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Formatik
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| Quote: | | Originally posted by -=HeX=- Would a H2SO4 (w/ SO3) and 70% HClO4 mix work instead of 100% HClO4? |
There might have been a good reason why they used the harder to obtain and handle anhydrous HClO4, than a HClO4/H2SO4 system. Maybe the esters are
incompatible with that acid? Adding to the posts above, SO3 and anhydrous HClO4 are said to exotherm (explode) despite diluents, so oleum might be a
bad idea.
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-=HeX=-
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Well, no way to find out but to try. I am on a break from renovating the lab, today I was selling scrap steel (2 metric tonnes) to a scrapyard and am
too tired to bother renovating. I will try on test tube scale first, and video it  however it could be easter or summer by the time I get to try, with school, tests and spending all my money on an airsoft gun so no money for
chemicals at the moment. I can get 70% HClO4 easily enough, so maybe I distill the stuff maybe.
I worked out that even azides of the compoudfs could, in theory, be formed, so a gas mask is needed for the HN3 because death is not THAT exciting
 and I am not some emo punk who wants to be horribly disfigured. Im innocent http://www.sciencemadness.org/talk/images/smilies/shocked.gi... (looks like wide, staring eyes) I am being oh so careful because I know exactly
how hard being blown apart hurts.
If you give a man a match he will be warm for a moment. Set him alight and he will be warm for the rest of his life.
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Formatik
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With something like HN3 I would be more worried about it blowing up, that compound is so dangerous it might seem to someone that it explodes for no
reason at all. HN3 explodes from the slightest vibrations, things like a rising gas bubble in the boiling liquid which contacts sharply-edged glass
will create enough friction to detonate it. Even its aq. solutions are explosive. And when HN3 which is 97.6% nitrogen, goes, it detonates with utmost
violence and a blue light. 0.05 g of HN3 is known to be enough to vaporize glass apparatuses. 0.7g is enough to blow nearby glass vessels to pieces
due to the pressure generated. Curtius was quadruple distilling to get concentrations like 91% but he circumvented what makes it tick.
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The WiZard is In
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ethy perchlorate
Attachment: Chem Ethyl perchlorate.txt (10kB)
This file has been downloaded 1212 times
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Formatik
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Roscoe description of EtClO4 is also in Ann. 124, 124.
| Quote: | | ... in explosive violence, it is not surpassed by any substance known in chemistry |
That was until ozobenzene (C6H6O9): Ann. 170 [1873], 123: "The explosion of only several decigrams of this substance cause such an air vibration, so
that the windows of the room are infallibly shattered. It is therefore dangerous to handle, and one may for such experiments use not more than 3 to 5
milligrams."
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The WiZard is In
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Putting aside that "power of explosives" had a definite meaning,
no sense in letting it stop up from having fun...
Attachment: Explosive Azoimide.txt (2kB)
This file has been downloaded 1150 times
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The WiZard is In
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most powerful explosive
SAYS NAZIS USE ATOMITE
Californian Asserts Explosive Was Invented by Coast Men
The New York Times. October 25, 1939
SAN DIEGO, Calif., Oct. 24 (UP) —Milton T. Vanderslice, California Park Commissioner, said today "there was virtually positive proof" that
Germany is accomplishing tremendous destruction in her aerial bombings with an explosive invented In the United States.
The explosive is atomite, a third again more potent than TNT, was invented by "two men In Berkeley named Hauck and cCloud" five years ago and
offered to the United States Army at the time, he asserted. He was fiscal agent for the inventors at that time, he said, and the formula was patented
in several countries, including Germany.
"There is virtually positive proof that Germany used this explosive in the destruction of Warsaw and Polish military airdromes and depots," Mr.
Vanderslice declared, "for we know there is no bomb now in use by European armies that literally can slice through and crumble huge concrete and steel
buildings, except the atomite projectiles which the Nazis have been using for two years.
He said the explosive was used with "telling effect" in Spain.
-------
Anyone want to buy a bridge?
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JohnWW
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"Atomite"
"Atomite"? I looked that name upon Google, and found that it refers to one of two substances:
(a) Finely divided CaCO3, or chalk powder, noted for its opacity and whiteness, see e.g. http://www.chemindustry.com/chemicals/0300405.html and http://www.imerys-perfmins.com/usa/ProductDetail.asp?PID=304 ; and
(b) the glassy light-green substance, also called Trinitite, that was formed on the desert floor, from sand consisting mostly of silica and feldspar
(microcline and plagioclase) derived from granite, at Alamogordo, N.M.,, which was the site of the "Trinity" test site where the first plutonium-based
atomic bomb was tested on 16th July 1945; see http://en.wikipedia.org/wiki/Trinitite . The stuff, now a collectors' item, is still radioactive, but not dangerously so, due to long-lived
radio-isotopes formed by the fission of plutonium. The light green color is probably due to ferrous iron, from hornblende and magnetite in the
granite-derived sand.
