Sciencemadness Discussion Board

Bad days in the lab or with glassware?

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The WiZard is In - 1-7-2010 at 05:10

History of the Royal Society: from its institution to the end of the ...
By Thomas Thomson
1812

Charles William Scheele was born in 1742, in Stralsund, the capital of Swedish
Pomerania, where his father was a tradesman. Young Scheele, at a very early period
of his life, showed a strong inclination to learn pharmacy, and was accordingly bound
an apprentice to Mr, Bauch, an apothecary at Gottenburg, with whom he lived about
eight years. Here he first felt the impulse of that genius which afterwards made him
so conspicuous. He durst not indeed devote himself openly to chemical experiments ;
but he contrived to make himself master of the science by dedicating those hours to
study which were assigned him for sleep. According to the testimony of Mr. Grunberg,
his fellow apprentice, he was of a very reserved and serious disposition, but
uncommonly diligent. He attended very minutely to all the processes, reflected on
them while alone, especially during the night time, and read every thing relating to
the subject in the writings of Neuman, Lemery, Kunkel, and Stahl. Kunke’s Laboratory
was his favourite book. He used secretly, during the night time, to repeat
experiments out of it. On one of these occasions, as he was employed in making
pyrophorus, another apprentice, without his knowledge, put some fulminating
powder into the mixture. The consequence was a violent explosion ; the whole family
was thrown into confusion, and our young chemist was severely chastised.

the Z man - 1-7-2010 at 06:40

Sorry to post about me again.To woelen and the others, I only wanted you to know I'm glad you have understood me and I want to thank you for your concern. I'm really sorry to hear that we lost a member, I hope you're wrong woelen :( . I promise I won't be the next. After a few accidents you start to understand the dos and don'ts. You see, i'm mainly into energetics, that's surely not the best for a newbie. It is especially critical not to do any error. One wrong move and your life could change forever, or you can even loose it. to But it's what I love and you can't choose what you are fascinated by. You can only do all you can not to fall victim of your passion. But when I read stories of those who lost a hand for .3 g MHN cap or for stupid errors or even for bad luck, I start to think "what if I was him? Would I do the same error?". That's what pushes me to always try to improve. As you can see it's a strong motivation.
To Skyjumper: I see your point. I think it's the worst fault for an experimenter to let an error affect the others or even the family. You can be sure that if do something wrong I will be the only affected.I peform every experiment that I know could go wrong alone and making sure first to have a way for not damaging the others in any way. For the lead thermite see my reply on the thermite thread.

JohnWW - 1-7-2010 at 08:49

Scheele was either the chap who discovered the mineral scheelite, one of the the major ores of tungsten, formula CaWO4 with some of the Ca being replaced by other divalent metals such as Cu, Zn; or had the mineral named after him . See http://en.wikipedia.org/wiki/Scheelite . There is a deposit of it near Glenorchy in the South Island of New Zealand.

Humphrey Davy

The WiZard is In - 2-7-2010 at 05:38

Annals Of Mechanical Philosophy, Chemistry, Agriculture, And The Arts.
January, 1813.


Scientific Intelligence and Notices of Subjects Connected with Science.

Compound of Chlorine and Azote.

SOME time ago Sir Humphrey Davy received a letter from Paris
[from Ampere], containing, among other particulars, a paragraph
to the following effect: " I suppose you have heard of the
discovery which has been made in France, of a combination of
chlorine and azote, a discovery, which cost the person [P. Dulong]
who made it, an eye and a finger." Sir Humphrey Davy, before
the receipt of this letter, had made many unsuccessful attempts to
produce such a combination. He immediately ran over all the
recent French journals, to see whether he might not have
overlooked some account of this new compound; but could find no
trace of it whatever. While in this perplexity Mr. Children put him
in mind of a discovery made some time ago in England, by Mr.
Burton, who, by passing a current of chlorine through a solution of
nitrate of ammonia, had obtained a white oily looking substance,
so volatile that he had been unable to collect it. On this hint Sir
Humphrey Davy immediately set to work, and speedily succeeded
in forming the supposed oil. It was volatile; and when heated on
the surface of water burnt rapidly, with a feeble puff or explosion.
Messrs. Davy, Children, and Warburton agreed to repair to the
laboratory of Mr. Children, and examine this new substance with
some care. They succeeded in forming it, by passing a current of
chlorine through solutions of oxalate of ammonia, as well as
nitrate of ammonia. They put solutions of different ammoniaeal
salts into a succession of Woulfe's bottles, and passed a current of
chlorine through them. The substance in question was formed,
and, during the course of the experiment, exploded with
prodigious violence, and broke the bottles to atoms. They had
recourse in consequence to small tubes, and used quantities of the
oil, not exceeding the size of a pinhead. Notwithstanding these
precautions, in one of their trials, the tube, broke, and a fragment
of it entered Sir Humphrey Davy's eye, through the cornea. This
untoward accident prevented him from prosecuting the
experiments any farther. But they were continued by Messrs.
Children and Warbnrton. The following are the principal facts
which they ascertained :

When this substance explodes, a gas is emitted, which when
examined turns out to be azotic gas. Hence it seems fair to infer,
that the oily substance is a compound of chlorine and azote, and
the same substance as that discovered by the French chemist, and
alluded to in the letter received by Sir Humphrey Davy, above
referred to. When a little of this substance is thrown upon the
surface of olive oil or oil of turpentine, a dreadful explosion takes
place. It explodes also when it comes in contact" with phosphorus,
but not with so much violence. During all these explosions
considerable heat is evolved.


M. Rouelle, the celebrated chemist, was extremely absent at his lectures

The WiZard is In - 3-7-2010 at 05:50

Critical Review; Or, Annals of Literature
By Tobias George Smollett
1806

M. Rouelle, the celebrated chemist, was extremely absent at his lectures; he usually
brought with him a brother and a nephew to assist him in his experiments ; but, as
his assistants were not always there, he would cry nephew ! why nephew ! but the
nephew not coming he would go himself to the laboratory, always continuing his
lecture as if he had still been with his auditors, and, at his return, had commonly
finished the demonstration he was then about. One day, in the absence of his
brother and nephew, being left to perform the experiments by himself, he said:
Gentlemen you see this cauldron upon this brazier.—Well, if I were to cease stirring a
single moment, an explosion would ensue, which would blow us all into the am This was
no sooner said than he forgot to stir, and his prediction was accomplished ; the
explosion took place with a horrible crash, all the windows of the laboratory were
smashed to pieces, and two hundred auditors whirled away into the garden.

ET Chapman — Methyl nitrate

The WiZard is In - 4-7-2010 at 12:34

The Year-book of facts in science and art
By John Timbs
1873

E. T. CHAPMAN, the distinguished young chemist, whose name is well known as one of
the authors of the ammonia process of water analysis. He was killed by an explosion
in his laboratory at Riibeland, in the Hartz, on the 25th of June. Four years ago, Mr.
Chapman was the most industrious contributor to the Chemical Society. He will be
especially remembered by chymists for his very beautiful researches on " limited
oxidation," and for his remarkable faculty of performing unpromising chymical
operations with quantitative accuracy. Last autumn he left England to take charge of
a large wood distillery in the Hartz, and a short time ago had commenced the
manufacture of nitrate of methyl on a gigantic scale. Under certain conditions, nitrate
of methyl is terribly explosive, and it is supposed (for no one survives to tell what
took place) that the terrible explosion which shivered a bomb-proof building, killing
Mr. Chapman and two workmen who were with him, was an explosion of nitrate of
methyl. If the substance was nitrate of methyl, the above lamentable accident
furnishes another proof of the treacherous nature of explosives which, like nitro-
glycerine and gun-cotton, contain hydrogen and carbon associated with nitrogen
oxides. Mr. Chapman was only 26 years old at the time of his death. A few years ago,
it would have been deemed a strange thing for England to send out a chemist to take
charge of a German factory; but that the most promising of the young chemists of
England should have found no room for him here, and should have taken service in a
foreign land and perished there, is melancholy in the extreme.—British Medical
Journal.

Teriodide of antimony

The WiZard is In - 5-7-2010 at 05:46

Hand-book of chemistry, Volume 4
By Leopold Gmelin, Henry Watts
1850

ANTIMONY AND IODINE.

