1. PPE Use Standard (SSP-0011) Y Full Face Shield / Goggles Hood Clothing—Chemical Protection Gloves—Chemical Personal Fall Protection Respirator / Filter Mask Supplied Air Job Hazards Y es Job Hazards Y es Access and EgressMoving Parts Activities of OthersNoise Adverse WeatherRail Movement Chemical ExposureSharp Edges ElectricitySlips, Trips, and Falls FatigueStatic Electricity Fire and ExplosionTrip Injuries Ground ContaminationTrapped Pressure Manual HandlingWorking at Height Other: References / Documents  Appendix 1: Materials and Reagents  SSP-0023A  SSP-0023B  UOP # AreaUnitOperating Procedure #Certified byRevision #DatePage 3LabOPS-LB-AL-00509.20.20111 of 4 Determination of HF Acid Strength and Water Content Environmental Special Instructions Scope / Objective Note: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet. Completed Date:Prepared By:Approved By: Determination of HF Acid Strength and Water Content WARNING: Neoprene gauntlets must be worn over protective gloves at all times when handling materials used for HF analysis. Full face shield and vinyl jacket must be worn at all times while dispensing HF acid. 1Turn on power to hot plate (250 ml beaker with 100 ml of mineral oil should already be placed on hot plate). 2Weigh 2 clean, labeled 500-ml and 125-ml plastic bottles w/caps. Record weights. 3Pour into the 500-ml bottles enough DI water for the weight of each to be 380 g (+/- 15 g). Reweigh and record weights. 4 Place each of the 2 bottles with water in 1000-ml beakers. Add sufficient ice to entirely surround the containers. Place layer of ice on the bottom of 2 500-ml beakers and place the empty 125-ml bottles on layer and add ice as before. 5Allow approximately 20 minutes for bottles to chill. 6 Retrieve the HF acid sample containers. Containers should have a red tag (indicating that the container has HF acid in it) and clearly display the reactor number. 7Under exhaust hood with the capped end facing away from you, ensure valve is closed and unscrew cap from cylinder labeled Rx 1. 8Rinse sample container and cap with acetone, then dry. 9Screw on the delivery tube to the container and tighten. 10Securely fasten sample container onto stand using clamps. CAUTION: Smaller bottles used for % water determination must always be filled first in order to avoid contamination of water from larger bottles. EquipmentMaterials and Reagents  300-ml Columbia LT-50 Monel® Cylinders  Buret, 25-ml  2 125-ml Nalgene® bottles (labeled 1 & 2)  2 500-ml glass beakers  Anhydrous Pyridine  Reagent grade Acetone  Pipet, 20-ml Volumetric (borosilicate glass)  Hot Plate (110-140°F)  Balance  Aquatest cma Karl Fischer Coulometric Titrator  2 500-ml Nalgene® bottles (labeled 1 & 2)  2 1000-ml glass beakers  1 N NaOH soln.  Phenolphthalein Soln, 1% in 50% IPA  Mineral Oil  Rubber Bulb Pipet Filler  1-ml Disposable Syringe with 3 ½” needle

2. AreaUnitOperating Procedure #Certified byRevision #DatePage 3LabOPS-LB-AL-00509.20.20112 of 4 Determination of HF Acid Strength and Water Content Continued Note: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet. Completed Date:Prepared By:Approved By: Determination of HF Acid Strength and Water Content (continued) 11 Uncap 125-ml plastic bottle labeled 1; place entire beaker (with bottle in ice) so that delivery tube is submerged inside bottle (use blocks to elevate beaker). 12 Carefully open valve of sample container and dispense sample until ½” layer of sample is in bottle and close off valve to sample container. 13Remove beaker with bottle from wooden blocks, replace cap tightly onto bottle. 14Uncap 500-ml plastic bottle (labeled 1) and with the use of blocks, insert the delivery tube below the surface of the water. 15 Carefully open valve of sample container to obtain at least 10 grams of sample and close valve. Remove beaker with bottle from blocks and replace cap. 16Repeat steps 7 – 15 for cylinder and bottles corresponding to Rx 2. 17Remove the 125-ml plastic bottles with sample from ice and wipe dry. Reweigh bottles and record weight. 18 Under hood with bottle cap angled away from you, remove cap from each of the small bottles and replace with similar cap with ¼“ hole and place each in beaker with mineral oil on pre-warmed hot plate for 1 hour. WARNING: Face Shield and Vinyl Jacket may be removed after Step 19, however, Gloves and Safety Glasses must be worn at all times throughout testing. 19Remove 500-ml bottles with sample. Thoroughly wipe dry, reweigh bottles and record weights. 20Add additional aliquot of approximately 20 – 30mls DI water to bottles (until about 1 inch from the top of container). 21Reweigh bottles and record weights. 22 Shake bottle #1 until acid and water are well mixed then pour 10 to 15 grams of solution (solution should not quite cover stir bar) into a plastic beaker with stir bar. Reweigh bottle and record weight. 23Add approximately 75 ml of DI water along with several drops of phenolphthalein soln. to beaker. 24Titrate sample using 1.0 N NaOH until pink endpoint which persists for 30 seconds. 25Repeat Steps 22 – 24 for bottle #2. 26 Calculate HF acid strength as follows: % HF = 2*(ml of NaOH needed for titration)* (A/B) C Where: A = Difference in weight between the empty 500-ml bottle (Step 2) and bottle with sample and total water (Step 21) B = Difference in weight between Step 3 and Step 19 C = Difference in weight between Step 21 and Step 22 27After 1 hour, remove small bottles from hot plate, replace original caps and thoroughly wipe bottles. 28Ice down the bottles in the beakers as before, taking care not to introduce moisture into the bottles.

