Suppliers of Anhydrous Ethyl Ether
I believe diethyl ether in the market almost always goes about 99+%. ACS grade usually about >99.8% with minuscule amount of stabilizing agent such as BHT. Without stabilizers, you're more likely to form peroxides which will be explosive. Supposedly, in Europe, you can buy it OTC (although not as pure.)
You will find it extremely difficult if not impossible, as a private individual, to buy diethyl ether in most Western countries due to its increasing use in illicit drug manufacture. In most countries the authorities have massively restricted the general public's access to ether. Bona fide institutions such as universities and research institutes plus established fuel manufacturers can still obtain it, but it is highly unlikely the latter will on sell to individuals. Unless you have a contact within the university, research or an industry user, I do not think it likely you will be able to readily obtain ether-at any price.
You could check these threads:
Common Sources of Chemicals Listed by The Society for Amateur Scientists
Sources of Supplies for Citizen Chemist
"I don't know if Artchemicals.com will sell to you without a business license, but they have the smallest quantitities (i.e., 50ml) of ether available that I've seen listed anywhere."
You could make it yourself...
(NOTE: This, like many other chemistry experimentals, can be dangerous. The nature of both Diethyl ether, and Sulfuric acid are potential hazards to your safety. Don't attempt this without the proper safety measures in place! Be ready in the case of fire or toxic spill.)
Get you some 100% Ethanol solution or as close as possible anyways...(Denatured alcohol works fine unless u need super purity), and concentrated Sulfuric acid (at least 90%). Both can be found at your local hardware store or chemical supply house -- Ethanol as denatured alcohol and Sulfuric acid as drain cleaner.
You also need, for this experiment:
1 sealable glass vessel (glass bottle, for instance - preferably clear)
1 vessel for use as an ice-bath.
Ice
Water
Thermometer (optional)
Experimental:
1. Fill the larger vessel with a good amount of ice, and add some water. This is your ice-bath.
2. Place the sealable bottle into the ice-bath.
3. Add an amount of Ethanol into Vessel 1.
4. SLOWLY add drops of Sulfuric acid to Vessel 1. Add a few drops, and seal the container. Shake, repeat. Note that this reaction is exothermic and generates a good amount of heat. This is what the ice-bath is for. The reaction temperature should stay below 34.6C, and MUST stay below 130C -- otherwise Ethylene will be formed, not Diethyl ether. Generally if the acid is dripped in slowly enough, and enough ice-water is present to keep the reaction cool, this is not a problem.
-Make sure that after each addition, the bottle is re-sealed while it is cooling again. The boiling point of Diethyl ether is 34.6C (94.28F), and we don't want to lose our ether to the atmosphere.
5. When the reaction is complete, distill the contents of the cool, sealed vessel to a temperature between 35C and 78.4C (BP of Ethanol) over a spark-free electric hot plate. Or, as a safer alternative one may use hot water to distill the mixture. Utmost care must be taken not to generate any sparks/friction during this distillation - as Diethyl ether is very flammable. Collect the ether from the product vessel.
Your ether should be of high purity, with any traces of other chemicals likely being small amounts of Ethanol - that risk increasing the higher the distillation temp was. Sulfuric acid's boiling point is 290C so it is not likely that any should remain in the final product.
It would likely be hard to separate the Ethanol and Sulfuric acid since Ethanol forms an azeotrope with water at 95% conc. or so, and Sulfuric acid needs a small amount of water to prevent fuming.
One more note: If Denatured alcohol is used, it is possible that a small amount of Di-m-ethyl ether (up to 4%) will be formed as well. However, this substance is a gas at room temperature and thus should evaporate quite readily.
SAFETY NOTES:
1. Have Sodium bicarbonate (Baking soda) on hand in case any Sulfuric acid spills. In the case any spills onto the skin, pour an excess of Sodium bicarbonate on the area immediately, THEN wash the area with water, then soap. Rinse off, and dry thoroughly. Concentrated Sulfuric acid reacts violently with water and that is a reaction you don't want on your skin.
2. Have a fire extinguisher, or at least some water, on hand in the event of a fire (which is very possible in this experiment.)
3. A gas mask or fume hood is recommended but not required. Diethyl ether is not toxic in small amounts but is intoxicating. Sulfuric acid is toxic but is not likely to become a gas during this reaction. Basically the best advice is to not breathe any fumes from a chemical reaction (ever.)
This is the key: never distill to dryness!. That way any peroxides in the pot never get hot enough to explode. Also remember that dry peroxides can be detonated by friction as a localized high temperature is produced that way.
As for keeping your ether safe, and peroxide free, anything with an hydroxide ion can inhibit peroxide formation. NaOH, KOH, CaOH etc. Just throw a bit in the bottom of the bottle, and shake it up real good, then filter.
