vulture
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ETN / PETN ( 2 / 5 ) Melt Composition by Mr. Anonymous
An experimental melt castable PETN composition has been made for evaluation of an alternative method to press loading the base charge
in a compound detonator.
It has been found that by blending dry
crystals of ETN and PETN in the ratio 2 parts of erythritol tetranitrate
(m.p. 61 degrees Centigrade) with 5 parts of pentaerythritol tetranitrate,
that a suitable mixture results.
The dry blended powders will slowly
fuse into a stirrable dense slurry after about 30 minutes exposure to the
heat provided by a water bath maintained at 75 degrees Centigrade.
A slightly warmer bath , perhaps 80 degrees may hasten the melting
and blending.
The Erythritol Tetranitrate tends to melt slowly and it also appears that the molten ETN has solvent properties towards the PETN.
Because the molten ETN is mildly viscous , the mixture requires some stirring to evenly wet all of the PETN crystals and form a smooth molten slurry.
It is something like mixing dry sugar which is wetted very gradually and increasingly by syrup, slow heating and
stirring the viscous mixture is required until the mixture is uniformly
blended.
Before the warm mixture is stirred it has the appearance of
a slightly damp powder, and the damp powder gradually melts into a
slurry as it is stirred.
After the melt is uniformly blended , it
consists of a continuous liquid phase in which is suspended solid crystals of
undissolved PETN.
The consistency of the melt composite is similar to what would be observed if just sufficient fiberglass resin was mixed
with fine sand to completely fill the spaces between the grains and form
a stiff paste. The density of the solidified melt is 1.69.
It does
not appear to shrink upon cooling in small sections.
The melt has mildly
adhesive properties for polypropylene , but does not attack the material ,
so unwanted residues are easily removed with a swab moistened with
acetone.
Polypropylene culture tubes 5ml , 75mm X 12mm were used
for tests of the consistency of various ratios.
Sample mixtures ranged
from 1.8 to 3.8 grams, and the volume for the 3.8 gram sample was
less than half the capacity of the culture tube, occupying 2.25 ml after cooling and solidification of the melt.
The useful percentage of ETN
for producing a smooth slurry may vary somewhat depending upon the
mesh of the PETN crystals which remain undissolved.
The range of percentage for ETN found to be useful, related as a percentage of the
total combined weight of ETN and PETN in the composite, was found
to be 26 to 36 per cent.
Lesser percentage of ETN did not fully
submerge undissolved PETN in a continuous melt, and greater amounts of ETN resulted in a layer of clear melt excess above the undissolved PETN
slurry.
The object was to form a smooth, solids filled slurry free of voids and
this was accomplished by percentages of ETN in the above range for my particular sample of crystalline PETN which has a granulation mesh similar
to table salt. The compaction and stirring of the warm test melts was
performed manually upon the tubes in the bath using a bamboo skewer about 3mm
diameter .
Initiation sensitivity tests on the 2 / 5 ETN / PETN melt cast composite
have not yet been performed.
The initiator which will be used for the
experiments will be the 4 / 12 azo-clathrate which was described in an
earlier communication.
A quarter gram of the 4 / 12 moistened with dextrine solution to form a putty , deposited on the surface of the 2 / 5 composite and allowed to dry
for a couple of days , should guarantee its reliable
(overdriven) initiation.
The sensitivity of ETN is a third greater than PETN so this should offset
any loss of sensitivity as is sometimes observed for cast compositions.
I have not been able to find any references concerning a 2 / 5 ETN /
PETN
melt cast composite.
At this early stage of evaluation it appears to be an interesting composition which could be useful, perhaps equal or even superior to press loaded
PETN compositions.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Basement Chemist
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i wish i was mr anonymous
I am curently hiding from the DEA...
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Mumbles
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I may need to try out making some ETN. This is really the first time I've ever really seen it. The only other time was on the DEA list of
explosives. I just thought it was the samething as PETN, only with a different name. I did some looking around and found very little information.
They briefly mention it on the E&W. I believe it is mentioned in a few books. Urbanski, and the Preparatory Manual of Explosives are two.
Unfortunatly I have no access to either. At least in a readable form. I should learn German.
Another driving point is the extreme low cost of the main precursor. Around $9 a pound I believe. Its sold as a sweetener. I'm going to search
for some here, and if all else fails order it from the internet. This is very interesting.
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vulture
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ETN/PETN patents by Mr. Anonymous
US1691954 production of Erythritol Tetranitrate
US1660651 similar method
US2370437 efficient simple method works extremely well for PETN ,
using density 1.5 HNO3 containing one half per cent urea nitrate
and nitrating at 18 to 23 degrees for one hour ,
however the same method works extremely poorly for ETN
probably because the ETN does not precipitate as it is formed ,
but remains dissolved in the acid where it produces an unfavorable
equilibrium shift for the nitration reaction .
