Chemical Plant DEF Testing - Urea Content by Refractive Index using the ATAGO Pocket Refractometer

PURPOSE This procedure describes the determination of urea content as % m/m by measuring the Refractive Index (RI) at 20 C of the sample using the ATAGO Pocket Refractometer. This method is ONLY applicable to a Blend DEF sample. For a Batch DEF sample, the ATAGO bench top Refractometer Model RX-5000 is used for maximum accuracy. The procedure is developed according to ISO 22241-2:2006(E), Annex C. 2.0 SCOPE This procedure applies to the DEF chemical operations at the Kilsyth plant. 3.0 SAFETY & ENVIRONMENTAL INFORMATION Item Sim No NA Comentrios Tipo de Resduo x Trade (x) Prescribed (x) Geral (x) Waste Agreement Req: x Conforme EPA/OHS x OHS de 2004, & EPA de 1970 Requisitos PPE x De acordo com este documento e poltica de PPE

4.0 RESPONSIBILITY Operations Manager: To ensure all personnel are trained and authorized in the application of this procedure. To ensure any incidents are reported and documented in accordance with reporting procedures. To ensure this procedure has been reviewed in line with document control procedures. Chemicals Area Supervisor: To ensure all applicable personnel are training and authorised in the application of this procedure That only trained and authorized personnel operate equipment That this procedure is reviewed and updated with any changes and in line with document control Supervising Chemist: To ensure this testing is carried out according to the procedure described herein. To ensure this procedure has been reviewed and updated in line with document control procedures. 5.0 OHS INSTRUCTIONS Protective equipment must be used where there is exposure to chemicals as detailed in the appropriate MSDS. As a minimum while handling and measuring chemicals the following should be adhered to: Wear Safety glasses, Nitrile Protective Gloves and Good work clothes Ensure other employees are not at risk while handling chemicals Never store or consume food and drink within the laboratory or near where chemicals are handled. Ensure any minor spills are cleaned up immediately Report all incidents no matter how minor to your supervisor or manager. Never perform any task or job unless you have been trained and authorised. Never operate any equipment unless you have been trained and authorized APPLICABLE DOCUMENTS AUMGT 224 - CHEMICAL HAZARD SPILL AUMGT 468 - Incident Reporting Procedure AUSMS 066 - PPE Procedure AUSMS 038 - Safety Standards 7.0 CRITICAL PROCESS STEPS HEREIN 7.1 Measurement is based on the proportional relationship between refractive index and the concentration of urea in the DEF at a definite temperature. 7.2 ISO 22241 stipulates a definite temperature of measurement at 20.0 +/-0.02 C. 7.3 The temperature of the DEF Blend sampled shall be brought to 20.0 C in a water bath.

8.0 INSTRUCTIONS 8.1 The Equipment ATAGO Pocket Refractometer 8.1.1 The ATAGO Pocket Refractometer is factory-calibrated to measure the refractive index of aqueous Urea. 8.1.2 The Refractometer produces a reading of Urea % with an accuracy of 0.1% m/m. 8.1.3 COMARK digital thermometer with a stainless steel rod sensor. 8.2 Sampling: from Blend Tank 16 8.2.1 Sampling and testing shall only commence after the DEF blending process is completed. 8.2.2 Completion of the blending and mixing is indicated by a visual/audible alarm set off in Citect. 8.2.3 Acknowledge the alarm and sample the DEF from Tank 16 as follows. 8.2.4 Ensure valve to sight tube is closed. 8.2.5 Place DEF waste bucket underneath manual sampling valve. 8.2.6 Remove urea which has crystallized around the sample point. 8.2.7 Open sample valve and flush the sample line by running about 1litre of the DEF into the bucket. 8.2.8 Rinse the 1-litre HDPE sample bottle with about 200 ml DEF. Discard the rinse into waste bucket. 8.2.9 Fill the sample bottle and secure the lid. 8.2.10 Label the sample bottle accordingly. 8.2.11 BLEND NUMBER yyddd0802tt-nn yyddd = Julian date of year followed by day of the year. 0802 = Australian plant. tt = tank it was blended in and finally nn = the blend of the day. An example being 09255080216-01 Which means it was blended in 2009 on the 12th of September in the Australian plant Tank 16 and was the first blend of the day. 8.3 Sample Preparation Temperature Equilibration: 8.3.1 Prior to measuring the RI/Urea%, ensure the sample is brought to ISO defined temperature 20 C. 8.3.2 Due to the endothermic reaction occurring in the dissolution of urea prill in DI water, the temperature of a freshly blended DEF is usually below 10 C. 8.3.3 Place sample bottle in the warm water bath of 30 C. 8.3.4 Clean the thermometer sensor rod with DI water. Dry with clean tissue paper before placing it in sample. 8.3.5 Stir and mix sample with the sensor rod. 8.3.6 Ensure sample is not contaminated by the water in the water bath. 8.4 Measurements: 8.4.1 Calibrate the ATAGO Pocket Refractometer with DI water at 20 C. 8.4.2 Dispense DI water onto the prism surface of the Refractometer. Press START button on the unit. The unit should display 000 8.4.3 Clean and dry the prism surface with soft tissue paper. 8.4.4 Confirm temperature of DEF sample is at 20 C and measure the RI/urea. Introduce sample to Refractometer using a new disposable liquid dropper. 8.4.5 Repeat Steps 5.4.2 and 5.4.4. Ensure Refractometer is cleaned and dried between each measurement taken. 8.4.6 Record the urea content of two identical measured readings. 8.4.7 Record the urea content and RI in the DEF Analysis Worksheet Refractive Index & Urea Content. 8.5 Blend Report in Citect: 8.5.1 To call up a blend report Click on Tank 16 Report on the DEF Citect main screen. 8.5.2 Select Blend and press the Confirm button 8.5.3 The Report shall open up on the screen. 8.5.4 Enter the required fields including the Urea Prill Bag Batch numbers used for the blend. 8.5.5 Once complete the Not in Spec shall cease to flash, return to the DEF Tank16 Control page. The blend is ready to be transferred into one of the three Batch tanks.(NOTE: Provided that the destination tank is not already full or certified) 8.5.6 Press the Destination button; select either Batch Tank 17, 18 or 19 as required. Citect prevents transfer to a Batch tank if the content in this tank has been and is still certified or tank has already 3 blends transferred to it 8.5.7 Once selected press the Waiting to Complete button. Authorized operator name and password are required to initiate the transfer. 8.5.8 The system will save the data to the database and print out a blend report for that particular blend. 8.5.9 All Blend reports for the same Batch shall be retained together with the Batch report generated by Citec once the Batch is completed. 9.0 OPERATOR CARE INSTRUCTIONS: Ensure the prism surface of the Refractometer is not scratched. 10.0 DOCUMENT REVISION HISTORY