A. TERIODIDE OF ANTIMONY.—The two elements unite at ordinary temperatures, the
combination being attended with great rise of temperature and evolution of iodine
vapour, and even with explosion, if large quantities are used.—On one occasion,
when a few ounces of the mixture were put into a retort, the retort burst with a loud
report, even before heat was applied, and the compound was thrown up to the
ceiling of the laboratory. (Brandes, Jf. Br. Arch. 21, 319.)

Sedit - 5-7-2010 at 05:57

Since this is a bad days in the lab thread Ithink my last couple days would count.

I decided to build a new bench and the bench kicked my ass. I broke a drill bit which incidently managed to fined its was into my finger which was oh so plesent. I have more splinters in my hands from the cheep Plywood used then a woodchuck has in his teeth a 2x4 fell over and landed on my making me look like an abused child and to top it all off..... I kicked a giant steel block on accident and broke my foot....

Im just starting to build a real lab so to speak what im already getting my ass kicked by it before its complete.

I have however managed to build myself a very nice bench with a shelf above and plenty of storage under it, but I have yet to run the electric and taps for steam and N2 like I am going to do soon. Im going al also fix up my mini kiln I build a while back and use that for alot of experments so that will be awsome whn I haveit finished.

I got along ways to go, lets hope that the next few days are better then the first. I pretty much have to wait till I can walk right again before I go out woking with any power tools first tough.


[edit]

Oh yeh I almost forgot the final fun fact of the entire experience. Luckly for me the wood was infested with Mites so I woke up the next day chewed alive with, a broken foot, bruised from head to toe, full of splinters and because of the mite infestation I look like someone used my whole body as a fuking dartboard. Now I am going to have to seal the whole bench with epoxy paint before I can ever use it.

I feel like when I finilly complete it and stand back to enjoy the fruits of my labor the entire thing will burst into flames as on big last F-U from god.

[Edited on 5-7-2010 by Sedit]

psychokinetic - 5-7-2010 at 13:29

Quote: Originally posted by Sedit  
making me look like an abused child

[Edited on 5-7-2010 by Sedit]


Get to your room and don't come out until you've made a right chemical mess of it.

Sedit - 5-7-2010 at 22:24

Dude I have never had my ass kicked like this by anything. I build the bench away from the area and it was a breeze taking a matter of minutes maybe an hour tops , all I had to do was mount it on the wall. The wood i was tring to mount it to though was stuburn plywood with some flex and appears to be treated and would reject the screwes or worse appear to take them just to have them fall on my head when I let go. It was like someone was watching me playing god and having a good laugh at my expense.

But When done its going to be awsome I hope. Im going to paint the periodic table on it and coat it in the clear epoxy paint they use in bars. The person I spoke with said it is chemical resistant, crystal clear and very durible. So my bench will be the coolest bench around for years to come.

psychokinetic - 5-7-2010 at 22:43

Quote: Originally posted by Sedit  
Im going to paint the periodic table on it and coat it in the clear epoxy paint they use in bars. /rquote]

Geekcore :D
I'd like too see that once complete.

Sedit - 5-7-2010 at 22:48

You and I as well....

Iv been known for my artwork and I am much better at that then I am chemistry or being a carpenter so I think it will look down right awsome when completed.

nitrate of potash and acetate of soda

The WiZard is In - 6-7-2010 at 05:20

American journal of pharmacy, Volume 45. 1873.
EXPLOSIVE MIXTURE OF NITRATE OF POTASH AND ACETATE OF SODA*
BY M. VlOLETTE.

An accident in the author's laboratory made known to him a singular reaction
between nitrate of potash and acetate of soda, which, under the influence of heat,
constitutes an explosive mixture equal in force to gunpowder. In some researches
upon saltpetre he had heated moderately in a small phial a few grams each of nitrate
of soda and acetate of soda, both previously fused and anhydrous. The two salts
melted formed a colorless and transparent liquid, which gave off a few gaseous
bubbles. At the same moment, a violent explosion occurred,, accompanied by flame
and smoke, which scattered the phial in fragments all over the laboratory ; a fresh
gaseous combination between the elements of the salts had taken place, leaving a
slight residue of alkaline carbonate.

In repeating the experiment a gram of nitrate of potash was melted in a small
platinum capsule at a gentle heat, and a gram of acetate of soda previously fused
added to it. At a temperature of about 300o C the mixture remained fluid,
transparent and without alteration as long as the temperature remained constant ;
upon raising it to about 350° C. there was a slight ebullition followed instantly by a
loud explosion, with light and smoke, similar to that of gunpowder. As before, there
was a slight residue of alkaline carbonates. The same result followed when a
substance in ignition without flame was plunged, into the liquid at 300° C.

If the melted mixture be poured upon a cold surface a white
substance is obtained, which is hard, brittle, rather hygroscopic,
more fusible than nitrate of potash, and being melted explodes
violently In the solid form it does not burn when placed in
contact with an ignited body ; but reduced to fine powder, it
deflagrates violently upon the application of a flame.

The explosive properties of the mixture are only developed when the nitrate of
potash and acetate of soda are present in certain proportions—from 50 to 100 parts
of the acetate to 1OO parts of the nitrate—the most explosible mixture being 100
parts of the fused nitrate to 60 parts of the fused acetate. When the nitrate is in
excess, the combustion is only partial and of short duration : when the acetate is in
excess, the mixture burns slowly and similarly to a light wood.

A mixture of nitrate of soda and acetate of potash was found to have the same
explosive properties, but to be more hygroscopic. Mixtures of nitrate of potash with
the acetates of copper and baryta did not yield an explosive product.—Pharm. Journ.
and Trans. Jan. 11, 1873.

* Journal de Pharmacie et de Chimie, xvi, 333.


Sedit - 6-7-2010 at 15:37

This is our good and bad day in the lab thread Wizard no place for copy and paste jobs here.


I have great news the laws of physics once again prevail and all to often people seem to forget that humans and there emotions must abide by the laws of physics....

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.

The irony of the whole thing is the chemistry books I have been looking for for years where where else but... RIGHT NEXT TO ALL MY CHEMICALS!!!!!! The box was mislables as someone elses junk and I never once thought to look there I even pushed it aside to make room for some of my stuff.

To give a rough idea the one box I found contains relatively little of my chemistry book collection but the titles I did find are

Handbook of Chemistry and Physics- 42nd edition 1960-1961
This is a big little book with so much data on azeotropes and chemical preperation ect that it was hard to work without it when I didn't have the internet.

Antoine Levoisier- Elements of Chemistry
This was one of the first books that got me highly into chemistry and I love it this many was the fter of modern chemistry.

Teachers Edition of Prentice Hall-Chemistry-The study of Matter

A very nice teachers edition chemistry book for im assuming collage students, some of you may even have copy of this yourselfs I dunno but it is indeed a very informative text book I suggest anyone to read.



So remember no matter how bad things seem to be going(Im running a 102f fever have a cold sore, broken toe, and all kinds of aliments) The laws of physics will do what it can to restore balance and give you the good with the bad. This finding in my lab has made the past couple days of living hell more then make up for it by far. Im so excited that I have the potential to find my old notebooks which are still MIA. When I wrote in those books I had far more knowledge then I do now and my brain was running in a way that left even the doctors astounded and even I have a hard time comprehending the stuff in someof my old notes now. When I find them it will be like getting a long lost part of my life back.

sundry misadventures

The WiZard is In - 7-7-2010 at 05:54

American druggist and pharmaceutical record
Volume 47. 1905.
LABORATORY ACCIDENTS

of a similar nature are of course one of the regular risks run by chemists. A Parisian
daily, commenting on this subject, reminds us that when the famous Berthollet was
experimenting with potassium chlorate gunpowder in 1800 he saw all his assistants
killed before his eyes and only escaped himself by a miracle. Later on, Dulong and
Gay-Lussac were injured by nitrogen chloride. Slow intoxication by fluorine was what
killed Knox and Louget; but in 1885, in the laboratory of Dr. Ribau at the Paris Faculty
of Sciences, Besson had nearly the whole of one band blown off when experimenting
with the same substance, and Rigaut (Professor Troost's preparator) lost one of his
eyes by a sudden explosion. In 1880 M. Zede had his thigh broken by a huge glass
stopper which was blown out of a bottle in St. Clair Deville's laboratory, and at the
Sorbonne in 1891 M. Lippmann's preparator, M. Letang, had his face badly burned.
M. Lucien Poincare, brother of the well-known French politician, received similar
injury when a bottle of nitric acid burst in M. Bouty's laboratory; while the burns that
MM. Becquerel and Curie received during their researches are part of the history of
the discovery of radium.

the Z man - 7-7-2010 at 06:36

Quote: Originally posted by The WiZard is In  
American journal of pharmacy, Volume 45. 1873.
EXPLOSIVE MIXTURE OF NITRATE OF POTASH AND ACETATE OF SODA*
BY M. VlOLETTE.

