Safety in alchemical experiments

Alchymical survival.

Some notes on safety in alchemical experiments
by Tom McRae.

1. MERCURY. Beware of any process involving distillation of mercury unless you have had extensive training in such techniques and possess a fume hood and relevant equipment. Mercury is no substance for the kitchen table chemist! Never handle it with bare hands. It may be fun but you'll absorb small amounts which accumulate until they reach harmful levels. Should you spill any, collect it immediately, you can absorb it in small quantities using a sponge. Squeeze the metal from the sponge into a jar containing some water, cover, and set aside. Do not dispose off down the sink, try selling to a scrap dealer instead. Same applies with broken thermometers, sponge up any spillage and put the lot, along with broken thermometer bits, into your water jar. Remember that despite its apparent solidity mercury is highly volatile and you can easily inhale the toxic fumes.

2. PHOSPHORUS. Gloriously alchymickal element with a cryptic message concealed on all containers. It says....LAY OFF! This stuff is very very bad in the hands of untrained workers and has accounted for a few trained ones as well. A fleck on your skin will burn pretty deep. Same applies to

3. SODIUM and POTASSIUM. Play safe, don't use if you don't know how. Nobody can tell you how with an email. If you need them take an advanced chemistry course.

4. ACIDS. Never forget the old dictum inscribed on Enoch's pillars (maybe) and in every sane textbook. ADD ACID TO WATER...NEVER WATER TO ACID! Why? The water will heat up rapidly in contact with the denser acid and things will start spurting around your wife/mother's kitchen and all over YOU. And do add that acid very slowly to the water with full precautions. Can't do without acids but handle them with care. Wear a full face visor, (you can buy those as industrial face protectors), rubber gloves, and a plastic or rubber apron. You'll look odd but not half as much as you would with half your face burned off! If you must use hydrofluoric acid be especially careful, this stuff can eat through glass. If it gets on your skin it is very difficult to remove completely and can cause severe ulceration. Glacial acetic acid's fumes are enough to spot preserve living tissue cells, imagine what it will do to the inner lining of your lungs if you inhale it. It's not just extra strong vinegar. Should you accidentally splash any acid on your bare skin don't panic, wash it away immediately with lots of cold running water. If you're a chem freak don't even think about preparing a neutralising agent. The professor of inorganic chemistry at the University of Edinburgh in the late 40's had a drop of sulphuric acid spurt into his eye. To show off to his students he calculated the relevant amount of neutralising agent required and washed the acid out. He neutralised the acid O.K. but lost his bloody eye! Cold water, running fast O.K.? If you spill the stuff once again don't panic. Keep a bag of kitty litter around, unused naturally. If you've a neutralising agent handy such as bicarbonate of soda, or even ground chalk, scatter this liberally over the acid. No matter what you do you've ruined the floor already. Scatter kitty litter very liberally over the neutralised acid until it's all absorbed. Put on those rubber gloves and carefully sweep the lot into a plastic dust pan. Pour into a plastic bag, and dump. Wash what's left off the floor area very thoroughly with a squeezy mop and lashings of water and hope nobody notices the mess that's left. Blame it on the cat. If you must dispose of acid the acid to water rule can be suspended. Put on that visor and the gloves and get your cold water tap running fast, but not spraying around. Very carefully and slowly trickle small quantities of your acid into the water, be very very slow and careful with this process and you'll be all right.

5. BENZINE. Used to be quite a routine solvent, in the seventies it was found that it was highly carcinogenic and accumulative. There is evidence that leukaemia in petrol station attendants was caused when this was used as an additive. If your process calls for benzene use toluene instead, still quite nasty but preferable.

6. ETHER Great stuff for cold plant extractions but also so flammable I teach that it should be considered as explosive. Can go off from static sparks or even from fluoro starters. If you must use it remember the Great Outdoors and do it there, or use a fume hood. Many people recommend storing ether in the fridge due to its low boiling point, for heaven's sake don't! The vapour slowly leaches from the best sealed bottles and accumulates in the fridge until it reaches a combustible concentration. Most domestic fridges have interior thermostats fitted, each time they switch the fridge motor on they emit a tiny spark, a sealed fridge with ether vapour inside makes a marvellous bomb!

