MicroDistillation of Process Samples by ISL PMD110 Are

Micro-Distillation of Process Samples by ISL PMD-110 Are a Unit Operating Procedure # 3 Lab OPS-LB-PS-017 Job Hazards 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 Revision # Certified by Scope / Objective Yes Date Page 09. 201 1 1 of 2 PPE Standard (SSP-0011) This procedure covers the determination of the distillation characteristics of process samples with boiling range between 20 – 400° C (68 – 752° F) at atmospheric pressure using an automatic micro distillation apparatus. Use Y Full Face Shield / Goggles Hood Clothing—Chemical Protection Gloves—Chemical Personal Fall Protection References / Documents Respirator / Filter Mask q ASTM D 7345 q ISL PMD-100/110 SOP Supplied Air Other: Equipment q PMD-110 Automatic Micro- q Citizen IDP-3551 Printer Distillation Analyzer Materials and Reagents q Granular Pumice Stones q Toluene q 10 ml Disposable Syringes with q ISL 10 ml Mini Distillation Flasks q Acetone Nozzle Tube Special Instructions Environmental Micro-Distillation of Process Samples by ISL PMD-110 1 Place volatile samples in ice bath to chill prior to analysis. 2 Power on the PMD-110 from main switch on rear panel just above power cord. 3 Press any key to bring display to the START menu. NOTE: If analyzer already on, access the START menu by pressing of key on front panel. 4 (back key) located to left Check and empty the condenser waste beaker if level is too full. NOTE: Testing cannot be started without the waste beaker in position due to a safety micro-switch. 5 Press the PRODUCT button. 6 Select the sample type from list by navigating the highlighted bar with the arrow pad on keyboard. 7 Press OK button. 8 Press the SMPL ID button and input the alphanumeric sample ID; press OK button. 9 (Optional Step) Press OPER button and select user running test with arrow pad; press OK. 10 Into a clean, dry distillation flask add about 4 – 8 chips of small grain pumice stone. 11 Fill plastic 10 ml syringe with sample; invert syringe and push plunger to 10 ml mark ensuring any air bubbles are removed Completed Date: Note: Prepared By: Approved By: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet.

Micro-Distillation of Process Samples by ISL PMD-110 Are Revision Unit Operating Procedure # Certified by Date a # Continued 3 Lab 09. 201 1 OPS-LB-PS-017 Page 2 of 2 Micro-Distillation of Process Samples by ISL PMD-110 (continued) 12 Insert the syringe nozzle into distillation flask (while orienting the side arm of the flask upward) and slowly dispense sample into flask. NOTE: If sample is dispensed too quickly, spillage will occur which will alter result of the test. 13 Life plastic protection shield up and away from the heating compartment. 14 Attach distillation flask to measuring head assembly ensuring flask is fully seated inside the black rubber lip seal (a click is heard when properly seated). 15 Ensure spring loaded push rod for heating element is in the lower position. NOTE: Inspect o-ring on measuring head attachment for any cuts or wear – replace if needed. 16 Insert glass side arm tube of flask to condenser tube gasket opening, then gently press in the spring, clip as you attach measuring head (missing verbiage that wasn’t able to view on scanned documents). 17 Press the spring loaded push rod for the heating elements to raise it to the upper position against flask bottom. 18 Lower plastic protection shield over the heating compartment. 19 Press START NOW button to begin test. NOTE: Once distillation is complete, result is automatically calculated and displayed on screen. A print-out of the results will be automatically initiated. 20 An audible alarm will sound at end of test – press button with picture of bell ( condition; i. e. “end of test”. 21 Press button for ACQUIT to silence alarm. ) to display alarm NOTE: At end of test, the heater compartment cooling fan will run for five minutes. 22 Lift plastic protection shield and press spring loaded push rod to lower flask heating element. 23 Once distillation flask has cooled, press spring clip of the measuring head and gently pull it from the connection. 24 Remove distillation flask from measuring head and place in flask holding device. 25 Immediately wipe liquid condensate from measuring head with a lint free tissue – wipe both temperature probes and the upper hole around the black sealing ring. 26 Return the measuring head to the holder. 27 Clean distillation flask first with toluene and then with acetone. 28 Return distillation flask to holder in the inverted position to allow it to drain. 29 If any flasks are heavily coated with carbon residue, place them in muffle furnace to clean. Completed Date: Prepared By: Approved By: Note: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet.