Bechtel BWXT Idaho, LLC IHRG MSN-99-789 Area 200 Procedure 6 1. (11/11/00- Rev. #4.0) Pb-Alloy Corrosion Study Procedures Identifier: Revision: Page: Pb Procedures 0 1 of 4 NaOH/Pb Corrosion Cell Assembly Effective Date: 01/11/01 PURPOSE Provide detailed assembly steps of the corrosion cell for molten extraction of Tellurium. 2. SCOPE AND APPLICABILITY This procedure provides the safe framework for assembly, loading solid Pb-alloys, and pressure check of the corrosion cell for experimental NaOH/Pb operation. Changes to the experimental setup for a particular run will be delineated in the experimental run plan. Any deviations from this procedure that may affect lead exposure will be approved by I.H. in the experimental run plan. 3. PREREQUISITES 3.1 The corrosion cell is cool to the touch. 3.2 The following PPE is on hand: - respirators - gloves for NaOH handling - disposal Tyvek clothing or Lab coat - safety glasses - steel toed safety shoes 3.3 The ventilation system is operational per procedure 300-2. 3.4 The following cleaning supplies are on hand: 3.5 - wet wipes - paper towels - glass cleaner - receptacle marked for Pb-containing trash - receptacle marked caustic containing wastes. Operators are current in lead training and respirator training, which will be handling the material. 3.6 GHT is assembled per procedure 300-1. 3.7 Gas injection system is assembled per procedure 100-1. Bechtel BWXT Idaho, LLC IHRG MSN-99-789 Identifier: Revision: Page: Pb Procedures 0 2 of 4 NaOH/Pb Corrosion Cell Assembly Effective Date: 01/11/01 Area 200 Procedure 6 4. (11/11/00- Rev. #4.0) Pb-Alloy Corrosion Study Procedures INSTRUCTIONS 4.1 Weigh the mass of the crucible The next step requires I.H. approved PPE (see procedure 100-2 for posted PPE). NOTE: At a minimum, researchers will don the following: - gloves for NaOH/Pb handling - lab coat or disposal Tyvek clothing - safety glasses 4.2 Load NaOH and Pb-Bi into reaction crucible as listed in the run plan. Place the external thermocouples on to the corrosion cell. 4.3 Verify the heaters are unplugged from the wall. 4.4 Place the crucible inside the corrosion cell; place the corrosion cell into the test stand. 4.5 Connect the thermocouples to the recording system. 4.6 With gaskets install the square flange 4.7 Tighten bottom flange bolts. 4.8 Bolt top flange onto the corrosion cell. 4.9 Make the following connections to the top plate: 4.9.1 Insert lance. 4.9.2 Connect oxidation/reduction lines. 4.9.3 Connect relief valve. Ensure tubing from the relief valve is run to ventilation duct. 4.9.4 O2 probe (if used). 4.9.5 Internal thermocouple (if used). 4.9.6 GHT exhaust line. 4.9.7 Cooling lines Bechtel BWXT Idaho, LLC IHRG MSN-99-789 4.9.8 Identifier: Revision: Page: Pb Procedures 0 3 of 4 NaOH/Pb Corrosion Cell Assembly Effective Date: 01/11/01 Area 200 Procedure 6 4.10 (11/11/00- Rev. #4.0) Pb-Alloy Corrosion Study Procedures Sample probes Perform gas leak check of the corrosion cell in the following sequence: 4.10.1 Verify the 10-psig relief is connected to the corrosion cell. Cap the offgas line to the GHT. 4.10.2 Open the inert gas cylinder valve and set the regulator pressure at 30 psig. 4.10.3 Pressurize the system (corrosion cell) to 5 psig, using the corrosion cell pressure gauge as indication. 4.10.4 Hold pressure at 5 psig 1 for 5 minutes. If the pressure cannot be held, then find leak and restart test. 5. 4.11 Connect the off-gas line to the GHT and the ventilation to the corrosion cell stand. 4.12 The system is now ready for experimental operation per the experimental plan. Note the maximum operating temperature is ½ the boiling point of the constituents added so as to keep the vapor pressure down. The boiling points are Pb 1620C, KOH 1320C, and NaOH 1390C. Therefore the maximum operating for an experiment is 660C. RECORDS 5.1 6. Log assembly and any abnormalities in the Pb-alloy Corrosion Laboratory Notebook. DEFINITIONS 6.1 Corrosion Cell: A piped section, which contains the molten Pb-alloy. The cell is gas tight. 6.2 GHT: Gas Handling Train. This system removes Pb particulate from the gas stream. 6.3 Top Plate: The top of the corrosion cell which is actively cooled and allows a feed-through of injection ports. 6.4 Crucible, a crucible with nominal dimensions of 3” OD and 3” in height, made from such materials as: nickel, carbon, alumina, schedule 40 pipe, etc. Bechtel BWXT Idaho, LLC IHRG MSN-99-789 Area 200 Procedure 6 7. (11/11/00- Rev. #4.0) Pb-Alloy Corrosion Study Procedures Identifier: Revision: Page: Pb Procedures 0 4 of 4 NaOH/Pb Corrosion Cell Assembly Effective Date: 01/11/01 REFERENCES 7.1 Corrosion cell schematic drawing. 7.2 MCP-2726 Respiratory Protection 7.3 MCP-2715 Hazard Communication 7.4 MCP-153 Industrial Hygiene Exposure Assessment 7.5 MCP-2716 Personal Protective Equipment 7.6 MCP-2980 Log Keeping 7.7 MCP-2747 Specialized Ventilation 7.8 MCP-2720 Controlling and Monitoring Exposure to Lead 7.9 MCP-2728 Compressed Gas 7.10 MCP-2737 High-Temperature Systems