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PERCHLORIC ACID

Written January 2007

Perchloric acid (ClHO4) is a strong corrosive mineral acid. It is a colourless, odourless, oily liquid that is very hygroscopic (i.e., it absorbs moisture from the air). It is an oxidizing agent. At high concentrations or when it comes in contact with organic or combustible material, it presents an explosion hazard. The purpose of this safety notice is to provide information on the safe handling and storage of perchloric acid. PERCHLORIC ACID CONCENTRATIONS UP TO 72.5% In concentrations up to 72.5% and when used at room temperature, ClHO4 is normally stable. Precautions for using perchloric acid under these conditions are similar to those for other mineral acids: Wear suitable gloves, chemical splash and impact goggles, and other protective clothing to protect in the event of splashes and spills. Dilute only by adding perchloric acid slowly to water while stirring, not the other way around. Limit quantities in storage to what is needed for the next 6-12 months. Perform all work involving evaporation of perchloric acid inside a perchloric acid fumehood with the sash down. This is a specially designed fumehood that has a wash down system that will prevent the build-up of explosive perchlorates in the ductwork. Do not store organic materials near perchloric acid. Do not allow perchloric acid to come into contact with strong dehydrating agents (e.g., concentrated sulphuric acid, anhydrous phosphorous pentoxide, etc.). Handle the smallest quantities of perchloric acid possible for the task at hand.

PERCHLORIC ACID CONCENTRATIONS AT OR ABOVE 72.5% At concentrations equal to or above 72.5%, ClHO4 is often referred to as anhydrous perchloric acid. Anhydrous perchloric acid is a powerful oxidizing agent. It is unstable and dangerously reactive, capable of decomposing explosively while standing or when subjected to shock. It will also react vigorously with water, evolving heat very rapidly. Because of these properties, anhydrous perchloric acid should not be used without proper authorization from DOHS. Note that perchloric acid does not become anhydrous in storage because of the azeotrope formed with water at a concentration of 72.5%. Perchloric acid should not be mixed or used with organic materials if there is a possibility that temperatures will become elevated beyond ambient levels. Perchloric acid digestions and other uses at elevated temperatures require that the procedures be conducted in a perchloric acid fume hood (as defined earlier).

If work with anhydrous perchloric acid is absolutely necessary and has been authorized, as noted above, the following precautions MUST be observed: Only experienced researchers may work with anhydrous perchloric acid and must be thoroughly familiar with the literature on this acid. Work with anhydrous perchloric acid must never be done alone. A second person must always be in view at all times and must be trained to perform rescue should the need arise. A safety shield must be used to protect against a possible explosion and the work must be done in a specifically designed fumehood, as noted above. Chemical splash and impact goggles, a face shield, protective gloves, and a rubber apron MUST be worn at all times while handling this acid. Contact the chemical supplier for further information. Only freshly prepared acid should be used and only the absolute minimum quantity required for the work should be prepared. Dispose of any unused anhydrous perchloric acid at the end of the work via dilution and neutralization (see procedure for a small spill, below). Prevent all contact of this acid with organic materials, as an explosion will occur. If the anhydrous perchloric acid appears discoloured, it must be disposed of immediately, via the method indicated below.

SPILLS AND OTHER EMERGENCIES Restrict access to the location of the spill. The spilled material should not be mopped up nor should dry combustibles (e.g., paper towels, etc.) be used to soak up the acid. Contact DOHS immediately for consultative assistance to make sure perchloric acid spills are handled properly. Small Spill: Neutralize slowly with soda ash (Na2CO3) or other appropriate neutralizing agent. Transfer the slurry to a container of water for disposal. Water may then be used to thoroughly wash the affected area. This wash water can be flushed down the laboratory sink or sewer with additional fresh water. Do NOT use rags, paper towels, or sawdust and then put them aside to dry out, as such materials may spontaneously ignite. Likewise, spills on wood may present a fire hazard after the liquid dries. Large Spill: Contact supplier and emergency services (e.g., fire department, DOHS, etc.) for advice. STORAGE OF PERCHLORIC ACID Perchloric acid at concentrations less than 85% should be stored separately from other chemicals if possible. If it is not feasible to do this, store the solution with other inorganic acids and away from organic chemicals and materials. The containers should have secondary containment, such as a glass or porcelain tray, in the event of spills. Refrigeration provides no additional safety benefits.

Perchloric acid at concentrations above 85% should not be stored in any quantity. Dispose of any unused solutions at the end of the day via dilution and neutralization. Discolouration: Discard the material if a bottle containing perchloric acid has turned dark. Crystal Formation: If crystals have formed around the bottom of the bottle, there is a potential explosion hazard. Do NOT move the bottle, but contact DOHS or Security Services (ext. 33333) for immediate assistance. If white crystals have formed around the neck and cap of the bottle, these are almost always an ammonium salt. This may be washed off the bottle with water and the rinsate disposed of down the drain with plenty of fresh water. FUMEHOODS CONTAMINATED WITH PERCHLORIC ACID If you know that a regular fumehood (i.e., one that is not designed specifically for work with perchloric acid) has been used when heating perchloric acid, contact DOHS. For other questions and consultative assistance with respect to perchloric acid, contact DOHS at extension 55491. REFERENCES 1. 2. 3. 4. 5. 6. Canadian Centre for Occupational Health and Safety, Cheminfo database. Furr, A. Keith. CRC Handbook of Laboratory Safety, 4th Edition. CRC Press LLC, 1995. Auburn University, Risk Management and Safety website. University of Illinois at Urbana-Champaign, Division of Research Safety website. L.J. DiBerardinis et al. Guidelines for Laboratory Design, Health and Safety Considerations, Third Edition, John Wiley and son, New York, 2001. Prudent Practices in the Laboratory, Handling and disposal of chemicals, National Research Council, Seventh Edition, National Academy of Sciences, 2006.