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Author: Subject: Bad days in the lab or with glassware?
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[*] posted on 11-7-2010 at 06:34
Alloy of potassium


The Boston journal of philosophy and the arts, Volume 2. 1825.

Explosion of an Alloy of Potassium in the Laboratory at Cambridge.

—Having been lately
engaged in repeating some of the experiments of M. Serullas on the alloys of
potassium, in the laboratory of Harvard College, and having obtained some of them
as described at page 61 of this volume, which afforded all the phenomena noticed by
M. Serullas; I was desirous of examining the new compound soon after removal from
the furnace. Six hundred grains of tartar emetic, and 18 of lampblack were employed.
The crucibles well luted together were exposed to a strong red heat in a common
universal furnace during four hours. At the expiration of that time they were
removed, and allowed to cool one hour. I then separated the crucibles; the stratum
of lampblack with which the alloy was covered to the depth of about an inch was
perfectly black, cool, and apparently unaltered,—it did not take fire on exposure to
the air. Having poured out the lampblack, the alloy of antimony and potassium with
charcoal was seen adhering to the bottom and sides of the crucible. On inverting the
crucible it did not fall out, and a small pair of forceps were introduced to detach it.
Immediately on piercing the thin crust which had formed upon the upper part of the
mass, it exploded, with the evolution of much light, and the whole was projected
from the crucible. From the position in which my hand was, the greater part of the
inflamed mass was arrested by it, but much of it was thrown upon the forehead and
eyes. The instantaneous and involuntary closing of the eyelids prevented the burning
particles entering the eyes ; a few however were forced beneath the lid of the right
eye, which produced much pain and irritation. The hair and eyebrows were scorched,
and the fingers of the right hand, which held the forceps, were much burned. Had the
hand not been in the position in which it was, one or both eyes would undoubtedly
have been very seriously injured.

Great caution, therefore, should be used in preparing these alloys, and the crucibles
should not be opened till time has been allowed for a crust to form upon the mass. I
have removed it, after cooling six hours, with impunity. Care should be taken that
any instrument used to detach the mass is perfectly free from moisture, and also the
bottle in which the alloy is to be put.—J. W. W.

Page 61.
ART. IX.—On different Alloys of Potassium, and on the Inflammation of Gunpowder
under Water. By M. Serullas. From the Annales de Chimie et de Physique.]
GUNPOWDER may be fired under water by means of an exploding mixture of charcoal
with an alloy of antimony and potassium, which takes fire on the first contact with
water, and will instantly communicate it to the powder. This mixture is thus
prepared: mix by careful rubbing 100 grammes of tartar-emetic with 3 grammes of
lamp-black or common charcoal. Select crucibles holding 75 to 80 grammes, which
must not be more than three quarters filled, make the upper edge smooth, and rub
the whole inside with charcoal powder, that the charred mixture, when prepared,
may not adhere to its sides. Put some of the materials into the crucible, cover it with
charcoal powder, lute on the cover, and close every opening. Heat it for three hours
in a good reverberatory furnace, then set it by for six hours to cool. This time is
required to allow the air, which always penetrates more or less into the crucible, to
burn the exterior layer of the fulmi nating mass, for it is withdrawn too soon, if it
always takes fire spontaneously. Then without loss of time enclose the calcined mass,
without breaking it up, in a wide-mouthed vessel, where it gradually splits into
fragments of different size, and in this state will preserve its properties for years.
When the calcination has been well performed, the product is extremely fulminating,
so as to detonate with a report like fire-arms, by the first contact of water, and
without requiring any compression. Instead of tartar-emetic and lamp-black, the
following mixture may be used: carbonize cream of tartar by roasting it in an open
crucible till it has lost about half its weight; take 75 parts of this charred tartar, 100
parts of regulus of antimony, and 12 of lamp-black, and mix the whole by constant
rubbing. Then calcine it in the crucible in the way above described.
With this fulminating substance it is easy to fire gunpowder under water. The
experiment was made in the following manner : half an ounce of gunpowder was put
into a strong glass tube closed at one end, of which the powder filled about one
quarter. A piece of the fulminating alloy of the size of a pea, was laid upon the
powder. The tube was immediately closed with a cork, which had been previously
perforated with a small hole, stopped for the present with a little fat lute, soft
enough to be readily pierced with a sharp pin when required. The tube thus
prepared, was then sunk in a large vessel of water two or three .feet deep, and was
confined by weights to the bottom. Then the lute stopping the perforation of the
cork was pierced with a steel wire fixed to the end of a long stick, and the moment
that the water entered the tube the powder exploded, breaking the tube, and
throwing out a four pound weight which had fixed it down.