US2204059 excellent recrystallization method , recommended to use warm
water instead , containing about two per cent each of urea and
baking soda , and also to pre-neutralize the acetone solution with
a small amount of ammonia water . This method produces a very
highly purified and stabilized , dense crystalline product .
US2616920 shows usefulness of urea in aqueous phase for improving
the heat / storage stability nitroesters being recrystallized
GB343485 shows usefulness of paraffin as a graining additive for
pressed compositions
GB364624 shows high temperature nitrations are possible , whether
this is advisable or not .
US1850225 Inositol Hexanitrate , possible PETN substitute
US1951595 detonator application using inositol hexanitrate
The nitration of ETN dissolved first in excess sulfuric acid ,
to which is then added in small portions a solid nitrate may also be
a valid method , but I have not yet tried this . Caution should be
used since ETN is one of the more sensitive nitroesters , even though
it is reportedly stable . The literature supplies so very little information
concerning ETN , that ETN compositions are most definitely “experimental” .
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Nick F
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This is something I've wanted to try for a long time. I was considering using pure ETN, but was worried that it may contract / crack upon
cooling. Using it with PETN should reduce this risk since there is less molten material.
I don't mind pressing base charges, but I HATE pressing the primary, therefore I've been trying to find something to bind lead or silver
azide with, to form a hard, solid material, without much loss of performance. So far nothing has worked very well, starch and similar materials work
OK, but in my experience leave a crumbly product. I'm also wondering about mixing lead or silver azide into molten ETN. Those primaries are
sufficiently stable, but it would still be very scary, just because a pyros mind instinctively knows that it's a dangerous thing to do to heat a
primary. I imagine that only a relatively small amoutn would need to be incoorporated into the ETN to render it flame-sensitive, but testing would
need to be done... what do you lot think about this?
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vulture
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New message from Mr. Anonymous:
Initiation Tests of ETN / PETN 2 / 5 Melt Composition
A few preliminary tests have been performed to obtain
general information about the characteristics of the 2 / 5
ETN / PETN melt composite . The composite is not nearly
as sensitive to initiation , compared to the press loaded
PETN compositions described in the literature . There
also seems to be a capability for both low order detonation
and high order detonation , depending upon the quantity of
initiator used to effect the initiation . When just sufficient
primary is used to produce complete detonation of a small
amount of the composite , like two grams or less of the 2 / 5
having light confinement in a plastic tube and with three
tenths gram of 4 / 12 azo-clathrate primary lightly pressed
on top , with a tenth gram basic lead picrate loose igniter
fired by fuse , a low order detonation occurs which does
not show significant velocity nor brisance . The capability
for both low and high order detonation is revealed by many
explosives , including blasting gelatin , where the full velocity
is only realized if the initiator charge is sufficently powerful .
A subsequent test was done on a three and one half gram
charge of the 2 / 5 composite , topped with eight tenths gram
of the 4 / 12 azo-clathrate lightly pressed , and a loose igniter
of one tenth gram basic lead picrate fired by fuse . A positive
high order detonation was produced . For the 2 / 5 composite
to high order detonate requires about half as much initiator as
does picric acid under similar conditions of light confinement
for a 9 mm diameter column of the material .
The high order detonation of the three and one half grams
of 2 / 5 was surprisingly brisant , and produced very
little smoke . The initiation test was done in a two foot deep
hole in the ground about a half foot in diameter , and the 5 ml
polypropylene test tube containing the charge was taped to the
outside surface of a one inch square structural aluminum tube
of one sixteenth wall thickness , staked in the center of the hole
to half the depth and a solid concrete cover weighing about
twenty-five pounds was placed over the hole . Upon detonation ,
a three inch section of the square aluminum tube was granulated
to small shards and blown completely away while the rest of
the tube was left as two badly twisted and torn pieces .
The concrete cover was blown a foot and a half into the air ,
and fell back partway into the somewhat enlarged hole which
it had covered completely before the detonation . The soil around
the opening of the hole was dislodged and scattered in a ten foot radius .
Having observed these effects for a three and one half gram charge ,
I have concluded that three and one half grams is probably more
than the minimum amount of 2 / 5 which would be needed for
an entirely serviceable detonating cap . Somewhat smaller charges
should be adequate for the initiation of even relatively insensitive
energetic materials .
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Axt
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By what methods was the ETN neutralised?
For me, when initially precipitated from the acid mix it forms a very fine powder (very VERY fine) which is good. But recrystalistion from acetone
results in fine thin crystals (about 5mm x .05mm) which is less desirable.