An accident in the author's laboratory made known to him a singular reaction
between nitrate of potash and acetate of soda, which, under the influence of heat,
constitutes an explosive mixture equal in force to gunpowder. In some researches
upon saltpetre he had heated moderately in a small phial a few grams each of nitrate
of soda and acetate of soda, both previously fused and anhydrous. The two salts
melted formed a colorless and transparent liquid, which gave off a few gaseous
bubbles. At the same moment, a violent explosion occurred,, accompanied by flame
and smoke, which scattered the phial in fragments all over the laboratory ; a fresh
gaseous combination between the elements of the salts had taken place, leaving a
slight residue of alkaline carbonate.

In repeating the experiment a gram of nitrate of potash was melted in a small
platinum capsule at a gentle heat, and a gram of acetate of soda previously fused
added to it. At a temperature of about 300o C the mixture remained fluid,
transparent and without alteration as long as the temperature remained constant ;
upon raising it to about 350° C. there was a slight ebullition followed instantly by a
loud explosion, with light and smoke, similar to that of gunpowder. As before, there
was a slight residue of alkaline carbonates. The same result followed when a
substance in ignition without flame was plunged, into the liquid at 300° C.

If the melted mixture be poured upon a cold surface a white
substance is obtained, which is hard, brittle, rather hygroscopic,
more fusible than nitrate of potash, and being melted explodes
violently In the solid form it does not burn when placed in
contact with an ignited body ; but reduced to fine powder, it
deflagrates violently upon the application of a flame.

The explosive properties of the mixture are only developed when the nitrate of
potash and acetate of soda are present in certain proportions—from 50 to 100 parts
of the acetate to 1OO parts of the nitrate—the most explosible mixture being 100
parts of the fused nitrate to 60 parts of the fused acetate. When the nitrate is in
excess, the combustion is only partial and of short duration : when the acetate is in
excess, the mixture burns slowly and similarly to a light wood.

A mixture of nitrate of soda and acetate of potash was found to have the same
explosive properties, but to be more hygroscopic. Mixtures of nitrate of potash with
the acetates of copper and baryta did not yield an explosive product.—Pharm. Journ.
and Trans. Jan. 11, 1873.

* Journal de Pharmacie et de Chimie, xvi, 333.



Somewhat similar to yellow powder. Interesting.... Anyway acetate and nitrate don't get on well together. There are a lot of stories about mixtures of HNO3 and acetic acid or acetates suddenly exploding.

Curie and Becquerel

The WiZard is In - 8-7-2010 at 06:00

Physiological Action of the Radiation from Radium.
H. Becquerel and P. Curie.
Comptes. Rend. 132 [22], 1289-1291.
In - The Journal of the Society of Chemical Industry, 8 [20], 845. August, 1901.

The action of the radiation from radium on the skin, announced by Walkoff and by
Giesel, has been confirmed by M. and Mme. Curie, and by Becquerel. Preparations
of radium, carried next to the arm or in the waistcoat pocket for periods of two to
six hours, gave rise to inflammation increasing very gradually, but lasting many
days, and leaving after treatment and recovery, little permanent scars. The intensity
of the physiological action depends on the activity of the radium and the duration
of its application. When handling radium and its compounds the finger tips become
hard and painful ; the pain often remains long after the inflammation has disappeared.*

* This and worse befell early experiments with Rontgen's
deadly Rays.


At no extra charge —

Metallic Radium
P. Curie and A. Debierne.
Comptes. rend., 1910, 151, 523-525.
In:— The Journal of the Society of Chemical Industry.
29 [18]1111-1112. September 30, 1910.

By making use of the method described by Gruntz (this J., 1903, 800 ; 1905, 278
; 1906, 80) for the preparation of barium, the authors have succeeded in isolating
metallic radium. A liquid radium amalgam, unstable in the air, was prepared by
the electrolysis of a solution of 0.106 grm. of pure radium chloride, using mercury
cathode (10 grms.) dried, transferred to an iron boat and heated in a quartz tube,
in an atmosphere of pure hydrogen, the pressure of latter being kept above the
vapour pressure of mercury at the temperature of the iron boat. Most of the
mercury had distilled over at 270o C., and the temperature was then raised
gradually to 700o C., when the whole of the mercury appeared to have been
expelled, and the radium commenced to volatilize ; the radium vapour vigorously
attacked the quartz tube. The residue in the boat consisted of a bright white
metal, melting at 700o C., which adhered strongly to the iron. The metal is rapidly
attacked by the air, becoming black, probably owing to the formation of a nitride.
It blackens paper and decomposes water, passing for the most part into solution ;
the dark-coloured residue dissolves completely on addition of a few drops of
hydrochloric acid. The radio-active properties of the metal appear to be normal.
As radium is much more volatile than barium, the authors propose to purify the
metal by sublimation in vacuo.

rrkss - 8-7-2010 at 07:26

Wizard, this thread is for personal bad days in the lab. I would prefer if you would create another thread for copy and pastes from newspaper articles.

JohnWW - 8-7-2010 at 07:38

I understand that Marie Curie and Becquerel died of cancers due to exposure to intense radiation from radium and/or polonium; and Pierre Curie, who also had cancer, would have also died from it if he had not been killed in a street accident.

Bad days in the lab or with glassware?

The WiZard is In - 8-7-2010 at 09:28

RKSS scribed 8vi2010

Wizard, this thread is for personal bad days in the lab. I
would prefer if you would create another thread for copy and
pastes from newspaper articles. [Emphasis added. The WiZard is
In.]


Oh!? How was this determined?

This from the original post.

So I'm sure that while accidents aren't funny, I'm sure we have
some minor things that aren't major accidents, or involve
breakage of glassware. I thought I'd share my bad day in the
hopes that others have had similar experiences. Perhaps there
is something to learn? [Emphasis added - again.]

Does the original poster own the thread, i.e., no reply can
expand upon it, or any post that does not with laser like
precision answers the question be not allowed?

I have an idea that would make this work. The original poster
we automatically be moderator of their thread and could allow
only whatever amused them.

Only one of the moderators with their God like powers could
move my C&P, &c. to another thread. If I were to start
another thread all the There is already a thread that covers
this topic, would crawl out from under their rocks complaining most loudly.

Absent a suggestion from a moderator ....

Why do I get the feeling that some of the chemical minded here —
got into chemistry when they flunked out of Indian bureaucrat or
French Customs Agent school?


djh
-------
Hexameter—

Hexameter, the name of the earliest and
most important form of classical verse in
dctylic rhythm. The word is due to each line
containing six feet or measures, the last of which
must be a spondee and penultimate a datyl,
though occasionally, for some special effect ,
a spondee may be allowed in the fifth foot.
The four other feet may be either spondees or
dactyls….. The most usual places for the
caesura are at the middle of the third, or
the middle of the fourth root: the former
is known as the penthemimeral and the latter
as hepthemimeral caesura.

Sedit - 8-7-2010 at 11:07

Quote:
Why do I get the feeling that some of the chemical minded here —
got into chemistry when they flunked out of Indian bureaucrat or
French Customs Agent school?


Because the chemical minded folks here for the most part can use google themselfs and don't need copy and paste exerpts to know what a bad day is like. They break there own shit, there glass, there mantles, there chemicals, recently my toe.... Thats a bad day in the lab.

But I digress, indeed you are right if it keeps your hyperactive copy and pasting to a generalized area then have at it. But I find anymore when I go to use the search engine much of what I find is early 1900 accidents and news reports that are not really that helpful at all other then I now know, john doe knows, not to blow his fingers off. Its an issue I have mostly keep quite about while others have bashed you for it but if you wish to repeatedly push my buttons then I will gladly open up if you wish.

psychokinetic - 8-7-2010 at 13:18

" thought I'd share my bad day in the
hopes that others have had similar experiences. Perhaps there
is something to learn? [Emphasis added - again.]"