The author then proceeds to describe several triple alloys of potassium and sodium
with antimony and other metals…….




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[*] posted on 11-7-2010 at 09:28


Wizard, are you even reading what others are saying? Although I find your articles interesting, I think they disrupt the flow of conversation in this thread. Another thread just for your articles may be better suited.
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[*] posted on 12-7-2010 at 07:17
Argento-Chloride of Ammonia


The Annals of chemistry and practical pharmacy
VOLUME 1 1843

ART. VI.—Argento-Chloride of Ammonia, or Ammonio-Chloride of Silver.

DISSOLVE silver in nitric acid, using an excess of acid, precipitate with common salt, and
wash the precipitate with warm distilled water. Expose the still moist precipitate to
an atmosphere of ammoniacal gas, as by setting a small cup of solution of ammonia
in an evaporating bason containing the precipitated chloride, and covering both
vessels with a plate or sheet of paper. After it has been thus exposed for a few hours,
digest the precitate in a Florence flask closed with bladder perforated by a pinhole,
with liquor ammonias fortissim. sp. gr. .880, assisting the solution by the very
gradually applied heat of a water bath. When the water in the bath has been brought
to the boiling point, remove the flask, and set aside to cool; crystals will form, and at
the same time, provided the chloride had been in (be slightest degree discoloured by
exposure to light, a brown pulverulent precipitate, of which take care: it is a
fulminating compound of the most dangerous description. This precaution is the more
necessary, since on one occasion, when endeavouring to investigate the cause of this
decomposition, an explosion took place which instantly converted the laboratory
furnace beside which it had been placed, into a heap of rubbish. The crystals are
removed from the liquor, washed in very cold weak solution of ammonia, and dried
by folds of blotting paper.

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[*] posted on 15-7-2010 at 06:28
Pyrophosphorus



The New monthly magazine. 1826

Explosion of Pyrophophorus.—Dr. Hare prepares pyrophorus in the following
manner : Take lamp-black three, calcined alum four, and pearl-ashes eight parts, mix
them thoroughly, and beat them well in an iron tube to a bright cherry-red for one
hour. This pyrophorus rarely fails. When well prepared, and poured out upon a glass
plate, and especially when breathed upon, it kindles with a series of small explosions,
a little like those produced by throwing potassium upon water. There is even danger
to the face and eyes, from the number and rapidity of these explosions.
A preparation of this substance having been made, was left eight or ten days, well
corked in the iron tubes, and being then opened for transference to another vessel, a
common ramrod was introduced to loosen the pyrophorus, the motion of which
produced considerable friction; when an explosion took place as loud as a common
musket, by which the contents of the tube were blown out, in a jet of fire two or
three feet long, scorching the hair and eyebrows of the person conducting the
operation, and a violent jerk was given to the hand that held the ramrod ; u glove,
with which the band was fortunately covered, was burnt in several places to a crisp.
On putting the ramrod into a second tube, containing pyrophorus, and very
cautiously and gently touching the substance with it, a second explosion took place
violent as the first; it was not thought prudent to repeat the experiment with the
third and larger portion. This pyrophorus had been observed to be unusually good,
and, when breathed upon in the air, kindled in many places at once with a slight
explosion. The tubes, well stopped, had stood within eight or ten feet of the
laboratory fire, and could not have imbibed moisture.—Silliman's Journal, x. 366.



Mechanics' magazine
1827

EXPLOSION OF PYROPHORUS.