Alchemy's a gas!

Carrying on with my safe use campaign let's look at a few gasses in common use. Some processes require leaving materials in an atmosphere of gasses other than our atmospheric mixture, let's have a look at a few and dangers associated with them.

1. OXYGEN. A gas that's highly reactive with organic substances and also a great supporter of combustion. A pure grade is normally required which would have to be purchased in a cylinder. Gasses from such cylinders are obtained via a suitable regulator, please be warned that only the correct oxygen regulator must be used with an oxygen cylinder. Remember oxygen reacts with organic substances and internal parts of general purpose regulators are usually well greased. This grease is liable to react with the oxygen turning the regulator into a mini bomb. Oxygen regulators are specifically fabricated to make use of this grease unnecessary. Still on cylinders please secure them upright in your lab, even a cycle security lock holding the thing to a table leg is enough but do not let them stand free. Those cylinders contain gas at very high pressure, if one falls over and the top's knocked off we have a rocket which randomly flies around the room. I know of cases where they've crashed right through walls . People have died after being hit by a flying gas cylinder, a simple chain and padlock will prevent such disasters.

2. HYDROGEN. This stuff's incredibly dangerous in the hands of a fool. I remember a 13 year old idiot who manufactured it in a conical flask using sulphuric acid acting on granulated zinc. He sealed his flask with a rubber stopper through which a glass tube pulled out to a fine point protruded. Lighting gas emitting from this tube he created a good clean hydrogen lamp that impressed his friends. To stop the action he removed the stopper and added lots of water before replacing it. As there was still a little effervescence he applied a lighted match to the tube....BANG! That flask vanished in a thousand fragments, he'd learned an important lesson, hydrogen/air mixtures explode. I was lucky I wasn't permanently blinded, aye that idiot was me! If you must use hydrogen make sure you are familiar with it beforehand and use a regulator specifically for it. It's useful for creating an anaerobic environment when it displaces air in a suitable sealed container after which an electric charge between two electrodes burns it off. Should you require anaerobic conditions spend money on the correct equipment, don't improvise where hydrogen is concerned.

2. INERT GASSES An anaerobic atmosphere be more safely created by using an inert gas such as Krypton, Argon, or Helium. We use Krypton as a carrying agent for gold plasmas created in the course of specimen preparation for electron microscopy. We also use it to break the vacuum in those instruments, unlike air it has no adverse effect on the metals of the microscope. I pass on one warning with regard to Helium. A favourite party trick is to inhale the gas which makes you talk like Donald Duck. Fun? Like hell! It can kill you! It only takes two deep inhalations of Helium gas to displace the air in your body, making it an anaerobic vessel. Deaths and brain damage have resulted from this silly game...don't do it.

4. CARBON DIOXIDE Easily made from the action of hydrochloric acid in marble chips. Good for certain methods of plant work and a superb anaesthetic for insects. Solid carbon dioxide, dry ice, is an excellent cooling agent and the gas released from it is an attractant to many biting insects. Once again avoid inhalation.

6. BROMINE AND CHLORINE Both are lethal! If you must use do so in a fume hood. No fume hood? Forget it, it's an agonising way to die. A shocking incident on this campus some years ago involved a highly reactive, bromine-based volatile liquid. Long term experiments by an expert worker involved filling a heavy metal cylinder with the vapourised liquid while the trial was done. The guy was very safety conscious and knew the risks of a mistake, alas fate caught up with even him. At the end of the experiment the volatile fluid was forced back into its container by pumping an inert gas into the chamber. Gas continued to purge any residues out prior to the cylinder being opened, unfortunately this time traces of the reagent remained. Although minute they were enough to destroy the scientist and his laboratory. Moral, when using dangerous techniques make sure you are totally alert at all times.