Neither of these "atomites" have ANY explosive properties. None of the Google results refer to any explosive of that name, which may have been an
explosive used in aerial bombs and artillery shells made in Germany, and used in the late 1930s by the Fa$cists in the Spanish Civil War (probably
including the bombing of Guernica in 1937) and by the Nazis in the opening actions of World War 2. (I wonder if the same stuff might also have been
used by the Japanese when they went to war against China in 1937, and later from 1941 at Pearl Harbor and subsequently).
If there really was an high explosive called "atomite", and it was patented in several countries including the U$A and Germany around 1934, being
offered to the U$ Army (it is not clear whether they bought the stuff), what are the patent numbers?
By the way, if it was so dangerously explosive, I am rather surprised that it was patented at all, and not kept as a "trade secret". Or if it was
patented in 1934, that it was allowed to be patented outside the U$A, including in potential enemy countries like Nazi Germany, and that the U$ patent
was allowed to be publicly disclosed, for national security reasons.
[Edited on 4-4-10 by JohnWW]
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The WiZard is In
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Like i said - "Anyone want to buy a bridge?" Da Brooklyn Bridge.
The German bombing of the Spanish city of (look up its name) was the
first large bombing of a city in history. Granted the Bosch bombed London with
Dirigibles in WW I. So no one had any experience in such matters, therefore,
people let their imaginations run free searching for an explanation of
the damage. I am surprised they didn't start a new religion.
The bourgeoisie of the whole world, which looks complacently
upon the wholesale massacre after the battle, is convulsed
by horror at the desecration of brick and mortar.
Karl Marx
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Formatik
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There is Popular Mechanics articles from around 1928 calling it radium atomite. The Royal Engineers Journal from 1929 says it has a claimed VOD of
3270m/s, which isn't much. The material probably develops a very high reaction enthalpy, like mixes of aluminium dust with HEs.
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franklyn
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Due to characteristic sensitivity , alkyl perchlorates are only of academic interest.
Organic Perchlorate salts are another matter.
Ethylenediamine diperchlorate discussed here is a better use of perchloric acid.
http://www.sciencemadness.org/talk/viewthread.php?tid=13174#...
Guanidine Perchlorate is about equal with picric acid.
It's sensitivity is halway between it and PETN.
.
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The WiZard is In
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Radium containing green powder "Atomite" pops-up in
Popular Science August and September 1928 and
Popular Mechanics September 1928.
You can read them at Google.com/books.
---------
"It is essential that persons having explosive
substances under their charge should never
lose sight of the conviction that, preventive
measures should always be prescribed
on the hypothesis of an explosion."
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chief
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The name of the bombed spanish city must have besn "Guernica" ...; Picasso painted it, Hitler saw it and asked Picasso: "Have you done this ?" and
Picasso answered: "No, you" ... ; famous and known occasion ...
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chief
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Should it help anyone: A search for ethyl and chlorate in the chemical name yielded the following:
+---------------------------------------------------------------------------+-------------------------------------------------------------------------
-+
| chem_name | authors_text
|
+---------------------------------------------------------------------------+-------------------------------------------------------------------------
-+
| Tetramethylammonium chlorate(VII) | Palacios, E.; Burriel, R.; Ferloni, P.
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| Tetramethylammonium chlorate(VII) | Palacios, E.; Burriel, R.; Ferloni, P.
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| Tetramethylammonium chlorate(VII) | Palacios, E.; Burriel, R.; Ferloni, P.
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| Tetramethylammonium chlorate(VII) | Palacios, E.; Burriel, R.; Ferloni, P.
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| N,N-(dimethylthiourea)gold(I) perchlorate | Staples, R.J.;Fackler, J.P.Jr.;Costamagna, J.A.
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| Hexakis(N,N-dimethylformamide)aluminium perchlorate | Suzuki, H.;Ishiguro, S.I.
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| Hexakis(N,N-dimethylformamide)-nickel diperchlorate | McKee, V.;Metcalfe, T.;Wikaira, J.
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| Bis(N,N-dimethylthiourea)silver perchlorate | Pakawatchai, C.;Sivakumar, K.;Fun, H.-K.
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| Tris(N,N-dimethylthiourea)silver perchlorate | Pakawatchai, C.;Sivakumar, K.;Fun, H.-K.
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| Tetrakis(dimethylsulphoxide-O)copper bis(perchlorate) | Blake, A.J.;Grimditch, R.S.;Parsons, S.;Schroeder, M.
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| cis-Dimethyl-bis(trimethylphosphine)gold(III) perchlorate dichloromethane | Schuster, O.;Schmidbaur, H.
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| Hexakis(hexamethylphosphortriamido)neodymium tris(chlorate(VII)) | Galdecka, E.;Galdecki, Z.;Huskowska, E.;Amirkhanov, V.;Legendziewicz, J.
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+---------------------------------------------------------------------------+-------------------------------------------------------------------------
-+
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chief
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Besides: Ever haered about "oxonium chlorate" ?
+---------------------------------------------+-----------------------------------------------------+
| chem_name | authors_text |
+---------------------------------------------+-----------------------------------------------------+
| Oxonium chlorate(VII) | Truter, M.R. |
| Oxonium chlorate(VII) | Lee, F.S.;Carpenter, G.B. |
| Oxonium chlorate(VII) | Nordman, C.E. |
| Oxonium Nitro Diperchlorate | Herzog-Cance, M.H.;Belin, C.;Herzog, J.F. |
| Oxonium chlorate(VII) | Rahman, A.A.;Usman, A.;Chantrapromma, S.;Fun, H.-K. |
| Oxonium chlorate(VII) | Rahman, A.A.;Usman, A.;Chantrapromma, S.;Fun, H.-K. |
| Oxonium pentaaquacopper tris(chlorate(VII)) | Bramsen, F.; Bond, A.D.; McKenzie, C.J. |
+---------------------------------------------+-----------------------------------------------------+
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chief
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Here again with references ...; probably everyone know, what the abbreviations mean ...
+--------+---------+--------+--------+------+------------+-----------+-------+------------------------------------------------------------------------
---+
| IDNUM | REF_SEQ | CODEN | VOLUME | YEAR | PAGE_FIRST | PAGE_LAST | ISSUE | chem_name
|
+--------+---------+--------+--------+------+------------+-----------+-------+------------------------------------------------------------------------
---+
| 74075 | 1 | ASBSDK | 59 | 2003 | 625 | 633 | NULL | Tetramethylammonium chlorate(VII)
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| 74076 | 1 | ASBSDK | 59 | 2003 | 625 | 633 | NULL | Tetramethylammonium chlorate(VII)
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| 74077 | 1 | ASBSDK | 59 | 2003 | 625 | 633 | NULL | Tetramethylammonium chlorate(VII)
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| 74078 | 1 | ASBSDK | 59 | 2003 | 625 | 633 | NULL | Tetramethylammonium chlorate(VII)
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| 201258 | 1 | ACSCEE | 53 | 1997 | 1555 | 1558 | NULL | N,N-(dimethylthiourea)gold(I) perchlorate
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| 201274 | 1 | ACSCEE | 54 | 1998 | 586 | 588 | NULL | Hexakis(N,N-dimethylformamide)aluminium perchlorate
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| 201347 | 1 | ACSCEE | 52 | 1996 | 1139 | 1141 | NULL | Hexakis(N,N-dimethylformamide)-nickel diperchlorate
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| 201377 | 1 | ACSCEE | 52 | 1996 | 1954 | 1957 | NULL | Bis(N,N-dimethylthiourea)silver perchlorate
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| 201378 | 1 | ACSCEE | 52 | 1996 | 1954 | 1957 | NULL | Tris(N,N-dimethylthiourea)silver perchlorate
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| 201381 | 1 | ACSCEE | 52 | 1996 | 514 | 516 | NULL | Tetrakis(dimethylsulphoxide-O)copper bis(perchlorate)
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| 204224 | 1 | ZNBSEN | 61 | 2006 | 1 | 5 | 1 | cis-Dimethyl-bis(trimethylphosphine)gold(III) perchlorate
dichloromethane |
| 801659 | 1 | JALCEU | 257 | 1997 | 182 | 190 | NULL | Hexakis(hexamethylphosphortriamido)neodymium tris(chlorate(VII))
|
+--------+---------+--------+--------+------+------------+-----------+-------+------------------------------------------------------------------------
---+
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Formatik
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Try not to quadruple post. All of those compounds are not organic esters, they're mainly salts of organic bases and complexes.
