#6 Spill and Accident Procedures

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1 Standard Operating Procedure (SOP) for filling 4L (1 gl) canisters with 1% Hydrofluoric (HF) and 1% Nitric (HNO3) acid mixture for use in the Ultrasonic bath #1 General Process Description This SOP describes the filling of the 2/4L (0.5/1gl) canisters with low concentrated 1% HF and 1% HNO3 acid mixture. The canisters are then filled with the sample and used for etching/cleaning your quartz sample in the Ultrasonic bath. Preparing the acid mixture is described in the SOP for preparing a 20L (5gl) 1% Hydrofluoric (HF) and 1% Nitric (HNO3) acid mixture for use in canisters in the Ultrasonic bath. All work described in this SOP will have to be conducted in Mitchell A20. Contact Principal Investigator (PI): Prof. George E. Hilley for more information (hilley@pangea.stanford.edu or (650) ). This SOP is from 05/04/2007. #2 Hazardous Chemicals/Class of Hazardous Chemicals We are not using concentrated acids in this SOP, but rely on a low concentrated (1%) mixture of HF and HNO3. However, all equipment that came into contact with the low-concentrated acid mixture must be wiped and rinsed off. All wipes are hazardous waste and belong into the hazardous waste container near the 55gl drum. #3 Personal Protective Equipment (PPE) Before any acid is handled, ensure that you will at least meet the following protective requirements: 1. goggles (prescription glasses are not enough!) 2. double glove - neoprene 3. closed-toe shoes with socks 4. long pants (no shorts!) 5. lab coat 6. face shield 7. neoprene apron 8. small Chemical Spill Kit

2 All Material Safety Data Sheets (MSDS) are located in the red folder in the storage cabinet opposite of the dishwasher under the vertical laminar flow unit. Ensure the Calcium Gluconate is not expired and is available in the event of an exposure. The Calcium Gluconate is stored below the sink right next to the entrance door and in the closet above the sink right next to the entrance door. #4 Engineering / Ventilation Controls All work for filling the 4L canisters has to be done in the fume hood with the protective shield drawn down as much as possible, but allowing to work comfortable. Make sure that you place the 20L canister that you use for filling the 4L canisters far enough inside the fume hood. The ultrasonic unit is in a sound-proofed room and should only be run with the door closed. #5 Special Handling Procedures and Storage Requirements Store the 20L canister in its appropriate space near the oven and telephone. Ensure that the 20L canister is in its secondary containment. Do not store any low concentrated HF/HNO3 acid mixture in glass, metal, and ceramic containers, as they are not compatible with HF. Place a secondary containment tray in the fumehood, when you are filling and handling 4L canisters. In case you overfill or spill acids, it will stay in this secondary containment. Also, the 20L acid mixture bottle will stay always in its secondary containment, unless it is being used for filling the 4L canisters. Transport the 20L acid mixture only on the cart and only in its secondary containment tray. Place the 1% acid mixture in its secondary containment at its dedicated space on the cart. No rinseates with ph below 5.5 may be drain disposed. Please review the last page for emergency contact and notifications. #6 Spill and Accident Procedures 2

3 If you spill acid and the spill is an immediate threat to your health, call Remain nearby. In the event of an HF exposure, follow Stanford University Hydrofluoric Acid First Aid Instructions posted in Mitchell A20. If you accidentally spilled the low concentrated acid mixture (HF/HNO3) (e.g., while filling the 4L canisters): Don t panic! Remain calm. If the spill is small (less than a few ml up to 30mL), place a pads from small spill kit over the spill. Find a plastic/neoprene-disposal bag in the shelf above the scales and carefully place the soaked pads into the bag, and place in container provided with kit. To minimize contact with HF during clean-up, use Teflon tongs to move the soaked pads into the bag. All of this must be done in the fumehood. If the spill is significant larger (> 0.5L) use the yellow spillcontainment pads under the sink by the door. Place them over the spill. Call If spill is greater than 30 ml, or cleanup takes longer than 15 minutes, document the cleanup activity either by calling EH&S at or by notating the lab inspection forms. If you have spilled parts of the 1% acid mixture, carefully wipe it off with small spill kit pads or soak it up with the yellow spillcontainment pads. Rinse the area with plenty of water, collect rinseate, and wipe off afterwards. To confirm that cleanup is complete, wipe area with moistened ph paper. #7 Waste Disposal If you ve spilled acid and soaked up acid containment bags, make sure they are in disposable neoprene bags placed into the container provided by EH&S These containers will be labeled with an EH&S label and disposed separately. #8 Training requirements Prior to entering and working in the laboratory, you must have completed the EHS-4200 General Safety Training and EHS-1900 Chemical Lab Safety. You will have to retain training documentation for at least one year. 3

4 Any person conducting work in Mitchell A20 using this SOP must receive training on the contents of this SOP. #9 Approval Required All research staff must get initial PI approval prior to starting work with Hydrofluoric Acid. Under no circumstances it is allowed to work with concentrated HF, while being alone in the laboratory. Always ask a second person to be in the lab with you. If you have to work with concentrated HF and you are alone, you have to ask for approval from the PI, Prof. George E. Hilley. #10 Decontamination All glassware and measuring cylinders that have been used during the process should be thoroughly rinsed with DI water (3 times) and then with Millipore water (1 time). Collect first rinseate as hazardous waste. #11 Designated Area Filling of the 4L canisters with HF and HNO3 should only be done in the fumehood in a secondary containment tray. Upon leaving a designated work area, remove any personal protective equipment worn and wash hands, forearms, face, and neck. After each use (or day), wipe down the immediate work area and equipment to prevent accumulation of chemical residue. At the end of each project, thoroughly decontaminate the designated area before resuming normal laboratory work in the area. 4