7. VOLATILE SOLIDS. Remember that many solid chemicals can sublimate to emit dangerous gasses. Potassium cyanide is a good example playing an important role in extracting some metals including gold. It also emits very toxic fumes that kill in low quantities by preventing the haemoglobin in the red blood cells taking up oxygen. Some isotopes of Uranium, plutonium, and other radioactive elements emit radioactive gasses such as Radon, Don't play with radioactivity unless you are fully trained in associated safety, handling, and storage techniques.

8. VOLATILE LIQUIDS We've mentioned ether and mercury in a previous mailing. Carbon disulphide and hydrogen sulphide emit dangerous fumes and are also quite explosive, steer clear. If you smoke don't do so when working with chloroform, this reagent is not inflammable but its vapour passing through the hot tip of a cigarette is converted to phosgene a good old military killer gas. Ammonia is yet another liquid that must be used in a fume hood, it has most unpleasant fumes. Many acids including sulphuric, and nitric have corrosive fumes, yet again avoid inhalation.

9. PLASMAS The alchemist's dream! Highly charged elemental masses , neither solid nor liquid, sort of like a cloud made of solids. As mentioned above I use gold plasmas with low charges in some of my work. Instructions are around on how to create high energy plasma balls, once again don't do it! A pretty cluey amateur in this area built a special magnetic retaining chamber in which he created a plasma ball using very high voltage. Idea was it would be held safely in the magnetic fields, supplying energy for his main project. Alas it was all too much for the fields and the thing broke down. Suddenly X found he'd released the genii from its bottle and it drifted round his lab as a perfect shimmering sphere. Veritable ball lightning created in the lab, all he wanted to do was get out. He was lucky, the thing contacted his fridge and discharged its energy with a great bang, the fridge was totally demolished. Moral? It's not only within magic circles that demons are generated. Many things are far too dangerous to play around with.

More advice on laboratory safe practice.

READ THE LABEL!

Many's the worker who has come to grief through not fully reading the label on jar or bottle containing the required reagent. No matter how well you may think you know a chemical give that label a close scrutiny before you use the thing.

If details on the label are scant you have very old stock and old chemicals lose their potency. Unless you are playing with stuff in a decayed state follow the second great maxim on those ancient Enochian pillars....'WHEN IN DOUBT, CHUCK IT OUT!' Down the sink in most cases with lashings of cold water.

Poisons should have a label stating this with advice to read safety instructions before opening. DO SO! Nowadays other warning signs are appended to containers based on international standards. If the product requires a warning it will be contained within a diamond symbol which states what hazards attend its use. A small drawing illustrates what the hazard is and a number at the base of the diamond indicates which schedule the chemical is listed under.

Details of schedules should be available in any good chemical catalogue, generally speaking the higher this number the greater the risk. Chemicals can, among other things, be flammable, explosive, corrosive, toxic, radioactive, reactive, or carcinogenic. If you are unfamiliar with the meanings and implications of any of those terms you shouldn't really be handling them at all!

Safety directions should always be appended if a reagent is hazardous. READ THEM THOROUGHLY! Finally details of first aid treatment are frequently given, envisage an accident involving the chemical and run through in your own mind how you could handle this. If you can't envisage things applied alchemy is not for you.

The chemical formula should appear on the label followed by a number. e.g. the title Potassium Hydroxide would have below it....KOH=56.11. This number is the molecular weight of the compound, useful information when you need to make up molar solutions. (Saves a lot of calculations).

Chemical suppliers should also have Material Safety Data Sheets (MSDS) available on their products. Whenever you order reagents insist on a copy of the latest for the items required. Build up a file of those and keep referring to them.

Reagents come in a range of grades actual names of which can vary from one manufacturer to another, check relevant catalogue. Generally ANALAR products are not only the purest available but also the most expensive. A list of impurities and their proportions should appear on every label.

