Replacing Karl Fischer Reagent and Cleaning Generator Cell

Replacing Karl Fischer Reagent and Cleaning Generator Cell for the Are Revision Aquatest CMA Unit Operating Procedure # Certified by Date Page a # 3 Job Hazards Lab Yes Job Hazards Access and Egress Moving Parts Activities of Others Noise Adverse Weather Rail Movement Chemical Exposure Sharp Edges Electricity Slips, Trips, and Falls Fatigue Static Electricity Fire and Explosion Trip Injuries Ground Contamination Trapped Pressure Manual Handling Working at Height OPS-LB-NM-041 0 6/28/11 References / Documents Yes 1 of 2 PPE Use Standard (SSP-0011) q N/A Y Full Face Shield / Goggles Special Instructions q Any problems, notify Shift Supervisor or Duane Chaisson. Environmental Hood Clothing—Chemical Protection Gloves—Chemical Personal Fall Protection Respirator / Filter Mask Supplied Air q N/A Other: Quality Assurance WARNI NG CAUTION q N/A Replacing Karl Fischer Reagent and Cleaning Generator Cell for the Aquatest CMA 1 Remove generator cell leaving black plug attached and dispose of the generator solution. 2 Rinse cell with water. 3 Place cell in a small beaker of nitric acid. 4 Allow cell to sit in acid for at least one hour. 5 Rinse cell thorough with water to remove acid. 6 If necessary, remove frit from bottom of cell to clean out any pieces of septum or debris trapped between frit and ground glass fitting; reattach frit when finished. 7 Rinse cell with methanol to ensure completely dry, then set aside. 8 Remove the sensing electrode, the teflon septum cover and dessicant assembly from titration vessel and set aside. 9 Release clamp around titration vessel and remove vessel. 10 Dispose of spent pyridine reagent under hood as pyridine has very pungent odor. 11 Clean vessel with water followed by acetone and place in drying oven for 15 minutes. 12 Under hood, pour contents of Photovolt solution “A” into bottle “B”, then swirl to mix well. 13 Allow mixture to stand for about 30 minutes to mix well and cool. 14 Pour about 150 ml of mixture into dried titration vessel. NOTE: When attaching greased joints to titration vessel rotate glassware back and forth to ensure good seal. 15 q Replace dessicant and sensing electrode after applying small amount of silicone grease to ground glass joints. Procedure Completed Date: Prepared By: Approved By:

Replacing Karl Fischer Reagent and Cleaning Generator Cell for the Aquatest CMA(continued) Are Revision Unit Operating Procedure # Certified by Date Page a 3 # Lab OPS-LB-NM-041 0 6/28/11 2 of 2 Replacing Karl Fischer Reagent and Cleaning Generator Cell for the Aquatest CMA (continued) 16 Add fresh silicone grease to generator cell joint and place cell back in titration vessel. 17 Break open ampule of generator solution and using disposable pipet add entire ampule to generator cell. 18 Remove used septum from teflon holder, then clean and regrease before reattaching to titration vessel. 19 Reattach electronic plugs from generator cell and sensing electrode. 20 Turn on titrator and set stirrer speed to 4. 21 If display reads “Over Titrate” or gives error, slowly add one drop at a time of the neutralizing solution (water in methanol) until color changes from brown to pale yellow. 22 When display reads “READY” or “ADD SAMPLE”, the system is ready for sample analysis. q Procedure Completed Date: Prepared By: Approved By: