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Author: Subject: Ethyl perchlorate anyone?
niertap
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[*] posted on 6-8-2011 at 09:51
Ethyl perchlorate anyone?


I saw the synthesis in the link below. However it did not seem so reputable(2). But, someone else talked a little bit about a synthesis that seems slightly safer(1). Anyone up for it? I can pretty much guarantee it will be exciting.


1. At STP mix together ethyl sulphate, with Barium Perchlorate. It then said they distilled it off at room temp, which seems like a really efficient way to lose your hands and grow another very manly testicle. There was also talk that it is impossible to make it directly from the alcohol. I have a feeling the hydroxyl concentration should be kept as low as possible.




http://pipeline.corante.com/archives/2006/05/30/things_i_won...



2. secret milkshake on May 31, 2006 3:48 AM writes...

I have seen a step-by-step writup for ethyl perchlorate from Ba(ClO4)2 and EtOSO3Na. One could actually distill gram quantities of the material at reduced pressure. It is an oily liquid, unstable to moisture. A small drop of this material heated on a Bunsen burner likes to blow a hole right through a metal spoon.

The maniac who described this prep (including the photos of his garage lab) noted that the material has a fruity smell and a sweet-musty taste. I guess he would not have to worry about Et-perchlorate being alkylating agent, tumors take years to develop so this would not play any role during his lifespan.

On similar note- many years ago I tried to dry a wet acrolein with magnesium perchlorate. Suprise- the stuff disolved and became warm. "Oh, it is polymerising" I thought. So I started distilling the mix. There was bright orange flash in the flask and sound as if shuttle was taking off. The thing did not explode, just burned like a rocket and within seconds produced several buckets of very fine and greasy soot that settled all over the lab.




Ignorance is bliss

Outliers in life are modeled by chemical kinetics
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[*] posted on 6-8-2011 at 10:34


Quote: Originally posted by niertap  
I saw the synthesis in the link below. However it did not seem so reputable(2). But, someone else talked a little bit about a synthesis that seems slightly safer(1). Anyone up for it? I can pretty much guarantee it will be exciting.


How much excitement are you up for?

Ye old Schumacher sez. p 214 —

Of ethyl perchlorate, prepared as long ago as 1841 by Hare
and Boyle [35] its synthesizers said, "in explosive violence
it is not surpassed by any substance know to chemisty."
Although this claim is somewhat out of date, [60] the
perchlorate esters are unquestionable of exceptional explosive
hazard. The methy, ethyl and proply perchlorates are oily
liquids which are very sensitive (more than the corresponding
nitrate esters) to head, shock and friction, and extraordinarily
explosive. [71]


A Treatise on chemistry, Volume 3
By Sir Henry Enfield Roscoe
1881
[Google.com/books]

230 Ethyl Pcrchlorate, C.2H6C104, is the only known ethereal
salt of the oxyacids of chlorine. It was first prepared by Hare
and Boyle4 by distilling a mixture of barium perchlorate and
barium ethyl sulphate, but was afterwards more completely
investigated and analyzed by Roscoe.5 It is a colourless liquid,
which, in the dry state, undergoes sudden spontaneous
decomposition even when poured from one vessel to another,
or when its particles are in any way slightly shaken. The
violence of these explosions is extreme. About two decigrams
of the substance contained in a thin test-tube exploded with
such force as to bore a hole 15 mm. in diameter and 5 mm.
deep in a filter stand of hard wood, and all the glass vessels
standing near were shattered. The greatest care must,
therefore, be taken in operating with this body, and gloves and
glass-screens arc absolutely necessary. In contact with water
the ether is much more stable, and may be shaken or even
distilled without any explosion occurring. Heated under a thin
stratum of water, it boils at 74°.

Journal - Chemical Society, London,
Volume 15
By Chemical Society (Great Britain)
1862

Dry perchloric ether undergoes an explosive decomposition
when poured from one vessel to another, or when its particles
arc m any way slightly shaken. The violence of these explosions
is extreme; about 0-2 grm. of the ether contained in a very
thin test-tube exploded with such force as to bore a hole 15mm.
in diameter and 5mm. deep in a filter-stand of hard wood, and
all the glass vessels near were shattered. The greatest care
must be taken in working with this body; gloves and glass
screens are absolutely necessary.



---------
After the water has drained off, the drop of æther remaining at
the bottom of the filter may be exploded either by approaching
it to an ignited body, or by the blow of a hammer. We are
induced to believe, that in explosive violence it is not surpassed
by any substance known in chemistry. By the explosion of the
smallest drop, an open porcelain plate will be broken into
fragments, and by that of a larger quantity, be reduced to
powder. In consequence of the force with which it projects the
minute fragments of any containing vessel in which it explodes,
it is necessary that the operator should wear gloves, and a
close mask, furnished with thick glass plates at the apertures
for the eyes, and perform his manipulations with the
intervention of a moveable wooden screen *.

* Having suffered severely, on several occasions, from the
unexpected explosion of this substance, we would earnestly
recommend the operator not to neglect the precautions
mentioned above.

Hare and Boyle.

------
You can DL H&B's original paper from Google.com/books

Also check Google.com/books for other refs.

By da H&B say — The perchlorate of æthule obtained in this way
is a transparent, colourless liquid, possessing a peculiar,
though agreeable smell, and a very sweet taste, which, on
subsiding, leaves a biting impression on the tongue resembling
that of the oil of cinnamon.


djh
---
If you kill yourself synthesizing this
chemical terror — can I have you
chemistry set?
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[*] posted on 6-8-2011 at 10:59


Quote: Originally posted by niertap  
I saw the synthesis in the link below. However it did not seem so reputable(2). But, someone else talked a little bit about a synthesis that seems slightly safer(1). Anyone up for it? I can pretty much guarantee it will be exciting..



I be (just) finding this written down in a book.

Meyer and Spormann [250] reported that the methyl
ester [b.p. 52o] and the ethyl ester [b.p. 89o] are
extremely powerful explosives and that they were unable
to avoid explosions in spite of great foresight taken in
handling them.


[250] J. Meyer and W. Sportmann. Z. anorg. u. allgem.
Chem., 228, 341 [1936]


djh
---
"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."

Marcellin Berthelot - 1892
Explosives and their power - Page 47


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