3. AreaUnitOperating Procedure #Certified byRevision #DatePage 3LabOPS-LB-AL-00509.20.20113 of 4 Determination of HF Acid Strength and Water Content Continued Note: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet. Completed Date:Prepared By:Approved By: Determination of HF Acid Strength and Water Content (continued) 29 Turn on power to Karl Fisher titrator.  Press “Stirrer Speed” button, then “4”.  Press the button to start stirrer.  Press the “TITR CURRENT” button to count out any moisture present in the system. 30Allow bottles to cool for 15 – 20 minutes. 31Under hood, uncap bottle #1. 32 Angling bottle away from face, pipet 20 ml of pyridine into sample. Pipet tip should rest at an angle on inner wall of bottle to prevent bumping from reaction of acid with pyridine. 33Replace cap and return bottle to ice bath. 34Repeat Steps 31 – 33 for bottle #2. 35Wait a couple of minutes, then vent samples ensuring bottles are directed away from face. 36 Determine moisture for reagent blank as follows:  After flushing several times, draw 0.2 ml pyridine into syringe.  Puncture needle of syringe through septum of titrator ensuring needle does not touch liquid in reservoir.  Press “START/STOP” button.  Display will read “ADD SAMPLE”.  Lower needle to inject sample blank into liquid.  Wait for reading to display once analysis is completed (Display will flash “READY”).  Record moisture reading for blank. 37Remove bottle #1 from ice and wipe dry. 38Swirl sample and pyridine to ensure well mixed and analyze 0.2 ml of this mixture as before. Record number. 39Repeat Steps 37 – 38 for bottle #2. 40 Perform the following calculation for each sample to determine water content: % H2O = (Counts of sample mixture – Counts blank)/sample weight x 100. 41Turn off titrator. Clean Up After Analysis 1Add ice to the plastic waste container kept under hood. 2With sample cylinder clamped on stand, place the tip of delivery tube below the ice and insert blocks under plastic container. 3Slowly turn valve to empty HF acid into ice. CAUTION: HF will react vigorously when dispensed into ice.

4. AreaUnitOperating Procedure #Certified byRevision #DatePage 3LabOPS-LB-AL-00509.20.20114 of 4 Determination of HF Acid Strength and Water Content Continued Note: This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet. Completed Date:Prepared By:Approved By: Clean Up After Analysis (continued) 4Once cylinder has been emptied, valve is turned to fully open position. 5Pour approximately 250-ml acetone into beaker. 6Remove cylinder from stand and unscrew delivery tube. 7Pour acetone into cylinder and close valve. 8Invert cylinder several times to allow the acetone to clean the inside walls. 9Place cylinder back on the stand and open valve of container all the way to drain acetone in plastic container. CAUTION: Waste material is poured into a plastic one gallon bottle for disposal in the Alky unit. 10After draining cylinder completely, apply vacuum to opening to remove any moisture still present. 11Keep valve open and wipe cylinder clean. 12Screw on cap to cylinder and attach white tag on container labeled “Clean & Dry”. 13Repeat Steps 1 – 12 for remaining cylinder. 14Empty all plastic sample bottles into the one gallon plastic bottle for disposal and rinse bottles out with small washings of acetone. 15Add acetone to plastic bottles, shake well and allow to stand overnight.