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Standard Operating Procedure ________________________________________________________ Read the EH&S Standard Operating Procedures Fact Sheet before filling out this form. Print out the completed SOP and keep a readily accessible hard copy in the lab (also keeping an electronic copy is highly recommended). ______________________________________________________ Date: SOP Title: Using Piranha Solution for cleaning Principal Investigator: Room and Building: Lab Phone Number: Section 1 – Process A piranha is used to remove organic residues from substrates. Two different solutions are used. The most common is the acid piranha: a 3:1 mixture of concentrated sulfuric acid (H2SO4) with 30% hydrogen peroxide (H2O2). Section 2 – Hazardous Chemicals sulfuric acid (H2SO4) and 30% hydrogen peroxide (H2O2) Section 3 – Potential Hazards HIGHLY CORROSIVE STRONG OXIDIZER - May ignite flammable/combustible materials: DO NOT mix with ORGANIC solvents OVERPRESSURE EXPLOSION HAZARD – DO NOT confine while reaction continues to out-gas INHALATION HAZARD – perform work inside a fume hood Section 4 – Approvals Required Use of piranha must be approved by the Principal Investigator or Lab Safety Officer Section 5 – Designated Area Inside chemical fume hood Section 6 – Special Handling Procedures and Storage Requirements Whenever handling Piranha, only use glass containers (preferably Pyrex). Containers used during the experiment must be very clearly labeled and a warning sign, visible by any user working inside the fume hood, must be posted at all time to indicate that the solutions contains Piranha mixture. Mix the solution in the fume hood with the sash between you and the solution. Wear full personal protection, as described in Section 7. When preparing the piranha solution, always add the peroxide to the acid. The H2O2 is added immediately before the etching process because it immediately produces an exothermic reaction with gas (pressure) release. If the H2O2 concentration is at 50% or greater, an explosion could occur. Start out making small quantities, until you work out how much you need. Piranha solution is very energetic and potentially explosive. It is very likely to become hot, more than 100 degrees C. Handle with care. Substrate should be rinsed and dried before placing them in a piranha bath. Piranhas are used to remove photoresist and acetone residue, not the compounds themselves Leave the hot piranha solution in an open container until cool. Never store hot piranha solutions. Piranha stored in a closed container will build up pressure and possibly explode, spraying concentrated acid. Adding any acids or bases to piranha or spraying it with water will accelerate the reaction. This includes Photoresist, which is a strong base. Mixing hot piranha with organic compounds may cause an explosion. This includes acetone, photoresist, isopropyl alcohol, and nylon. Do not store wash bottles containing organic compounds on the piranha deck. Section 7 – Personal Protective Equipment The handling of Piranha solutions requires special protection equipment in addition to the regular clean room protection outfit The additional protective equipment include: a full face shield, heavy duty rubber gloves (disposable Nitrile gloves will not provide sufficient protection), as well as an acid apron to wear on top of the lab coat. Heavy Gloves are located in the cabinet, apron and face shield are available at ____________. As a reminder, open-toed shoes are not allowed when working in the lab and legs must be covered Section 8 – Engineering/Ventilation Controls Always work within a fume hood. Use sash to protect yourself from an accidental spraying of piranha. Make sure emergency eyewash is accessible and working properly before working with such hazardous materials. Section 9 – Spill and Accident Procedures In case of large exposure, the victim should be removed from the contaminated area, decontaminated under a safety shower while emergency personal is contacted (911). All contaminated clothing should be removed immediately with appropriate gloves and safely discarded. In case of contact with the skin, the affected area must be immediately rinsed with large amounts of water for at least 15 min. In case of contact with the eye, irrigate the eye for at least 30 minutes, keeping the eyelids apart and away from eyeballs during irrigation. Call 911, Place ice pack on eyes until reaching emergency room. In case of inhalation, it may irritate the respiratory tract. Conscious persons should be assisted to an area with fresh, uncontaminated air. Seek medical attention in the event of respiratory irritation, cough, or tightness in the chest. Symptoms may be delayed. Section 10 – Waste Disposal The primary hazard from storage of piranha etch waste is the potential for gas generation and over pressurization of the container when the solution is still hot. If you store a hot solution in a tight container, it will explode! Therefore prior to storing the piranha solution, it must be left in an open container in order to cool down for several hours (overnight). It is your responsibility to make sure that the open container is very clearly labeled and left in a safe area for overnight cool down. Once cooled down, the solution can be transferred into a loosely-capped glass container for waste storage. The container must be very clearly labeled with the solution name and composition and must include VERY VISIBLE warning signs not to add any other types of chemicals. Keep waste bottles loosely caped or use a vented cap. Verify there is no pressure before picked up for disposal through EH&S. Section 11 - Decontamination Rinse contaminated beakers and glassware with lots of water. Carefully pour the piranha solution into the piranha waste beaker in the piranha hood. Section 12 – Process Steps Process Steps 1. Place chips on glass slide (~ 4 chips for 40mL) Safety Measures Put on personal protective equipment, section 7 above. Make sure eyewash is working. 2. In hood, pour 30mL H2SO4 in beaker. 3. Add 10mL H2O2 & swirl gently. 4. Take levers on slide in one hand, & using tweezers in other hand to lower levers into beaker (watch orientation – don’t smash levers on bottom) & tap tweezers between levers. 5. Let sit ~30min (room temp). Put sign up on hood. 6. Rinse tweezers in lots of water. 7. Rinse & dispose of slide. 8. Tighten H2SO4 cap, rinse bottle, dry, & put away. 9. Fill 2 1000mL beakers with ~800mL DI water and one 100mL beaker with ~100mL DI water. Pickup chip (make sure you have a good grip!) & swirl gently for ~15 seconds in each of the large beakers. Then place in smaller beaker. Exothermic reaction – hot! 10. Repeat step 9 for all chips. 11. Dry on cleaned slide. Tap gently (non lever side!) to remove water and then leave under scope with light on. 12. Check levers to see if chip is usable (all there? Cracked?). Store in dessicator. 13. Clean up: Clear out sink. Rinse the “rinse beakers” with lots of water. Carefully pour the piranha solution into the piranha waste beaker in the piranha hood. DO NOT tighten the cap! Training Documentation Name (Printed) Signature Date