Others, meaning us.

rrkss - 8-7-2010 at 22:21

I just posted that because I prefer to read about and hear personal stories of things that happened to members of this site in their own words. If I wanted to read copy and paste stuff, I'd google it myself.

This site is for amatuer chemistry and strange things happen in an amatuer lab. My most recent bad experience was running a water sensitive reaction outdoors and had a freak thunderstorm.

The WiZard is In - 9-7-2010 at 06:13

Quote: Originally posted by User  
Ohm man today sucked.
I broke a mercury thermometer.

I was cleaning the wall of my lab with some ammonia really nice black smudge coming of.
There was a thermometer hanging on the wall, it was an old one and the mercury had split because apparently it was lying down for a long time.
Anyway somehow I and my stupid head tipped the thing of the hook and it fell down on my desk.
It god damn shattered. :mad::mad:

So yeah i had tiny drops of Hg all over the fucking table top.
I spent 2 hours of cleaning it with an eye dropper and still not convinced that it is all gone.
I used the last of my sulphur on the floor.
Now ill be putting the radiator at max with the window open hoping to evap all of it.
Maybe ill put my gassmask on and use a blow-dryer.

What a way to start your freaking day.
Any one got some tips?



Tip? Yup.

Extracted from —
Management and control of Hg exposure
American Laboratory July, 1988
David N Easton
Scanned! And you know what that means!!



-------------------------------
Mercury spill cleanup procedures:

Because mercury will disperse into fine droplets throughout the area where it is
spilled, an effective cleanup procedure requires two steps. Always wear rubber
gloves and take care to avoid spreading the spill through inadvertent contact.
Wear appropriate respiratory protection if testing shows that levels of airborne mercury are high.

1) A trap consisting of a filter flask connected to a vacuum source at the
side-arm and a length of Tygon tubing at the inlet is used to collect all visible
droplets. A Pasteur pipet at the inlet end of the tube facilitates the pickup. A good
flashlight is essential for finding fugitive droplets.
2) After the gross contamination has been removed, sprinkle the entire area of
the spill with a liberal application of elemental zinc powder. Dampen the zinc
powder with dilute (5-10%) sulfuric acid solution to create a paste-like
consistency. Work the paste into the contaminated surface with a sponge or a
brush. After the paste dries to a light gray color, it may be swept up for routine
disposal. The residual material is removed with soap and water.

This procedure results in an amalgam of mercury and zinc (the acidic solution
shifts the equilibrium toward the bound product). The more conventional
treatment with calcium polysulfide or flowers of sulfur merely reduces the vapor
pressure by coating the droplets. Subsequent frictional forces can disrupt this
coating and result in additional vapor release.

Mr. Easton is a Certified Industrial Hygienist at the Universirty of Virginia,
Environmental Health and Safety Office. Charlottesville, Virginia. This paper was
excerpted from a lecture by the author at the American Industrial Hygiene
Conference in Montreal, Canada, June 1987.

Chlorate of ammonia

The WiZard is In - 10-7-2010 at 07:22

Memoirs and proceedings of the Chemical Society of London
By Chemical Society (Great Britain)
1843

April 4.—The President, Arthur Aikin, Esq., in the Chair.

77. " On the Spontaneous Decomposition of the Chlorate of Ammonia," by Mr. Joseph
Wonfor.

Having occasion lately to prepare a quantity of this salt, the phaenomena which form
the subject of this communication were observed.

The salt was prepared by adding to a saturated boiling solution of bitartrate of
ammonia a saturated boiling solution of chlorate of potassa, the liquor being
strained from the precipitated cream of tartar and cooled as rapidly as possible, it
being observed that the ammoniacal salt underwent a change if allowed to remain at
a high temperature for any length of time; the solution was then carefully evaporated
at a temperature below 100° Fahr., and again strained from a small portion of cream
of tartar which separated as the liquor was concentrated. The chlorate of ammonia
crystallizes in small acicular crystals, or in plates similar to the chlorate of potassa.
The crystals are very soluble both in water and alcohol, and have a sharp cooling
taste.

This salt was partially examined by Vauquelm, but he does not appear to have
observed the change it undergoes at the ordinary temperature of the atmosphere,
which most likely arose from his using the salt immediately after it was prepared.

In Murray-s ' Elements of Chemistry,- vol. ii. p. 544, it is stated that Vauquelin
examined this salt: the author remarks, " it crystallizes in fine needles, and appears to
be volatile, as there is a considerable loss on evaporating its solution ; its taste is
extremely sharp; it detonates when placed on a hot body with a red flame ;
decomposed by heat it gives out chlorine gas, with nitrogen and a little nitrous oxide,
hydrochlorate of ammonia with hydrochloric acid remaining."

Brande states, in his ' Elements,- on the authority of Vauquelin {Ann. de Chim. xcv.
97), that " this salt probably consists of one proportional of each of its components,
or 17 of ammonia + 7 6 of chloric acid; but its composition has not been
experimentally determined." I have analysed the salt, by decomposing it with caustic
potash, collecting the ammonia in water acidulated with hydrochloric acid, and
evaporating the solution carefully to dryness ; the chloric acid was determined by
igniting the salt, after the action of potash, in a porcelain capsule; then calculating
the amount by the weight of the resulting chloride of potassium, my results gave one
equivalent of ammonia, one of chloric acid, and one of water.

After the salt had been prepared a few days, the colour was observed to have
changed from white to lemon-yellow, and gave out an odour which powerfully
affected the nose when held over the uncorked bottle, irritating the eyes much more
than chlorine, and causing a flow of tears ; this odour was dissimilar to that of any of
the oxides of chlorine. The salt was put away till an opportunity should offer of
examining the cause of this change. On going into the laboratory some days after the
alteration in the appearance of the salt had been observed, the bottle, which
contained about 4 ounces, was found broken into innumerable particles, and the
remains of its contents strewed about the floor; on inquiry I was informed that
during my absence it had exploded with a loud report. Imagining the explosion was
produced by the bottle being closely stoppered, an ounce of the salt was introduced
into a very strong phial, and connected with a vessel containing a solution of nitrate
of silver, through which the products of the decomposition had to pass, the
unabsorbed gases being collected in a jar at the pneumatic trough, hoping to collect
the gases as they were liberated. After gaseous matter had been quietly evolved for
twelve hours, it exploded with greater violence than before, no portion of the bottle
remaining (except the neck) larger than a pea. A quantity of chloride of silver had
precipitated from the nitrate, and the gas jar contained free nitrogen. Another
portion of the salt was then placed on a sand-bath, the temperature of which was
about 120° Fahr. ; this soon underwent decomposition, but only detonated slightly,
giving off dense white fumes, with the smell of nitrous acid.

Finding the salt was so easily decomposed, I proceeded to examine more closely the
nature of the changes that took place. 20 grains of the salt were introduced into a
strong flask, connected, as in the previous experiment, with a vessel containing
solution of nitrate of silver, but with the mercurial instead of the pneumatic trough ;
the flask was then very carefully warmed by a spirit-lamp ; the salt instantly exploded
with great violence and a loud detonation, breaking the flask to atoms. Five grains of
the salt were then operated upon, without the vessel containing the solution of the
silver salt, and the products of the decomposition collected over mercury; they were
nitrogen, chlorine, nitrous acid and water, with a little chloride of ammonium; but
from the rapidity with which the gases were eliminated, it was impossible to collect
the whole of the products of the decomposition, though the experiments were
repeated six or seven times, both with and without the vessel containing the solution
of nitrate of silver. When five grains of the salt were employed, the tubes (which were
filled with mercury when no salt of silver was used) were not broken; still the action
was so energetic that it did not allow of accurate indications of the quantity of the
gases evolved being obtained.

From the presence of free nitrogen and chlorine, both in the products of the
spontaneous and produced decomposition, I am led to conclude that chloride of
nitrogen is formed; but as the whole of the products were in no case obtained, it was
impossible to determine this experimentally.

Alloy of potassium

The WiZard is In - 11-7-2010 at 06:34

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…….




Skyjumper - 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.