5 #12 Precise Process Description 1. Verify that emergency eyewash/shower is accessible and tested within last month. 2. Verify that fume hoods are currently certified. 3. Check the location and expiration of the Calcium Gluconate and that a copy of the MSDS for HF is available 4. Ensure that the spigot of the 20L carboy is tightly screwed on and that the carboy is emptied completely. 5. Check the integrity of all containers and any connections prior to any filling. 6. During the entire process, carefully survey benchtop and floor area for any drips form the hose. Clean up spills immediately. 7. Check if all 4L canister are properly labeled and no label has been wiped off. Especially, the 1% Hydrofluoric Acid, 1% Nitric Acid, unique canister number must be clearly readable. 8. Check if the 4L canisters you intend to use are clean, healthy, and do not show any signs of cracking. If you push in the outside wall of a canister with your hands and the canister shows cracks, it is time to replace this canister. 9. It is essential that you wear a face shield over your safety glasses, double neoprene gloves, and the neoprene aprons to ensure proper protection for concentrated acid spills. 10. FUMEHOOD: Take the 20L carboy from its large, secondary containment tray and put it on the elevated surface. 11. FUMEHOOD: Place a medium, secondary containment tray in the fume hood below the 4L canister that will be filled with the low-concentrated acid mixture. 12. FUMEHOOD: Fill the 4L canister up to its 4L mark. 5

6 13. FUMEHOOD: After filling the 4L canisters, close the carboy and ensure that all spigots are closed. When the 20L carboy is empty, it is ready to be filled with a 1% HF/HNO3 acid mixture, following the SOP for preparing a 20L (5gl) 1% Hydrofluoric (HF) and 1% Nitric (HNO3) acid mixture for use in canisters in the Ultrasonic bath. 14. FUMEHOOD: Transfer the sample into the filled 4L canisters while they are still in the fume hood. Use a plastic spoon or a pyrex beaker with pre-weighted sample material. You can use 7.5g sample for 1L 1%HF/HNO3 solution for the first ultrasonic-bath run. That is ~30g for 4L 1% HF/HNO3. For the second and third ultrasonic-bath run, you can use 10-15g sample material for 1L 1% HF/HNO3 (~60g for 4L 1%HF/HNO3). 15. FUMEHOOD: Close the lid of the 4L canister tightly. 16. Once you have filled all 4L canisters with your sample material, ensure all lids are tightly closed. Open the door to the ultrasonic bath and place the canister into the cold ultrasonic bath one at a time. 17. Place all the canisters into the bath. You can put up to 8 4L canisters and 3 2L canisters into the ultrasonic bath. If you don t need all 8x4L and 3x2Lcanisters, you still have to put 8+3 canisters into the bath to ensure they are not sliding around. You can fill the remaining canisters without sample material with DI water. 18. Once all the canisters are in the ultrasonic bath, check the water level. Fill in DI water up to ~4cm (~1.5 inches) from the top of the bath. The exact amount is not really important, however, ensure that there is enough water in the bath to cover the bottom of the canisters. Never run the Ultrasonic bath without water, as it will shorten the lifetime of the unit. 19. Turn on the heat for the ultrasonic bath. It is automatically set to 70 C and it will take about 1hr to warm up the bath. 6

7 20. If needed, set the timer to the left of the bath. You run the ultrasonic bath and heater for 10 hours. 21. Turn on the ultrasonic unit and close the door. 22. Place the 20L carboy and its secondary containment tray onto the cart and move it back to its dedicated position. 7

8 Laboratory Spill Response Procedures Health Threatening Situation - In the event of an imminent or actual health-threatening emergency (threatening local or public health, safety, or welfare; or the environment outside the immediate area): 1) CALL FOR THE FIRE DEPARTMENT REMAIN IN THE AREA TO ADVISE RESPONDERS. 2) ACTIVATE LOCAL ALARM SYSTEMS 3) Once personal safety is established, call EH&S at and proceed with local notifications, below. Non-Health Threatening Situation In the event of a spill or release which may or has impacted the environment (storm drain, soil, air outside the building) or spill or release that cannot be cleaned up by local personnel: 1) Notify Stanford Responders: call (24 hours/day, 7 days/week), then 2) Provide local notifications: Name Phone Number Cell or Pager Title George E. Hilley Principal Investigator Bodo Bookhagen (415) Lab Manager Felicia Morales Lab Safety Coordinator Local Response Situation In the event of a minor spill or release that can be cleaned up by local personnel using readily available equipment (absorbent, available from EH&S in Small Spill Kit): 1) Notify personnel in the area and restrict access. Eliminate all sources of ignition. 2) Wear gloves and protective eyewear. Clean up using absorbent. Put the contaminated absorbent in a labeled hazardous waste container. 3) If greater than 30 ml, or cleanup takes longer than 15 minutes, make a record in your lab inspection report, or call EH&S at to record the spill, and notify your supervisor. 4) Submit online waste pickup request to EH&S at: wastepickup.stanford.edu 8

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