HERE'S A MORE THOROUGH DISCUSSION OF THE METHOD:
Ether is a very useful organic solvent that has fallen into ill repute because of its use by drug dealers. It is a watched chemical by the DEA, purchasing large quantities will put you on The List. Ether is an explosively flammable liquid that will easily fill a room with fumes just waiting to be ignited by the slightest heat, it ignites over 180 °C. Keep containers of ether tightly closed and away from all flame sources. Ether used to be an anesthetic back in the days, inhaling the fumes will cause unconsciousness, but not much damage if you get to fresh air. Ether can also form an explosive peroxide if it is old or exposed to air. In short, keep ether away from all flame, in a well ventilated area, and tightly sealed in its container. You might think that ether and water do not mix, wrong, ether can hold up to 1.2% water. The only OTC source of ether is in starting fluid for cars, among other contaminants, from which it can be distilled. Ether can easily be prepared by reacting ethyl alcohol with sulfuric acid.
Synthesis: Assemble the necessary equipment for fractional distillation, adding in a Clasien adapter. Place the fractionating column on the side arm of the Clasien, and a 2-holed rubber stopper in the straight arm. In the first hole, place a thermometer that extends to near the bottom of the reaction flask. In the second hole, place a length of glass tubing that extends to near the bottom and sticks up about an inch. Place a short length of rubber tubing on the glass tubing and connect it to an addition funnel. The rubber tubing is to slightly offset the funnel which would get in the way of the thermometer. If using a 500-mL reaction flask, add 146 mL of anhydrous ethyl alcohol. You can use 95% alcohol but the efficiency of the reaction will suffer because of the water. Slowly add 133 mL of anhydrous sulfuric acid, again you can use less than 100%, but the more water there is the worse the reaction will proceed. Place a magnetic spin bar in the flask and connect it to the rest of the apparatus. Using a hotplate or oil bath, no flame, heat the reaction flask, while stirring, to between 130-140 °C and hold it at that temperature. Be sure not to go in excess of 150 °C as ethylene gas will be produced. Once some distillate starts to come over, slowly add an additional 146 mL of ethyl alcohol from the addition funnel at the same rate as is collected from the distillation. That should be about a drop or two a second. The total distillation time should be over 2 hours. After the distillation is over, pour the distillate from the receiver flask to a large beaker and add 10% sodium hydroxide solution until the pH is neutral. Pour this mixture into a seperatory funnel and allow the lighter ether layer to float on top. Remove the heavier water layer and wash the remaining ether by shaking twice with a volume of saturated salt water equal to the volume of ether. Allow the last wash to sit for several minutes to insure complete separation then remove the water layer. Put the ether in a Florence flask and add 15 g of calcium chloride for every 100 mL of ether, stir this for 2 hours with a magnetic stirrer. Finally, do a simple distillation to remove the now anhydrous ether from the calcium chloride.
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OTC Ether
For those who don't care to synthesize ether, there is a readily available source in the automotive section of your local department store. Most people know it as starting fluid. The main component is diethyl ether. The current leading K-mart brand contains heptane(bp 98°), dimethyl propyl methane (2-methyl pentane, bp 60°), and diethyl methyl methane (3-methyl pentane, bp 63°) as added ingredients. The other ingredients all boil significantly higher than ether so the ether can be removed by distillation. To collect the ether for distillation, spray the contents of the can into a flask that is nestled in crushed ice (in a well ventilated area or outside). Once can use one of the "straws" that comes with a can of WD-40 to spray the starting fluid contents well into the flask. Distill the liquid collecting the portion boiling up to 35°C.
Here's one person's report of distilling ether from starter fluid:
I distilled some ether from starting fluid today, with good results. Two cans were emptied into a 1 L Erlenmeyer flask, coming to a volume of around 800-900 mL. The flask was sealed with a rubber stopper, and the rubber stopper was linked by plastic hose to a condenser. The condenser consisted of a copper coil inside a 3" diameter piece of PVC pipe filled with regular ice. I didn't feel like buying 5 pounds of dry ice for $5, when the same $5 bought me 35 pounds of regular ice. I didn't use it all however, only about 10 pounds or so for both cooling the receiving flask and the condenser. The flask was heated on an oil bath at 50-60 C for 4 hours at which point bubbles stopped forming. 150-200 mL of distillate was obtained, which made me a little dizzy when I caught a whiff. The operation appears to be a success. 200 mL of ether for a grand total of $2.50 isn't bad! I will proceed to dry it with calcium chloride later, but even now it appears to be quite pure.
Additional recommendations:
Add a piece of copper wire to the flask where you store the ether in, this prevents peroxide formation. This does not destroy already formed peroxides though. To destroy peroxides re-distill but add a dash of ferrous sulfate before starting the distillation.
So you have now 200ml of ether. A easy way to get it pure is to collect about 10ml at start of the distillation change receiving flask, collect about 150ml and change back again. The 150ml "middle fraction" resembles the pure stuff.
Usual ice/water mixture is absolutely ok for condensing ether. Don't forget to cool your receiving vessel and put the copper wire in from start.
Dry your product with lots of NaOH - this takes some weeks (yes weeks) but is the only way to get the ether dry.
Store in a dark (brown) bottle away from air and at a cool place.