A PREPARATION of this substance, having been made by
Professor Sillltman, was left eight or ten days well corked, in iron
tubes, (the same in which it was prepared) and being opened, for
transferring to another vessel, a common ramrod was introduced,
to loosen the pyrophorus, the motion of which produced
considerable friction, when an explosion took place, loud as a
common musket, by which the contents of the tube were blown
out in a jet of fire, two-or three feet long, scorching the hair and
eye-brows of the person conducting the operation, and a violent
jerk was given to the hand that held the ramrod. The glove with
which his hand was fortunately covered, was burnt in several
places to a crisp. His eyes and whole face were affected in the
same manner as if gunpowder had been discharged against them:
and this sensation continued several days; passing off, however,
without serious inconvenience. On putting the ramrod into a
second tube, containing pyrophorus, and very cautiously and
gently touching the substance with the end of the rod, another
explosion took place, equally violent as the first. It was not
thought prudent to repeat the experiments again, as the third
tube contained a much larger quantity of the preparation. This
pyrophorus had been observed to be uuusually good, and when
breathed upon in the air, kindled in many places at the same
time, with a slight explosion. The tubes, stopped with particular
care, had stood within eight or ten feet of the fire, in the
laboratory, and could not possibly have imbibed moisture. The
explosions doubtlessly resulted from (be friction and pressure of
the ramrod ; and they show ns the necessity of care, in regard to
a substance, against which the books, we believe, give us no
caution.

It may be proper to mention, that the pyrophorus was, in this
case, prepared from a recipe furnished by Dr. Hare; it was as
follows:—Take lamp-black three, calcined alum four, and
pearl-ashes eight parts; mix them thoroughly, and heat them well
in an iron tube, to a bright cherry red, for one hour.

This pyrophorus rarely fails. When well prepared, and poured out
upon a glass plate,, and especially when breathed upon, it kindles
with a series of small explosions, a little like those produced by
throwing potassium upon water. There is even some danger to the
eyes and face, from the number and rapid succession of these
little explosions; and one is forcibly impressed with the idea, that
they must be owing to potassium. Since the discovery of this
brilliant substance, there has been little doubt, that it is developed
in greater or smaller quantities, during the formation of
pyrophorus. The above process seems peculiarly adapted to the
production of an unusual quantity of potassium, since there is in
the mixture a larger quantity of the alkali, and also of carbon,
which, it is now known, is admirably adapted to the decomposition
of potass.

If a burning coal happen to drop into a silver crucible, containing
ignited caustic potass, there is a rapid succession of explosions,
and the liberated potassium and potassurated hydrogen burn with
a brilliant flame, and the fumes of regenerated caustic alkali are
extremely conspicuous. Indeed it has long been known, that
charcoal will, by intense ignition, evolve potassium from potash.
Curadeau first called our attention, to this fact, and more recently,
Professor Brunner has shown, that this process, skilfully
conducted, is even preferable to any other.



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[*] posted on 17-7-2010 at 06:37
Guess what just toppled off the bench ....!




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[*] posted on 19-7-2010 at 09:38
Guess what just toppled off the bench?


I posted this in da wrong place ... 2X. And have moved it
here were it be belonging.

Actually I cannot move my posts only delete them and repost.



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[*] posted on 22-7-2010 at 18:50


Quote: Originally posted by Sedit  

I have in my hands now my books, Not just any books but PART of my library which I amassed thruout the years and thought had been lost in a move over 4 or 5 years ago. I have spent countless hours searching and searching for these boxes of books something like 5 boxes atlest, some of which being full of my notebooks which where so dear to me at the time to think they where lost was heart breaking. I have found one of the boxes meaning that the rest are around as well more then likely in the same area.



OH QUITE!!
The last time we moved from the mansion in (insert name of expensive suburb here) the imbecilic layworkers set about confusing all my personal effects, such that it was i, who had to go through several hundred boxes individually, directly their unpacking to the wings of the manor as appropiate.
Apart from this tedious labour it also required i spend several hours in the company of those uncouths who originally were the cause of the problem.
Really.

How much shit do you have that you can misplace several boxes but they remain in your possession.

My dear departed mother used to say to me when i had lost a toy or something and wanted her to find it for me.
'the house doesn't lose anything'
That really shits you when you're 7, partly i as i didn't really understand what she meant.

And finally in the Wizards defense i thought this thread was bad days in the lab with chemicals or glassware. I think his post's are bang on topic. Besides the fact that i often learn something the not hard way simply by reading these accounts.
I would rate his contributions as very valuable, besides the fact the fact they are interesting. Importantly i find i limit myself to reading only a few at a time so i can hold the information better.
Consider it important OH&S training for the home chemist. Training that you should consider that you'll never get to the end of, lest you become one that is written about.

Dead Chemists
Lest we Forget.