Therefore I dont recrystalise, only water/bicarbonate/water.
#8 dets that contain PETN only have a base charge of 0.45g, so yeh 3.5g is overkill (though improvised dets should be a bit overkill).
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a123x
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Does anyone here happen to to have a good comparison of power of ETN with other explosives? The only thing that I've been able to figure is that
it would be similar in strength to NG because ETN has a very similar structure and oxygen balance to NG. It's pretty much a four carbon chain
with a nitrate on each carbon and NG is a three carbon chain with a nitrate on each carbon. Anyway, just a suggestion for anyone searching for more
information about ETN is to try butanetetraol tetranitrate, it means the same as ETN and I've seen it called butanetetraol tetranitrate once.
It's unlikely you'll find much more info but still might be useful.
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KABOOOM(pyrojustforfun)
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commercially available ETN!
ETN is used as medicine (diluted with lactose in non-explosive tablets). just wash with water through filter paper, let dry!
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Mumbles
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Erythritol is commonly sold as a sugar substitute. Well maybe not commonly sold, but available fairly easily. What would be the point to buy it as
medicine? Is this medicine even OTC? I don't know of that many OTC blood thinners. I am just assuming it is a blood thinner, as most Nitrate
salts used in medicine are. I doubt the medicine would be cheaper than $20 a pound(estimated).
The only power information I can find is that the VoD is about 7400 to 7700 mps.
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IgnorantlyIntelligent
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How about a ETN/NG brick explosives?
I was told (although I didnt do the math myself) that about a 85/15 ratio of ETN/NG would have an almost perfect OB. Does anyone know if this may be
true? How easy/hard is ETN to detonate on its own?
One could just use a small AP det. right?
Also, I found a site that sells Erythritol by the pound for $6.00 & shipping is only about $5.00. to anyone in the US.
http://www.n101.com/Static/Products/erythritol_HRITOL1543.ht...
\"People fear from ignorance what they do not have the intelligence to understand\"
\"Religion is the sigh of the oppressed creature, the heart of a heartless world, just as it is the spirit of a spiritless situation.\"
\"A fool would rather not question, a soldier is taught not to question, a slave dares not question.\"
\"To fight for nothing is to love nothing, to die for something is to have lived for something.\"
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a123x
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No mixture that contains only ETN and NG will have a perfect oxygen blance. They both have a positive oxygen balance so combining them does nothing to
equalize that.
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IgnorantlyIntelligent
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Sorry about the false information, I was only quoting my not-so-smart friend Ross. I do not know much (obviously) about ETN. It's new to me and I
have not read anything about it except its VOD and its synthesis. I have 2 videos of ETN detonating (complements go to axt for the vids). I will post
them if anyone wishes.
I plan on making 20g of ETN as soon as I get my Erythritol in the mail. I will post results. Before i go experimenting with this material I was
wondering if anyone could tell me how sensitive it is?
\"People fear from ignorance what they do not have the intelligence to understand\"
\"Religion is the sigh of the oppressed creature, the heart of a heartless world, just as it is the spirit of a spiritless situation.\"
\"A fool would rather not question, a soldier is taught not to question, a slave dares not question.\"
\"To fight for nothing is to love nothing, to die for something is to have lived for something.\"
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metal raven
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can any one tell me what ethirol is used for thank you very much
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rooster
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Erythritol is sold as a sugar substitute. I can get erythritol from a lab, but it is labelled meso-Erythritol, is this the same? Are there two
different isomers?
Will attempt synthesis of ETN soon. Anyone knows a H2SO4/HNO3 route?
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Flying Dutchman
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It's the same
Erythritol and meso-Erythritol is the same thing.
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K9
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Yep they're exactly the same.
Apparently while using HNO3, yields are seen to be decreased. Keeping the acids cool while mixing them and leaving the acid mix in a fridge overnight
prior to the nitration is supposed to prevent the problem of the decreased yeild.
[Edited on 29-10-2003 by K9]
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Axt
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Heres an Email I recieved by Mr Anonymous in reply to my question on recrystalisation.
| Quote: | Originally emailed by Mr Anonymous
Axt , Experiment recommended for recrystallization of ETN using warm ( 55 degrees centigrade ) denatured alcohol as the solvent , neutralizing with a
small amount of solid urea and sodium bicarbonate added to the rapidly stirred warm alcohol solution .
First use only sufficient denatured alcohol to form a saturated warm solution of ETN , and then add additional excess alcohol in an amount about
twenty per cent excess of that which was required to form the saturated warm solution , to drop the solution comfortably below saturation . To the
well stirred warm alcohol solution add a small amount like a couple of grams each of solid urea and sodium bicarbonate.
