectics mentioned above, using only AN plus an (earth)alkali metal nitrate, all have melting points around 115-120C. To make it pourable without
having it solidify instantly when it touches the container wall, you have to go approx. 20C above the mp, which gives 135-140C as the working temp.
Apart from having to use a stinky/messy oil bath instead of a water bath, these temps are too high for my taste to add any RDX, let alone a nitrate
ester |
Yes, you are absolutely right, in order to make HE additions we should aim for melting temperatures of around 100 deg. C. at the maximum. For RDX this
could possibly be 10 degrees higher...
In terms of the most easily prepared eutectic liquid base the following seems pretty interesting, as it melts around 100 deg C, probably even lower:
77% AN
15.5% KN
7.5% H2O
About 7% of emulsifier could be added as the fuel along with 20-60% finely powdered RDX or PETN to make the composition det sensitive...
The water could possibly be elimitated from the mixture using ethylene glycol or glycerol as the fuel, to form a composition something like this:
72% AN
14% KN or SN
14% glycerol or ethylene glycol fuel
[Edited on 20-1-2007 by nitro-genes]
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