Determination of Sulfide in Spent Sulfide Caustic Tank

Determination of Sulfide in Spent Sulfide Caustic Tank Cars by Are Revision Potentiometric Titration 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-037 0 6/28/11 References / Documents Yes PPE Standard (SSP-0011) q N/A 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 Determination of Sulfide in Spent Sulfide Caustic Tank Cars by Potentiometric Titration 1 Weigh 10 g sample into 1000 ml volumetric flask. 2 Dilute to volume with DI water. 3 Weigh approximately 3 g sample into plastic titration cup. 3. 1 Record weight to 3 decimal places. 4 Add 60 – 80 ml ammonical 4% Na. OH titration solvent. 5 Add stir bar. 6 Place sample on holder on Brinkman titrator. 7 Turn on stirrer by flipping red switch. 8 Lower electrode assembly into beaker. 9 Titrate sample with 0. 05 N Ag. NO 3 as follows: 9. 1 Ensure “MERCAP” method is selected. 9. 2 Press “START”. 9. 3 Wait for sample size box to display and enter sample size using keypad; press enter. 10 Once titration is completed, record mls titrant used from last endpoint detected. 11 Calculate result as follows: % Sulfide = (mls titrant)(0. 05)(16)(100) sample weight 12 Report result in Labworks to 1 decimal place. q Procedure Completed Date: 1 of 1 Prepared By: Approved By: Use Y