Argento-Chloride of Ammonia

The WiZard is In - 12-7-2010 at 07:17

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.

Pyrophosphorus

The WiZard is In - 15-7-2010 at 06:28


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.



Guess what just toppled off the bench ....!

The WiZard is In - 17-7-2010 at 06:37



Glassware-2.jpg - 133kB

Guess what just toppled off the bench?

The WiZard is In - 19-7-2010 at 09:38

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.



Glassware-2.jpg - 133kB

Panache - 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]

Sedit - 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.

psychokinetic - 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.

Panache - 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.

peach - 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

DDTea - 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.

psychokinetic - 27-7-2010 at 17:54

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

aonomus - 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.

Sedit - 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..........

peach - 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]

The WiZard is In - 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.

peach - 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.

peach - 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]

The WiZard is In - 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]

psychokinetic - 17-10-2010 at 00:09

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

hissingnoise - 17-10-2010 at 10:39

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

Bad day

chemx01 - 17-10-2010 at 12:19

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.

aonomus - 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...

The WiZard is In - 18-10-2010 at 06:45

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



The word is definitely not sanguine.

peach - 18-10-2010 at 11:08

Yeah, I'd agree with anomonus, sealing that was a bad idea.

I've never had a conical break under vacuum, or heating, despite going through a period of using them solely on a regular basis. Good luck is very random in it's occurrences.

{penises}
I saw a documentary all about extreme body modification. It started getting 'a bit dodgy' with the implanted crufices on the forehead, then went further and started with bisected penises. The doctor's reaction on seeing the photos was perfect. Pure silence for a few seconds then... "I suppose, if you're thinking of doing this, you really should consider psychiatric help".

There are also guys on the net cutting theirs off at home, for reasons entirely unknown to me.

For a real cringe, have a look for videos of emasculating livestock. One of them involves something that looks like a pair of pliers and a cordless drill. The 'pliers' are in the chuck. Guess the rest of that. It involves spinning.

[Edited on 18-10-2010 by peach]

aonomus - 18-10-2010 at 13:46

Um, I'll pass. This has nothing to do with bad days in the lab or with glassware. [/derail]

peach - 18-10-2010 at 21:55

I'm afraid I agree with the reply much earlier on in the thread, suggesting this was a bit of a silly question to start with.

Experiments gone wrong? The list is gigantic.

And reading someone else's opinions on the finer details of one specific situation won't stop a complete beginner from making the same mistakes, unless it's a very specific question.

I have two bits of advice regarding glassware.

1.) Don't keck clip the entire thing, and think about where you put them. I've had water back syphon when I was first distilling sulphuric, hit the sulphuric near 98% and 300C+, then blow a Hollywood style volcano out of one of the ports. Lucky for me, I'd left that one unclipped for that reason, as the flasks may have popped instead.

2.) If you have a big stretch of condenser and a big flask filling up on the other end, use a ball / cup joint at the still head so the condensing section has some degree of movement. A lab jack is good, but a ball / cup joint is cheaper and provides genuine flexibility and 100% clamping. A lab jack will still leave the glass strained to some degree, whereas the joint will let you rigidly clamp both the receiver and the starting point, with it taking up the error and strain. You'll see the cold fingers on rotovaps often have a ball / cup on the receiver flask for that reason, so the weight of the solvent can find it's own centre of gravity without snapping the joint. They also feature as permanent joints on the more expensive, large scale glass.

You can get ball / cup adaptors that go onto the straight tapers to add the 10-15 degrees of flex. Don't over tighten them, they'll never be rigid, they're not supposed to be, you'll just break it.

[Edited on 19-10-2010 by peach]

Magpie - 3-12-2010 at 11:53

I recently had a bad day with my buret. It hit the frame as I was removing it from my hood and I dropped it. I have a rubber mat on the floor so breakage happened only when it hit the cabinet on the way down.

The top 1" was broken off jagged but I trimmed that edge clean with a diamond wheel Dremel tool. As you can see I also broke the tip off. It is useable with a Scotch tape splice but I'd like to fuse it by glassblowing. I'm pretty sure it is borosilicate.

I would like to ask the experienced glassblowers if they think this is advisable. My glassblowing skills are rudimentary. For tools I have propane, MAPP gas, a regular bunsen burner, and a Meker burner.

Edit: Th ID of the tip at the break is ~2mm.

What do you advise?

buret tip.JPG - 44kB

[Edited on 3-12-2010 by Magpie]

watson.fawkes - 3-12-2010 at 13:11

Quote: Originally posted by Magpie  
I would like to ask the experienced glassblowers if they think this is advisable. My glassblowing skills are rudimentary. For tools I have propane, MAPP gas, a regular bunsen burner, and a Meker burner.

Edit: Th ID of the tip at the break is ~2mm.
I'm just guessing that you might want to work glass generally. Just guessing. If you don't, send it out for repair or scrap it. The ante for any (sane) glassworking in borosilicate is eye protection. Expect to drop on the order of $100 for something adequate. And then you can start spending more.

Get some 2 mm ID tubing and practice on that. Your first butt joints won't be adequate. For instruction, there are a number of out-of-copyright books that adequately show how to do this.

You'll likely need a finer flame than the burners you've got. You'll have an issue holding the small end while rotating it, even with a smaller flame. You may need to make a jig.

Propane/oxygen will be fine; propane/air may well not be hot enough.

There's more, if you want to go down this road.

UnintentionalChaos - 3-12-2010 at 18:12

Am I the only one who seems to keep breaking Keck clips? I've got some of the cheap off-brand ones and some good quality ones and neither seems to be immune to breaking. I own a 4-neck 1L flask and a 1-neck 1L as my largest flasks. Whenever I need more than one neck (like now), I have to stopper all the spare necks on the 4-necker. Now, being that constant breakage has my keck stock pretty low, I just left some of them with a heavy amount of grease while distilling off azeotropic HCl. So far, I've had 2 different episodes (over ~13hrs of distillation) where they've blown loose, spraying hydrochloric acid fumes into the air and getting droplets in the oil bath. This has forced me to move all the semi-available keck clips to the distillation flask.

As I was cleaning up the last one, the keck clip holding the recieving flask simply broke in half and fell onto the bench. I have no spares, but it is sitting firmly against a solid surface now (and I'm not under exclusion of air, so that's a non-issue).

I've looked into metal kecks, but they're a fortune when you'd need to buy 10 or so.

Aside from that, this distillation is infuriatingly slow. Even turned way up, and with wads of insulation, I can't squeeze enough power from my Corning PC-351 hotplate/stirrer to get a good distillation rate on anything water based. I'm getting less than a drop per second which makes reagent prep maddening.



[Edited on 12-4-10 by UnintentionalChaos]

Magpie - 3-12-2010 at 19:03

Thanks watson for your reasoned advice about repairing my buret. I don't really want to take on glassblowing so will live with what I have (Scotch taped) until I find a bargain on eBay. It seems like you can't even buy a decent glass buret for under $50-$100 on the open market. I'm sure I didn't pay over $25 for mine on eBay but that was some time ago.

I've ruined quite a few of the cheaper Keck clips, usually by overheating. I bought some Teflon clips that are quite beefy and a lot better, and will take a higher temperature too. But they are quite spendy.

In school we had some ss clips that used a spring, but I've never seen them for sale anywhere. I've been toying with the idea of making my own out of ss308 3/32" TIG welding wire. Garage chemist has some ss clips but I can't tell (from his pictures) if they are purchased or homemade.

watson.fawkes - 3-12-2010 at 20:15

Quote: Originally posted by Magpie  
Thanks watson for your reasoned advice about repairing my buret. I don't really want to take on glassblowing so will live with what I have (Scotch taped) until I find a bargain on eBay.
You can use a cyanoacrylate glue for a non-permanent repair, assuming the break is clean.

UnintentionalChaos - 3-12-2010 at 20:35

Quote: Originally posted by Magpie  
Thanks watson for your reasoned advice about repairing my buret. I don't really want to take on glassblowing so will live with what I have (Scotch taped) until I find a bargain on eBay. It seems like you can't even buy a decent glass buret for under $50-$100 on the open market. I'm sure I didn't pay over $25 for mine on eBay but that was some time ago.

I've ruined quite a few of the cheaper Keck clips, usually by overheating. I bought some Teflon clips that are quite beefy and a lot better, and will take a higher temperature too. But they are quite spendy.