Roscoe speaking of EtClO4 from the Ann. ref: "about 0.2 grams of the ether, which is in a very thin test tube, exploded with such violence, so that a
hole of 15 millimeters in diameter and 5 millimeters depth on a filter stand of wood resulted, and all glass vessels in the neighboring area were
broken. One must therefore when working with this compound be extremely careful; gloves, glass sheets are necessary."
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chief
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Yes; but maybe the literature-references lead somewhere ...
==> If I were on the subject I would walk uo to the library and check each of these references, for some hint always might be there ...
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chief
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Just quoting myself from the other thread ( https://www.sciencemadness.org/whisper/viewthread.php?tid=13... ):
==> Maybe this is possible for the esters of chloric acid too ??
====================
In The Urbanski, on page 19, there is mentioned "electrolytic nitration", Atanasiu and Berthelot, 1937/1937 ..
It's done from diluted HNO3, which is concentrated in the anode-space, where the nitration takes place ...
Storng oxydizing processes go on at the same time in this anodic space ...
====================
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Formatik
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No simple chlorate esters have ever been characterized or isolated. There are theoretical studies (e.g. on methyl chlorate).
Stettbacher estimated glycerin trichlorate would develop 3000cal/g compared to 1580cal/g (heat of combustion) for the
trinitrate ester. The material also isn't known.
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The WiZard is In
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Joseph Schumacher
Perchlorates: Their Properties, Manufacture and Uses.
1960
P. 214
Of ethyl perchlorate, prepared as long ago as 1841 by Hare and
Boyle, its synthesizers said, "in explosive violence it is not
suspassed by any substance know to chemistry." Although
this claim is somewhat out of date, [60].....
[60] Lothrop, W.C. and Handrick, G. R. Chem. Rev., 44, 419, 415-45 (1949)
One would be curious to know that L and H found to be more
explosively violent.
By da a Lead Block test value is a much better measure of
an explosives power than it detonation velocity.
Melvin Cook
The Science of High Explosives
1958
P. 271
L & H employed Trauzl-block data from a number of sources
(without regard to quality) for a large number of explosives
in their intersting correlation of power and brisance with
oxygen balance.
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Formatik
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We can at least say EtClO4 is still among the most violent. It takes a very brisant material to just blow a hole through a metal spoon at those
amounts. If they are less brisant, then nitrate esters should not do the same.
Modern testing of performance like the lead block test has been mostly abandoned from the looks of it, and researchers nowadays just crank out
computations to see if an energetic is worthwhile.
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a_bab
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It would be interesting to do some tests, but I know for sure NG can't do that, and I highly doubt RDX can do it in the given amounts (putting a hole
in a spoon, that is). It would be easy to imagine a test to avoid low order ddn for NG (heating the spoon till it goes off won't give you all the NG's
juice). A small amount of a good primary on the top of the test 'micro' charge, touched with a glowing ember... I dunno.
When I first saw the pic I couldn't believe it. EtClO4 is something surely gives you a punch!
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Anders Hoveland
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I once prepared nitromethylene perchlorate, by using AgClO4 dissolved in toluene and adding iodine and CH3NO2. The AgClO4 could not be dried so I had
to resort to anyhydrous Ag-Acetate and pure HClO4 dissolved in excess acetic acid. I am not sure how the reaction takes place, but I believe there
might be an intermediate IOClO3 forming, or possibly the action of I(ClO4)3 attacks the CH3NO2. Unable to isolate the nitromethylene perchlorate
though. As the toluene was allowed to evaporate, there was inevitably explosions. It made an interesting chemical time bomb though.
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Anders Hoveland
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Just made propyl perchlorate! Bromine vapor was allowed to react in propane gas in the presence of sunlight for two periods of six hours on
consecutive days. A glass gallon jug was used. A tiny ammount of bromopropane was left at the bottom. Most of the bromine had reacted, as evidenced by
the liquid collected being flammable. The bromopropane was extremely volatile. It appeared to be entirely a gas when heated by sunlight. An icebath
was used to make it more workable. Bromopropane is expected to be extremely toxic, and highly irritating. Swim goggles and a makeshift respiratory
filter were used. All handling was done inside a giant clear plastic bag, with gloves ducktaped into holes in the bag for handling. The bromopropane
reacted with anhydrous AgClO4 in toluene, making propyl perchlorate in toluene solution. The toluene was allowed to evaporate off in the shade. A
clear, somewhat opaque white liquid was left behind. This exploded violently when ignited. Obviously, not all the toluene had evaporated since the
explosion was not as powerful as the ethyl perchlorate described in this topic.
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