[Edited on 23-7-2010 by Panache]




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[*] posted on 22-7-2010 at 19:16


Its not so much that I had alot of stuff to misplace but it was more along the lines of my boxes are mixed in with 3 other peoples possessions whe placed in a large storage area and the ones in question where misplaced to the point where they should have in no way shape or form been where they where. I spent all my time going over and over my stuff looking for what should have been there finilly comming to the conclusion that they where left behind till I started to move some stuff because im building a real lab for a change and low and behold right next to where I had many solid chemicals stored I opened on of the boxes and there they where like a chest of gold in my eyes. I have still yet to find the rest but im excited I found my CRC handbook and some of the others I have.


As far as the value of wizards post in this thread.... well lets just agree to disagree. The forum is cluttered with his post of others mishaps and even though some are interesting its nothing I couldnt have found myself if I truly had the desire to google the same information. But Iv said my peace about that subject elseware so no need to continue on as it would not really change a thing.





Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
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[*] posted on 23-7-2010 at 00:20


I still have boxes from 5 or so years ago that I haven't inspected for years. I'd probably find some stuff I'd given up on.



“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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[*] posted on 23-7-2010 at 17:54


Quote: Originally posted by Sedit  

As far as the value of wizards post in this thread.... well lets just agree to disagree. The forum is cluttered with his post of others mishaps and even though some are interesting its nothing I couldnt have found myself if I truly had the desire to google the same information. But Iv said my peace about that subject elseware so no need to continue on as it would not really change a thing.


No man........I'm agreeing to disagree...fuck you...lol.

You're correct of course except that i don't have the desire to google stuff like this, its gets too broad too quickly, but i appreciate it being served to me, call it professional best intentions laid waste to the lazyiness monster.
There is a of course a degree of life insurance ad to the info as well, you know the ones where the mid thirties women and her three young children talk about the father who died and how they would be homeless without the life insurance. It's always interesting how even though they have the statistics the company never mentions the actual chance of this circumstance occurring. If you want to make someone make an irrational decision, engage their emotional brain. Thats why often young KEWL's are so at risk doing amatuer chemistry, they are acting not rationally but emotionally, 'sic man wicked woot!' this sort of data engages them emotionally but in a cautious way, which is good.
Of course this is all speculation.




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[*] posted on 27-7-2010 at 14:05


You're about to witness what is without doubt the most disturbing glassware accident I've ever seen in my life;

By clicking this 18+ only link, you've been warned, twice




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[*] posted on 27-7-2010 at 15:54


Well, I guess I live a very tame life these days. A bad day in the lab for me lately is when somebody steals my pen. So I wrote a poem:

To all the women and men,
Who like to steal my pen,
It's very uncool,
And makes you a tool,
So please don't do it again!

All things considered, though, working with large quantities of HF and HClO4, things could be a lot worse for me. If you're ever handling acid bottles, be careful picking them up: I've heard stories of the bottoms falling out on glass acid bottles and a gallon of concentrated nitric or perchloric falling over some hapless lab worker.




"In the end the proud scientist or philosopher who cannot be bothered to make his thought accessible has no choice but to retire to the heights in which dwell the Great Misunderstood and the Great Ignored, there to rail in Olympic superiority at the folly of mankind." - Reginald Kapp.
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[*] posted on 27-7-2010 at 17:54


I'm very glad my browser told me the name of the file before doing anything, peach :P



“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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[*] posted on 27-7-2010 at 19:57


Quote: Originally posted by DDTea  
Well, I guess I live a very tame life these days. A bad day in the lab for me lately is when somebody steals my pen. So I wrote a poem:

To all the women and men,
Who like to steal my pen,
It's very uncool,
And makes you a tool,
So please don't do it again!

All things considered, though, working with large quantities of HF and HClO4, things could be a lot worse for me. If you're ever handling acid bottles, be careful picking them up: I've heard stories of the bottoms falling out on glass acid bottles and a gallon of concentrated nitric or perchloric falling over some hapless lab worker.


At work, on the top shelf in the solvent room, this large plastic drum of phosphorous oxychloride is sitting there, and I'm always in fear of it rupturing while I'm getting solvent.
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[*] posted on 27-7-2010 at 20:55


Quote: Originally posted by peach  
You're about to witness what is without doubt the most disturbing glassware accident I've ever seen in my life;

By clicking this 18+ only link, you've been warned, twice



OMG WTF, not enough letters in the alphabet to state that this is the sickest fucking thing I have ever seen in my life. There are few things that leave my jaw on the floor and sadly this is one of them.