In school we had some ss clips that used a spring, but I've never seen them for sale anywhere. I've been toying with the idea of making my own out of ss308 3/32" TIG welding wire. Garage chemist has some ss clips but I can't tell (from his pictures) if they are purchased or homemade.


I can buy metal ones on ebay here ($9USD!! each :(), but I've never seen the PTFE ones. Just did a bit of research, looks like they're made for quickfit. Do you know offhand if quickfit sizes are compatible with US standard taper? I think the answer is yes, but I'm not entirely sure.

Magpie - 3-12-2010 at 22:03

Here's where I bought mine, a pkg of 5, part no. 89026-174 for size 19. I see they have other US sizes in the other part no. shown.

https://www.vwrsp.com/psearch/ControllerServlet.do?D=89026-1...


If you want to see what they look like see:
http://www.sciencemadness.org/talk/viewthread.php?tid=14768#...

psychokinetic - 7-12-2010 at 23:10

I'm sure someone mentioned the ability to google up there somewhere . . .

jtalmodovar26 - 1-1-2011 at 20:03

Accidentally took a huge whiff Ammonia and a collection of Iron Chlorides. My Eyes stung for awhile

kuro96inlaila - 1-1-2011 at 20:07

I don't know what to say,am I cursed or something?

Everytime I use an evaporating dish,sure it will broke!:(

Everytime............

Magpie - 1-1-2011 at 20:12

Quote: Originally posted by kuro96inlaila  

Everytime I use an evaporating dish,sure it will broke!:(

Everytime............


Are you heating it with a bare flame?

jtalmodovar26 - 1-1-2011 at 20:22

Yeah, I thought You were supposed to put a metal screen inbetween the dish and the flame?

Magpie - 1-1-2011 at 20:27

Quote: Originally posted by jtalmodovar26  
Yeah, I thought You were supposed to put a metal screen inbetween the dish and the flame?


That's what I have concluded too. I broke my 6" dish that way.
Also, I was heating some solids which hadn't yet liquified so heat transfer was poor and uneven.

kuro96inlaila - 1-1-2011 at 20:32

Quote: Originally posted by Magpie  
Quote: Originally posted by kuro96inlaila  

Everytime I use an evaporating dish,sure it will broke!:(

Everytime............


Are you heating it with a bare flame?


No,I heat it on a wire gauze.

Magpie - 1-1-2011 at 20:39

Quote: Originally posted by kuro96inlaila  

No,I heat it on a wire gauze.


Sorry for the mixup.

So you are using a wire gauze. Are you heating a liquid or a solid? Are you bringing up the temperature gradually and evenly?

Or, tell us what you are doing. It's always easier to address a problem when we know the details.

kuro96inlaila - 2-1-2011 at 06:10

Hm,I usually heat a liquid in it,
maybe temperature shock cause it to broke,
but I expect porcelain didn't have problem with that,
or does it?:o

bob800 - 2-1-2011 at 09:08

Quote: Originally posted by Magpie  
Here's where I bought mine, a pkg of 5, part no. 89026-174 for size 19. I see they have other US sizes in the other part no. shown.

https://www.vwrsp.com/psearch/ControllerServlet.do?D=89026-1...


Does VWR sell to individuals?

Magpie - 2-1-2011 at 09:22

equipment, yes

[Edited on 2-1-2011 by Magpie]

watson.fawkes - 2-1-2011 at 09:27

Quote: Originally posted by kuro96inlaila  
maybe temperature shock cause it to broke,
but I expect porcelain didn't have problem with that,
or does it?:o
All ceramics can be thermally shocked into breaking. Some are more resistant than others.

A very simple sand bath can ameliorate this: a metal plate with a rim, 1/2" of sand, evaporating dish on top. Increasing the thermal mass and the thermal conduction pathway evens out the heating profile at the cost of using a bit more heat.

bob800 - 2-1-2011 at 15:57

Quote: Originally posted by Magpie  
It seems like you can't even buy a decent glass buret for under $50-$100 on the open market. I'm sure I didn't pay over $25 for mine on eBay but that was some time ago.


Cynmar has some Class B teflon-valve and Class A glass-valve burets for <$20:

http://www.cynmar.com/item_detail.aspx?ItemCode=11520624.

http://www.cynmar.com/item_detail.aspx?ItemCode=11520660

kuro96inlaila - 3-1-2011 at 05:15

Quote: Originally posted by watson.fawkes  
Quote: Originally posted by kuro96inlaila  
maybe temperature shock cause it to broke,
but I expect porcelain didn't have problem with that,
or does it?:o
All ceramics can be thermally shocked into breaking. Some are more resistant than others.

A very simple sand bath can ameliorate this: a metal plate with a rim, 1/2" of sand, evaporating dish on top. Increasing the thermal mass and the thermal conduction pathway evens out the heating profile at the cost of using a bit more heat.


Thanks for the information!:)

peach - 3-1-2011 at 06:48

I can 100% confirm that borosillicate can be thermally shocked into shattering.

The smaller the glass is, and the simpler, the less and less likely it becomes. But, when working with multiple litres, or tens, it will shatter if it's not warmed and cooled uniformly and gently. The specific heat capacity of the liquid is another thing. I mean, to warm up a volatile solvent you will need very little energy, but something like water means there's a big, cold heat sink on the other side of the glass, and a thousand degree flame on the other.

For example, if you're working with ten litres of cold / RT water, that will take a long time to warm up to boiling, and a lot of energy. You really want to be using a mantle specifically for that size of flask, a big bath or a heating jacket of some form.

With 10's of mls (as you'd work with at school when 16-18), I can stick blow torches directly on the glass and it's fine.

I was in Italy at one point and the tour boat took us to a decorative glass blowers. The guy made a little horse, like you'd see on a Ferrari, then set it on the bench in front of us as he got going on something else. Around a minute later, as it cooled, it shattered into a broken pile on the desk.

Painful glassware incidents;

- Bursting a 10l flask

- Forgetting to weigh down my clamps and leaving a distillation to run. The receiver filled up, altered the weight distribution and toppled the vigreux, still head, condenser, vacuum receiver bend and receiver flask. I'm not sure which shattered more, the receiver bend or my heart.

- I have also broken two evaporating dishes, but through needing to tidy up / take more care rather than heat. If you're dish is 6" and reasonably tall, and filled with cool liquid, and being heated by a bunsen, it may be that you're simply applying too much heat too quickly. If you can, turn the gas down and set the flame so it's just going blue, to warm it more gently. Another simple solution is to not try warming so much at once. Pour SOME of your solution in and let it warm, then add the rest in portions until it's done. Filing glass too high from the start creates another major problem - wiping up the splashes on the surface :)

- Although it's never broken any glass, I am always annoyed when a solution thickens and the stir bar breaks free. It start swirling round and round like a coaster at the fair and, the motor free wheels and starts vibrating, and the glass tries to do the washing machine dance.

All the best to all my science nerds for christmas and new years (even the ones I argue with, who are probably my best nerds),
John

[Edited on 3-1-2011 by peach]

Saerynide - 3-1-2011 at 07:43

Quote: Originally posted by peach  
Although it's never broken any glass, I am always annoyed when a solution thickens and the stir bar breaks free. It start swirling round and round like a coaster at the fair and, the motor free wheels and starts vibrating, and the glass tries to do the washing machine dance.


Omg. I cant agree with that one more! Ive had a stir bar in a scintillation vial of a viscous pre-polymer mixture. The vial started to do the resonating washing machine thing when i wasnt watching and before i knew it, it unscrewed the cap and then flung my sample everywhere :o I couldnt even scoop up my sample to re-purify since it for bio stuff :(

peach - 3-1-2011 at 08:56

In response to.... MAGPIE
Quote:
It seems like you can't even buy a decent glass buret for under $50-$100 on the open market. I'm sure I didn't pay over $25 for mine on eBay but that was some time ago.


Quality certainly does cost when it comes to class A and new. The guys buying that stuff will get very picky as well - for example, they'll make sure their solutions are actually at 20C (or the specified temperature), density is another. If it's a high resolution balance, aw... then you're in trouble. :D You'll have to redecorate to make it happy.

If you're into high accuracy work, there is a great PDF on google that goes into a lot of detail about the standards, films on the glass and so on.