As a good example of how important reading labels is let me narrate an experience I had last year. In our storage area I noticed a strong, unpleasant, sulphidey smell which I tracked down to a single sealed jar from which the fumes were leaking. I was anxious to check the contents but fortunately checked the label first. On this was an explosive symbol with a warning that merely unscrewing the top could cause enough friction to set things off! Further details warned that the slightest jolt could do the same. The material was badly decayed and the label also informed me that fumes released were potentially toxic. This material had not even been placed in a fume hood!

Who dumped it there? Uni labs are places of mystery but I suspect it was a fool who'd done work on blowfly attractants. Guess who ended up walking carefully across a crowded campus taking this to a safe storage area? On that day of all days the place was full of morons with back to front baseball caps blundering dumbly around.

Did I survive? I'll tell you one day.

And so to Equipment

We have a great advantage over our predecessors of old as a wide range of excellent equipment is now available to us. Glass and ceramic ware, for example, is made to much higher standards and thus contains fewer impurities. An advantage? I wonder what role those impurities played in the achievements of some of those predecessors ?

First thing to do is find a reputable supplier. Those of you in the U.S. and Canada can contact firms like Cole-Parmer Instrument Company toll free on (800) 323-4340...(no I don't get a commission) requesting their latest catalogue. Such catalogues are excellent guides as to what is available and will help plan your work, get them from as many firms as you can...chemicals. glassware, general equipment.

A good source of equipment can be local auction rooms, check the papers as there are bargains around.

A few quick words now on glassware.

Alembics, pelicans, and retorts are now obsolete with Pyrex products even appearing in Frankenstein movies. Use only good quality glassware such as Pyrex which is heat resistant and less liable to crack when heat is applied. Unbranded soda glass junk used in elementary school chemistry classes must be avoided like the plague. Soda glass tubing is however preferable to Pyrex as it melts at lower temperatures and is thus more easily used in glass blowing work.

Clean all glassware before its first use with a lab grade detergent such as DECON 90. If bottles have ground glass stoppers ensure that bottle and stopper are kept together during washing. Such stoppers are ground to fit in the necks of specific bottles, mix them and you'll be ages finding what goes where. While on ground glass stoppers never put potassium or sodium hydroxide solutions in bottles having those. It doesn't take long for the stopper to fuse with the bottle neck, it may never open again! Under normal circumstances ground glass stoppers jammed in a bottle may be eased by GENTLY tapping the stopper. Belt it and you'll break the neck. Once you've put a solution into a container label it immediately with details of solution and date of manufacture. If hazardous give details as well. Always write out details in full, never use just a formula e.g. Potassium Hydroxide, never KOH. You know what it means someone else coming in contact with the stuff may not.

Good quality glassware comes in several grades always go for the best you can afford. This is particularly important with measuring beakers, pipettes, burettes, and cylinders, cheaper stuff will be a lot less accurate.

Some form of still is essential but ensure you are given full instructions by the supplier as to its use. A local dealer is an asset here as a rep can come round to do this.

A reflux condenser is useful for doing extractions in alcohol etc. Material is placed with solvent in a round flask with a ground glass top, a special condenser fits vertically into this making a tight seal, water runs through the outer jacket of the condenser as usual. Alcohol evaporates into the condenser, condenses (surprise) and falls back down into the flask. Extraction can be done over long periods with minimal loss of reagent but remember my warnings about heating.

Stem mercury thermometers are useful adjuncts but do not trust them as bought, they can frequently be a couple of degrees out. Calibration is a cinch, immerse thermometer in boiling water and ensure the mercury column stops exactly on 100 °C, if it doesn't make a mark with a fine pointed pen where the column is located at this temperature.

Now fill a container with a mixture of crushed ice and salt and insert the same thermometer, having allowed it to cool to ambient. Column should now stop at 0 °C if not mark scale again to show actual reading. Those marks can now be made more permanent with a diamond pencil and allowance made for any variation in subsequent readings. e.g. thermometer is actually 2° below the 100° standard, therefore if you require 60 °C you'll have to let column rise to 62°.Lab workers at our local oil refinery have found a great variation in thermometers used in their work, I pass this info from them.