A small amount of strong ammonia water can also be used if desired but don't overdo it . A warm ( 45 degrees centigrade ) aqueous solution up to
about two per cent each of urea and sodium bicarbonate is added dropwise to the rapidly stirred warm alcohol solution to bring about a gradual
preciptitation of the neutralized and stabilized , purified ETN crystals.
A few ice cubes dropped into the swirling mixture when the addition of the aqueous urea-sodium bicarbonate solution is begun will cause the formation
of many very small crystalline nuclei in the vicinity of the melting cubes . These nuclei will grow larger as the addition of the remaining warm
aqueous solution continues . Chill the mixture with more ice cubes to complete the precipitation . Rinse and filter and dry the crystals . ETN makes a
good energetic binder for melt casting PETN slurries which solidify on cooling.
Various other fillers are worth experimentation , RDX would probably do nicely , and even double base smokeless powder of the spherical variety might
make interesting cast compositions . For example Accurate Arms No.2 or No.5 cast in ETN might be a good experiment . In casts with PETN , my
observation is that the cast composite is less sensitive than is usual for the filler material alone , so the composite requires a strong initiator
influence to get it to show its true potential . But the output is very high from these dense cast charges once they do detonate at their full
potential velocity . I would estimate their performance is up there in the same category with the specialized military high output compositions , good
for metal cutting and other tasks which require high output from a compact charge.
The prospect of an ETN / RDX composite is interesting because of the OTC sources for all precursors . The Erythritol is a sugar substitute . And
hexamine is a trivial synthesis from dissolving mildewcide crystals ( paraformaldehyde ) in blueprint developer ( strong ammonia water ) in slight
excess , and boiling down until crystals of hexamine just appear . On cooling , the hexamine redissolves because of its inverse thermal solubility
curve , to form a saturated solution of hexamine . Instead of trying to isolate the highly soluble hexamine and then redissolving it to make hexamine
dinitrate , the saturated hexamine solution is used directly . To the very cold and rapidly stirred saturated hexamine solution is added slightly LESS
than the amount of theory of ordinary 68 per cent nitric acid to precipitate hexamine dinitrate , which is a precursor for RDX . Hexamine Dinitrate
should be precipitated , filtered ( no aqueous rinsing ! ) , dried and stored dry " in the cold " and not exposed to any excess moisture or
acidity or heat or it will hydrolyze and decompose.
Allow me to make a side note / speculation here that Hexamine Dinitrate should also be an * ideal * precursor for HMTD , although I have never seen a
published method, HMTD should form directly from dissolving Hexamine Dinitrate in a slight excess of theory of 27 per cent hydrogen peroxide , via a
self-neutralizing reaction requiring no additional materials . The reaction should proceed best in the cold , very cold , in the freezer for two or
three days would seem about right. I haven't tried such an experiment but others may wish to try their luck . A further digression , It may be
possible that HMTD forms a double salt with ammonium nitrate under certain conditions. See GB397600 . Other patents of possible interest are GB339024
, GB415900 , GB421138 , DRP263459 , DRP274522 , US2341263 . From my observations , the usefulness of HMTD is restricted to near term
"improvisational use" due to its poor storage stability and HMTD is one of those "keep it dry and in the freezer" items , like
certain organic nitrites and other things having storage and thermal and reactivity issues. END MESSAGE
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In regards to melt casting ETN with smokeless powder, since Mr A. has shown that molten ETN has solvent properties on PETN, as does NG with PETN/NC.
Its likely that molten ETN will have also show collioding with NC, so it likely wont matter what shape the powder is as it will form an ETN/NC
"double based powder". Give it OB with about 5:1 ETN:NC and you should have quite a simple yet potent cast charge.
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Axt
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Seems I overestimated ETN's solvent properties, heres Mr A's response giving reason to the choice of spherical powders. I believe all
winchester powders are double based and mostly ball powders, so their range could be experimented with.
| Quote: | Originally emailed by Mr Anonymous
Axt , ETN has very little solvent effect on PETN and ETN has no noticeable solvency on double base powder. The suggestion for using a spherical double
base powder is because of density and propogation considerations . You have experimented with hemispherical shaped charges so you should appreciate
that each individual grain of a spherical powder in a cast ETN matrix would become the focal point of many jets of opposing "hemispherical shaped
charges", emulated by the ETN matrix . Neat huh ? Experiments could reveal if a particular powder is best for this , and there is probably an
optimum grain size and optimum bulk density for the composite which will be related to which powder is chosen as a filler in the ETN matrix . END
MESSAGE
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KABOOOM(pyrojustforfun)
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all tetritols (4) have been known. only meso-erythritol isn't naturally made. the other tetritols are L- and D-tetritol and a racemic form.
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