IHRG
MSN-99-789 / Pb-Alloy Corrosion Study
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Area 200 Procedure 6 / NaOH/Pb Corrosion Cell Assembly / Effective Date: / 01/11/01
1.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
3.1The corrosion cell is cool to the touch.
3.2The following PPE is on hand:
-respirators
-gloves for NaOH handling
-disposal Tyvek clothing or Lab coat
-safety glasses
-steel toed safety shoes
3.3The ventilation system is operational per procedure 300-2.
3.4The following cleaning supplies are on hand:
-wet wipes
-paper towels
-glass cleaner
-receptacle marked for Pb-containing trash
-receptacle marked caustic containing wastes.
3.5Operators are current in lead training and respirator training, which will be handling the material.
3.6GHT is assembled per procedure 300-1.
3.7Gas injection system is assembled per procedure 100-1.
4.INSTRUCTIONS
4.1Weigh the mass of the crucible
NOTE:The next step requires I.H. approved PPE (see procedure 100-2 for posted PPE). At a minimum, researchers will don the following:
- gloves for NaOH/Pb handling
-lab coat or disposal Tyvek clothing
-safety glasses
4.2Load NaOH and Pb-Bi into reaction crucible as listed in the run plan. Place the external thermocouples on to the corrosion cell.
4.3Verify the heaters are unplugged from the wall.
4.4Place the crucible inside the corrosion cell; place the corrosion cell into the test stand.
4.5Connect the thermocouples to the recording system.
4.6With gaskets install the square flange
4.7Tighten bottom flange bolts.
4.8Bolt top flange onto the corrosion cell.
4.9Make the following connections to the top plate:
4.9.1Insert lance.
4.9.2Connect oxidation/reduction lines.
4.9.3Connect relief valve. Ensure tubing from the relief valve is run to ventilation duct.
4.9.4O2 probe (if used).
4.9.5Internal thermocouple (if used).
4.9.6GHT exhaust line.
4.9.7Cooling lines
4.9.8Sample probes
4.10Perform gas leak check of the corrosion cell in the following sequence:
4.10.1Verify the 10-psig relief is connected to the corrosion cell. Cap the off-gas line to the GHT.
4.10.2Open the inert gas cylinder valve and set the regulator pressure at 30 psig.
4.10.3Pressurize the system (corrosion cell) to 5 psig, using the corrosion cell pressure gauge as indication.
4.10.4Hold pressure at 5 psig 1 for 5 minutes. If the pressure cannot be held, then find leak and restart test.
4.11Connect the off-gas line to the GHT and the ventilation to the corrosion cell stand.
4.12The 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.
5.RECORDS
5.1Log assembly and any abnormalities in the Pb-alloy Corrosion Laboratory Notebook.
6.DEFINITIONS
6.1Corrosion Cell: A piped section, which contains the molten Pb-alloy. The cell is gas tight.
6.2GHT: Gas Handling Train. This system removes Pb particulate from the gas stream.
6.3Top Plate: The top of the corrosion cell which is actively cooled and allows a feed-through of injection ports.
6.4Crucible, a crucible with nominal dimensions of 3” OD and 3” in height, made from such materials as: nickel, carbon, alumina, schedule 40 pipe, etc.
7.REFERENCES
7.1Corrosion cell schematic drawing.
7.2MCP-2726 Respiratory Protection
7.3MCP-2715 Hazard Communication
7.4MCP-153 Industrial Hygiene Exposure Assessment
7.5MCP-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
7.9MCP-2728 Compressed Gas
7.10MCP-2737 High-Temperature Systems