I had a look for you but couldn't easily find it. If you google 'glassware to dispense to contain' you may be able to find it and the related documents. The one I'm thinking of is pages long and discusses the difference between ISO / BS and other standards.
Quote:

I've ruined quite a few of the cheaper Keck clips, usually by overheating. I bought some Teflon clips that are quite beefy and a lot better, and will take a higher temperature too. But they are quite spendy.


I am beginning to dislike standard keck clips. They're polyacetal.

They do indeed melt at too low of a temperature to be reliable - 125C from memory. That is well within the region of a normal distillation, meaning columns / flasks / heads and condensers need care when using them, because it is easily possible to soften / warp / melt the clip and have the glass fall apart.

In fact, I've just finished cleaning one off my vigruex after it did that trick.

Polyacetal is used because it is is reasonably resistant to chemical attack.

It is not, however, resistant to acid hydrolysis. This means if you're working with strong acids you have potential problems.

Acid gases are even worse.

Worse again, the polymer is particularly sensitive to chlorine donors. Meaning, hydrogen chloride is not it's friend at all.

I can promise you, I have thrown out a handful of clips that have literally fallen apart in the presence of tiny amounts of the gas escaping through Krytox greased QuickFit tapers.

It's worse than them melting, because there's no warning sign that they're about to go. They'll be absolutely fine, then a funnel will fall off and the clip with be split.

They can't handle it, at all.

There is a guy in the US, I think it's Expediglass on eBay, selling polyacetals for a lot less than united glass, who sell Schott Duran's clips. I have tried some of those. They're from China, because the envelope says so. They look kind of cheap in terms of them being faintly pigmented, but they perform just as well for a lot less money.

Schott Duran, QuickFit and Chemglass (they call it Durite - marketing balls) all use polyacetal as their standard for keck clips.

Stainless.... yes! Much higher temperature. However, stainless, even Innox, does start to corrode around the reactive gases. Only monel will withstand those outside of the platinums and it's not a standard alloy for most people (it's nickel based, rather than iron, and expensive).

If you're after the springs, Chemglass do them. But they're $18 for 6 tiny ones I think. You may be better eBaying those, as quite a lot of odd stainless or titanium springs and bolts appear on there for the engineering folk and guys doing their super bikes up.

I have a small number of them. They hold the receiving test tubes on the end of my short path. But... the tubes also take keck clips. And only the receiver tubes have the spikes for using them. The rest of the glass doesn't.

The only immediate benefit I see to springs is that they add a layer of insurance against the glass bursting, by letting the joints open if there's a sudden pressure rise. Other than that, they're fiddly and easy to loose.

PTFE is seemingly the best. The 250C temperature limit is dead on for what's needed during most organic work. The chemical resistance is second to none. They may swell with extreme solvent exposure, as PTFE does this around halogenated solvents.

But, at a whopping £7 PER CLIP, they certainly are NOT cheap!

The only person I've seen on here using them is Klute, who also has the tapered and screw together glass - again, the only person I've seen on here with it. I have two of the G thread to B taper PTFE adaptors, but none of that really detailed gear. Sigma sell it as System 45 with the Ace brand on it. There is also Rotaviss. I think System 45 is produced by ndstechnologiesinc.com. It's all over their page, they reference you to Sigma and I've had a chat with them - that's where my adaptors came from.

I think you can rest assured the PTFE clips weren't a waste.

I have wondered about making my own. The standard ones at the moment are moulded, which is very expensive to do with PTFE. I was thinking it'd be cheaper to buy a bar of it and simply cut them out. If I do, and they work, I'll stick some up on here for others to grab.

[Edited on 3-1-2011 by peach]

UnintentionalChaos - 3-1-2011 at 09:02

Quote: Originally posted by peach  

I have wondered about making my own. The standard ones at the moment are moulded, which is very expensive to do with PTFE. I was thinking it's be cheaper to buy a bar of it and simply cut them out. If I do, and they work, I'll stick some up on here for others to grab.


I'm under the impression that the PTFE clips are actually steel with a PTFE coating.

peach - 3-1-2011 at 14:01

They are.

At least the ones I've seen.

Moulding PTFE like that is not easy, hence the price - pure PTFE is A LOT cheaper than that.

If it can be done with polyacetal, I expect it could also be done with solid PTFE.

They may be using a steel wire due to the moulding process. A lot of moulded PTFE is 'grainy' and more like billions of bits of PTFE dust stuck together; sintered (it's not a thermoformable plastic so it can't be injection moulded or heat formed, which is it's main drawback and why things like PFA, FEP and ETFE came about). This is why I can stain PTFE stir bars black with precipitate - it's getting stuck in the grain structure.

It's moulded isostatically, where a lot of pressure is applied from each direction and the mould is then warmed up to squeeze and melt the grains together - so I guess it's a bit like a frit in that sense.

That's 'grainy'ness would not be good if that's all you were relying on for support.

Virgin, solid bars of PTFE don't have this, as they come fresh out of the polymerization.

[Edited on 3-1-2011 by peach]

peach - 3-1-2011 at 14:25

Quote:

I can buy metal ones on ebay here ($9USD!! each :(), but I've never seen the PTFE ones. Just did a bit of research, looks like they're made for quickfit. Do you know offhand if quickfit sizes are compatible with US standard taper? I think the answer is yes, but I'm not entirely sure.


I've used clips from the US on my QuickFit in the UK (QuickFit is a trademark of SciLabWare, and it's blown in Staffordshire in the UK - I have actually had a chat with SciLabWare about this and, if you check the wiki on QuickFit, I've added all the different names the glass has been blown under since they formed and the company merged with others). The glass had always been trademarked QuickFit, but the company name has changed quite a few times.

I wanted to make it clear in that article that quickfit does not mean 'tapered glass'. QuickFit is an actual trademark and sold by a specific company.

Works fine, there's no difference. ;)

The only important thing is the diameter, and that's the same for the UK and US tapers - only the length is different.

In the UK, the length is always the same for each B number. In the US, people like Chemglass will change the lengths a bit for each. There is more variation in the clamping between manufacturers and regardless of region based on how thick the ring section is around the top of the female joint. Regardless, they all clamp fine for glass and chemistry (tried Chemglass, Kontes, LIG, QuickFit and custom blown; there's no major difference).

I have found a couple of places doing the PTFE clips. One of them was some stoner's place selling pipes and bongs made with lab tapers on them, but they're all about the same price... £7 a clip.

Use sparingly.

It's probably a good thing, as clipping all of your glass means that bitch is going to burst (explosively / in flames / with cuts / burns) if something goes wrong.

Stoppers and such don't really need tightly clipping.

It's better then open and make a mess than the entire thing goes up.

[Edited on 3-1-2011 by peach]

The WiZard is In - 4-1-2011 at 07:35

Quote: Originally posted by kuro96inlaila  
I don't know what to say,am I cursed or something?

Everytime I use an evaporating dish,sure it will broke!:(

Everytime............



Buy one made of Corning Vycor® glass (Code No. 7913 glass,
96% silica). Corning years ago demonstrated it by pouring molten
lead into a Vycor dish sitting on a block of ice. My old (not dated)
Corning catalog only lists two sizes 45ml and 100ml.

Krell metal dobe better, however, the ship carrying the last
shipment of the metal from Altir-4 was forced down on the
planet Dubious-7 and has hot been heard from since.

http://en.wikipedia.org/wiki/Text

PS - Never/ever put one of them side arm vacuum flasks over a burner.

I wouldn't put mine on a hot plate.

peach - 4-1-2011 at 14:43

Do you know how the price of vycor compares to genuine fused quartz?

For the really slippery fingered, there is PFA 'glassware'. :D

Expensive is perhaps putting it mildly ($122 for a 100ml single necked flask, $473 if you want the luxury of three necks).

I think it must be used for hydrofluoric work and things like that.

[Edited on 4-1-2011 by peach]

The WiZard is In - 4-1-2011 at 17:34

Quote: Originally posted by peach  
Do you know how the price of vycor compares to genuine fused quartz?


Not oft hand... however, in my out of date Corning catalogue
Vycor is 10-12X the price of Pyrex. In my 1971 Lab Glass Inc.
catalogue the only quarts parts listed ground glass joints
(complete sets) the 45/50 is 5X more expensive then Pyrex.

I suffer from the feeling backed up by NO info - that for more
complex glassware there will be a greater difference on the plus side.

Nothing a little time w/ Google couldn't answer.....

peach - 5-1-2011 at 01:52

I'd love a whole set made out of fused Q, I know you can get it custom blown - but that's a lottery win scenario.

About the only thing I think I'd need from it are some bits of tube for lining furnaces - that's probably a bit more realistic.

Lambda-Eyde - 5-1-2011 at 05:29

http://www.technicalglass.com/

The WiZard is In - 5-1-2011 at 07:39

Quote: Originally posted by Lambda-Eyde  
http://www.technicalglass.com/



Curious do be I... they give the permeability for —
He, H2, Deuterium and Ne. Wonder I what quartz's
permeability to I2 — which it is claimed can migrate through
common glass is?

peach - 5-1-2011 at 09:46

Awwwww nice!

It may be a slow process, but I've never had any problems, or signs, of iodine getting into the glassware, let alone through it - and I have used extremely concentrated solutions of it (as it's perfectly fine to buy loads of it in England :)).

The other materials they've listed are for the physicist.

Quartz is quite often used for windows and apertures on ultra high vacuum equipment or weird furnaces.

A lot of physics involves deep UV to gamma spectrum radiation.

Normal glass is too opaque for that. I contacted Heraeus at one point about extreme UV lamps and they said even the quartz is annoying, as it has an opaque region between the end of UV and start of gamma.

Of coarse, many of these lamps are deuterium filled and have a quartz window. Helium, hydrogen and the other light gases are the main problems for ultra high vacuum, as they are a bugger to get rid of - e.g. hydrogen is often trapped in steels, and then bleeds out.

[Edited on 5-1-2011 by peach]

The WiZard is In - 5-1-2011 at 11:35

Quote: Originally posted by peach  
Awwwww nice!

It may be a slow process, but I've never had any problems, or signs, of iodine getting into the glassware, let alone through it - and I have used extremely concentrated solutions of it (as it's perfectly fine to buy loads of it in England :)).



Patience Grasshopper.


67. The permeability of glass to iodine and bromine vapours.
James Brierley Firth. Jour. Chem. Soc. Lond., 117, 1602-3 (1920).
—Iodine and bromine do not diffuse through glass under ordinary
experimental conditions. Only in extreme cases is there a
possibility of such diffusion. After a period of nine and one-half
years, iodine was found to have passed through a glass bulb 0.208
mm. thick. The bulb was heated to 360 °C for 100 days during the
experiment. In this experiment the bulb was placed in a large tube
and both tube and bulb evacuated. In another case, in which
iodine was found to pass through 0.211 mm. of glass, there was a
vacuum outside of the bulb and atmospheric pressure inside. here
was no evidence of bromine passing through a similar thickness of
glass after nine and one-half years. J. L. C.

http://tinyurl.com/33ct5wb

Possible others — I stopped looking after finding the above. /djh/

-------
Some years back Nature [England] had a series on long term
experiments, the one I remember was tar that every
70(?) years a drop fell from its funnel like container.


/djh/
-----
There are more things in heaven and earth, Horatio,
Than are dreamt of in your philosophy

[Edited on 5-1-2011 by The WiZard is In]

[Edited on 5-1-2011 by The WiZard is In]

This is your drige

smuv - 19-1-2011 at 16:40

*sobs* I broke a 3000L RB flask today. It was full of nearly 100g of freshly crystallized paracetamol.

It all started when I put the flask down to get a spatula, I just layed it on its side because I didn't have a cork ring on hand...I noticed across the room it was rolling off of the table. I shouted NOOOOOOOOOOOOO and ran across the room, throwing the spatula and disposable pipette (another casualty) in my hand. I didn't make it in time. You can't save 'em all.

Oh well, nothing gold can stay.

psychokinetic - 19-1-2011 at 18:28

3000L?

I sure how you meant mL, or else there are pictures necessary :P

UnintentionalChaos - 19-1-2011 at 18:37

Quote: Originally posted by psychokinetic  
3000L?

I sure how you meant mL, or else there are pictures necessary :P


It can go with Peach's 600m vigreux column. We're working on a full distillation setup for the Atlantic ocean.

smuv - 19-1-2011 at 19:02

lol. Peach, lets do it. Anyone got a heating mantle for this?

User - 20-1-2011 at 01:03

Lol , that happened to me 2 once (although not with a 3000L flask).
I use empty tape rolls as stands for rbf's :)



As for other stupidity:
It was a hot summer day and I needed some alcohol :P
So i filled up my 2 litre rbf with denaturated spirit.
Put on a vigreux and stoppered it to cover it from dust.
Went to a store etc etc, came back....


This was no pretty sight, the vigreux had launched itself apparently.
Probably because of to much pressure from the vaporizing alcohol.
another 200mm vigreux shattered to pieces, these things are too expensive for foolish actions like mine.
I thought about blaiming the cat :P , no this was just stupid.


[Edited on 20-1-2011 by User]

The WiZard is In - 20-1-2011 at 10:38

Quote: Originally posted by smuv  
*sobs* I broke a 3000L RB flask today. It was full of nearly 100g of freshly crystallized paracetamol.


Amateur.

Theodor Grewer
Thermal Hazards of Chemical Reactions
Industrial Safety Series Volume 4
Elsevier
1994


Explosion-Chemical-plant-1.jpg - 217kB Explosion-Chemical-plant-2.jpg - 185kB

Saerynide - 21-1-2011 at 10:01

Had my first implosion today... I put a rack of my samples in a supermassive vacuum dessicator, hooked up the vacuum pump and went off to lunch. When I came back to check on my samples, I saw what looked like really nice crystals where my samples were. Then I realized they were no crystals, but glass shards. I thought "what?? My vials imploded?? Thats not even physically possible!!" Then I saw the gaping hole and giant crack that almost split the 18 inch lid in half... The damn thing mustve had a hairline crack that no one noticed all this time :(

I am soooo thankful I put it in the fume hood and pulled the sash down all the way before I left... I'd hate to have my team cut up by exploding shards of 1/4 inch thick glass :S Im also glad it happened over lunch when the lab was empty. Woulda scared the living shit out of everyone :P I had even thought of wrapping it in duct tape before, but since no one had all these years before me, I decided itwould be over kil and they would look at me funny...

The WiZard is In - 21-1-2011 at 10:39

Quote: Originally posted by Saerynide  

I had even thought of wrapping it in duct tape before, but since no one had all these years before me, I decided itwould be over kil and they would look at me funny...



Me thinks the chance of anyone doing this is ....

Glass blowers after they anneal their work — put in between two
polarizers and look for stress. Would work for cracks
me thinks.


djh
----
Cunning, Care and Sheer Luck Save Rare Map
NY Times 17i11

White lines were visible where the map had ripped, the brighter inner fabrics of the
paper standing out from the stained surface. Mr. Derow visited Argosy Book Store on
the Upper East Side and bought a handful of obscure old books - among them, for
example, "The Select Dialogues of Lucian, to Which Is Added, a New Literal
Translation in Latin, With Notes in English," from 1804 - that were printed on cloth
paper, like the map, and not wood pulp.

He performed on them a technique that should chill the blood of any author,
wondering where his books will be in 200 years: he baked them in his kitchen stove
and boiled them in water. He painted the resulting brackish stew onto the white
lines, matching them to the rest of the map.



hissingnoise - 21-1-2011 at 11:02

Quote: Originally posted by User  

I thought about blaiming the cat. . .

The cat? You can't just let any animal into your lab!
If you want a pet in the lab - get a lab-rador . . .

peach - 21-1-2011 at 11:34

<iframe sandbox title="YouTube video player" class="youtube-player" type="text/html" width="640" height="390" src="http://www.youtube.com/embed/FkXwNQwrxZ4" frameborder="0" allowFullScreen></iframe>



Saerynide - 21-1-2011 at 22:07

Wow that is so neat! I cant believe I didnt know about this all this time :o

Sedit - 21-1-2011 at 22:55

Yeh LCD screens work by bending polarized light thru liquid crystals hence you need a series of Filters to cause the floresent tubes behind the screen to turn into an array of colors.

Floresent tube->Filter->Liquid crystals---light bent-->Filter= Color
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