Mainly because I watched it long enough to get to the really bad part..........





Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
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[*] posted on 28-7-2010 at 00:52


Quote: Originally posted by DDTea  

To all the women and men,
Who like to steal my pen,
It's very uncool,
And makes you a tool,
So please don't do it again!


That's excellent!

I have a lot of those moments when I turn around and an item I had in my hand three seconds ago disappears four three hours. If ghosts exists, that's what I'm going to do. In between perving at ( o )( o ) in shower rooms.

We used to have a toilet that was new but that had some major issues with flushing anything round the bend. It couldn't even hand two or three handfuls of TP, so I wrote a similar poem and stuck it to the back of the door...

Sending a sausage to the seaside, by Peach;

First the push, then a flush
Then go round to swipe a wipe
Before putting the rest down the pipe


It was censored shortly after.

On visiting the US, I did very much enjoy the no holds barred approach to toilet flush capacity in particular. I like a toilet that can deal with significant problems. And the American's reliance upon a similar desire and expectation was demonstrated when my US friend visited the UK and immediately blocked the hotel toilet to a 'beyond easily repairable' state.

Quote: Originally posted by Sedit  

Mainly because I watched it long enough to get to the really bad part..........


Is that the silence, other than the noise of crunching glass and dripping blood?

I've seen people having their faces blown off and other horrendous things, but there's a quality to that which seems to surpass even those.

Encylopedia Dramatica have on article on him. In fact, they worked out who he is and have been chatting to him, he's even a member on there, has gone out of his way to prove it's him (using other bits of glassware with notes attached) and posted other, equally odd videos.

As the article points out, his video demonstrates the inherent dangers of using low quality glassware for high end (or is that low end) experimentation.

Alex the, quite probably mentally ill, intertitz hero

[Edited on 28-7-2010 by peach]




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[*] posted on 28-7-2010 at 17:27


Quote: Originally posted by peach  
You're about to witness what is without doubt the most disturbing glassware accident I've ever seen in my life;

By clicking this 18+ only link, you've been warned, twice



People who enjoyed this would be interested in :—

Emilio de los Rios Magriñá
Atlas of Therapeutic Proctology
WB Saunders 1984
Translation of Atlas de Coloprotologia 1976

You would be amazed what can go wrong with such a
simple device.
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[*] posted on 28-7-2010 at 18:20


There is some truth to the motto of it being a one way traffic road.

Things tend to go wrong with it a lot more often the more people try driving the wrong way up it.

I once heard a story about some boys who thought it'd be kinky to drive cement the wrong way along the road, although cement trucks are banned on that road anyway. They didn't realise cement is fairly caustic, or that the many bends of that road would make it next to impossible to get the truck back down the other way once the load had gone off.




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[*] posted on 16-10-2010 at 13:59


I just saw those columns on the page back, that guy's serious hey?!

I've broken a 600mm vigreux before and was upset. Difficult to imagine how much more upset I'd be if it was that one in front of him.

Wizard, where on Earth does this vast encyclopedia of references to obscure books come from? I'm picturing your house right now, and every wall is lined with books. Do you actually remember those off the top of your head? Anuses.... anus... anus, anus...... hmmmmmm.... these references. :D

[Edited on 16-10-2010 by peach]




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[*] posted on 16-10-2010 at 15:12


Quote: Originally posted by peach  
Wizard, where on Earth does this vast encyclopedia of references to obscure books come from? I'm picturing your house right now, and every wall is lined with books. Do you actually remember those off the top of your head? Anuses.... anus... anus, anus...... hmmmmmm.... these references. :D



Well as an infamous chemist said to me years ago —
I picture you siting up there in NY sitting on a pile of books.

Walls lined w/ books. I am a master of (as used by Woody Allen)
the polymorphous perverse.

And while upon the subject I am reminded that I shelve —

Armandor R. Favazza, M.D.
Bodies Under Siege : Self-mutilation in Culture and Psychiatry
Johns Hopkins U Press
1987

For the really odd I also shelve...

Sex errors of the body: dilemmas, education, counseling
John Money
Johns Hopkins Press, 1968

Some are 'between.

Speaking of poetry, this from Hudson Maxims 1916 Dynamite Stories

LINES TO A LADY
SOME years ago, when I was conducting experiments with detonators for my safety
delay-action fuze, which was adopted by the United States Navy in 1908 as the service
detonating fuze for high-explosive projectiles, I received instructions that a parcel of
fulminate detonators, made at the torpedo station, had been received and were being
held for me at Fort Lafayette, and I was told to go to the Brooklyn Navy Yard, whence I
would be taken in a tug to the Fort for them.

