LABORATORY SPECIFIC STANDARD OPERATING …



SOP for: (check one) FORMCHECKBOX Process FORMCHECKBOX Hazardous Chemical FORMCHECKBOX Hazard Class of Chemicals Name of Procedure: Weighing and Working with Raney NickelApplies to Lab (name): Chamberland Research GroupSCI Room #: 313Prepared By: James Siegenthaler, Stephen ChamberlandDate: 9/6/12Revision: 9/11/12Special Notifications:Raney nickel is a pyrophoric solid used for chemoselective reduction reactions. Do not allow Raney nickel to dry out because it becomes pyrophoric when dry. Raney Nickel is classified as a 2B carcinogen.Hazard Description:Hazardous in case of skin contact, eye contact, ingestion or inhalation. The material is pyrophoric, meaning that it may ignite spontaneously when exposed to air. It may also become extremely hot. It is a strong reducing agent and reacts strongly with oxidizing agents. Protective Equipment:Fire-retardant lab coatProtective wrap-around gogglesFull-face shield Chemically resistant nitrile glovesFor large quantities, heavy, chemical-resistant gloves are requiredFor large quantities, a chemical resistant apron worn over the lab coat is required.Engineering Controls:Never allow the Raney nickel to dry out, for that is when it is most hazardous. Handling it wet does not allow precise measurement of the actual weight used. After readying the Raney nickel for the reaction, use it only in a chemical fume hood with the fume hood sash maintained as low as possible. Ensure adequate ventilation to prevent inhalation and dust from collecting. Have a ‘Class D’ fire extinguisher nearby in case of a fire. Clear a path to the safety shower so that the travel time is no more than 10 seconds.Special Handling or Storage Requirements: Keep away from heat and any source of ignition. Raney nickel must be stored as a slurry in water in a cool well-ventilated area. Do not allow it to dry out completely.Spill Response Procedure:For a small spill, exert extreme caution because of the potential for spontaneous combustion. Call for a coworker to provide back up, and place a fire extinguisher nearby. Carefully remove nearby flammable materials and smother the spill area with powdered lime or dry sand. Quench by slowly adding isopropanol and place the spill residue in a double spill bag for hazardous waste pickup. If necessary, call 911 for assistance.For a large spill exert extreme caution because of the potential for spontaneous combustion. Evacuate the spill area and call 911 for emergency assistance. Immediately notify the PI (Dr. Chamberland) and EH&S.If anyone is on fire, guide them immediately to the chemical safety shower and douse them with copious amounts of water.Decontamination/Waste Disposal:If spilled on any body part, wash with water for at least 15 minutes and seek immediate medical attention. Large quantities of solid chemicals should be disposed of as hazardous waste in the aqueous waste container.Quenching disposal:Raney nickel catalysts can be slurried into water; dilute hydrochloric acid is added carefully until the entire solid dissolves. Next carefully neutralize with a sodium hydroxide solution. The waste can now be discarded down the drain.Special Emergency Procedures: See Decontamination/Waste DisposalProcedure may be performed after normal working hours (M-F, 8-5)?Yes FORMCHECKBOX No FORMCHECKBOX Procedure may be left unattended?Yes FORMCHECKBOX No FORMCHECKBOX Step by Step Procedure:When handling, ensure that all PPE is being worn, that lab safety devices are in place, and that Raney nickel is not allowed to dry out completely. With the cap on the plastic jar, shake up the slurry of Raney nickel. Use a pipet to draw up some of the Raney nickel slurry and add it to a test tube filled with the reaction solvent. Estimate the amount of Raney nickel needed based on the size of the reaction. Most procedures will approximate the amount utilized.If water is to be excluded from the reaction, first remove almost all the water from the test tube containing the slurry of Raney nickel. Then add a few mL of the reaction solvent and agitate the suspension. Many Raney nickel reductions are conducted in water-miscible solvents like MeOH or THF, so one layer of liquid should result. Allow the solid to settle, and then remove the supernatant liquid above the solid using a pipet. Repeat this rinsing with the reaction solvent 2-3 more times to ensure that most of the water is removed. Suspend the Raney nickel one more time with a few mL of the reaction solvent. Agitate the suspension, draw it up into a pipet, and then add it to the reaction flask as slowly as needed. Raney nickel is magnetic and will adhere to the Teflon stir bar if the reaction mixture is stirred too slowly. So use rapid stirring. When Raney nickel is removed from the reaction by filtration through a cotton plug or frit, always have a squirt bottle of DI H2O on hand to continuously wet the Raney nickel to prevent spontaneous fires as it dries out.When handling the Raney nickel, never allow it to dry out, always have a bucket of DI water near by to douse or wet it if need be.Approved By (PI) : Stephen Chamberland, Ph.D.Date: 9/17/12PI Signature: ___________________________________________________Date: ______________EH&S Signature: ________________________________________________Date: ______________ ................
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