After having procured the package, I concluded that it would be much more expeditious
for me to take a trolley car home than to return by the tug. On entering the car and
seating myself, I placed the package beside me on the seat, keeping my eye constantly
upon it. It was, by the way, perfectly safe to carry if subjected to merely ordinary
handling, but it would not do to jump on it or to kick it about much, for, in that case, there
might be some energetic results.

No sooner had I comfortably seated myself in the car than a huge, determined, militant-
looking woman entered, brushing a few small men aside. Seeing all the seats occupied
except the space where the package was, she turned and hurled herself backward and
downward.

Her movements were so quick that I had barely time to throw my left arm firmly under
her, and, although I am unusually strong, I had all I could do to support her enormous
bulk. When she felt my arm beneath her, protecting the package, she was all the more
indignant and determined to crush the package in order to teach me a lesson, and she
glared upon me fiercely. I finally succeeded, by throwing my shoulder against her, in
toppling her sufficiently to remove the package with my right hand, and then I let her
down upon the seat.

I seldom wax poetical, and never permit myself to write verses to ladies when I am not
sure that they will be gratefully received. But in this case, I side-stepped a little from my
usual course, and, taking my note-book from my pocket, wrote the following lines, which
I folded up nicely, and when I arrived at my street, I handed the paper to Her Militancy"

Dear Madam, I'm an anarchist,
That package was a bomb.
I'm on my way
Someone to slay,
And this is really true-
I didn't want to waste that bomb
On just the likes of you.



djh
----
Former member —
The Society for the Scientific Study of Sex
Society for the Study of Economic Botany
Herpetologist League
&c., &c.

All of God's amateur experimenters are not wired to tightly!

CH Wecht & M Helpern Eds
Legal Medicine Annual 1969
Appleton-Century-Crofts
1969

Exsangiunation.jpg - 357kB

[Edited on 16-10-2010 by The WiZard is In]
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psychokinetic
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[*] posted on 17-10-2010 at 00:09


Now THAT'S a bad day in the anywhere with any-ware.



“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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hissingnoise
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[*] posted on 17-10-2010 at 10:39


Exsanguination? That's a bleedin' BIG word . . .

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chemx01
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[*] posted on 17-10-2010 at 12:19
Bad day


Just today I had very bad day with glassware.
I was making DNPO (bis(2,4 dinitrophenol)oxalate), quite simple, but i just did something plain stupid. I used erlenmayer flask and filled it with solvent (DCM) and add all the reagents and then leave it in a cold ice bath,but i thought that it would be good idea to stopper it, to exclude moist air coming in, then i came back and remove it from the bath and carefully dry it with towel. The flask had a very tiny crack, but since it's not exhotermic and not under pressure i didn't count it as threat, BIG mistake. So i touched the flash near the crack and BOOM the flask exploded cover everything in yellow dinitrophenol, not nice at all, and also quite waste of the reagents, and also the DCM+Dinitrophenol quickly attacks paint so it can't be removed.I just thought that in temperature about 5°C the DCM can't pressurize the flask, never underestimate it, i learned it hard way.
But that would be my first serious accident in 4 years, so that's not that bad.
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aonomus
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[*] posted on 17-10-2010 at 13:06


No matter what you think, never seal a glass vessel unless it is designed for it (ie: parr hydrogenator bottles or pressure flasks). If you want to avoid solvent loss, just add a condenser and maybe a septum with a needle in it to reduce the size of the hole where solvent can escape, as well as increase the distance stuff needs to go.

I have my own pressure vessel story, ran reactions under 15psi with a modified ace thread screw stopper. A hole was used to lead out a PE tube to a valve for pressure relief and a pressure gauge. It worked fine about 4-5 times, then one day a leak developed (somewhere) and the reaction mixture foamed and filled the entire tube (about 2ft long) and corroded everything inside the valve tree. Not a fun day to clean that up even though it was approximately 80mL of reaction mixture...
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The WiZard is In
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[*] posted on 18-10-2010 at 06:45


Quote: Originally posted by hissingnoise  
Exsanguination? That's a bleedin' BIG word . . .



The word is definitely not sanguine.
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