Queensland Energy Resources Limited Commercial and in Confidence STUART PROJECT EXPLORATION PERMITS (MINERALS) 3215 & MINERAL DEVELOPMENT LICENCE 177 and 225 ANNUAL REPORT FOR THE PERIOD 1st November 2007 to 31st October 2008 Queensland Energy Resources Ltd APPENDIX 3 Modified Fischer Assay Procedure November 2008 Distribution Electronic Copy (tab DME Brisbane delimited text) Electronic Copy (tab QER Brisbane delimited text) 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 1 Queensland Energy Resources Limited Commercial and in Confidence TABLE OF CONTENTS 1 SCOPE ...................................................................................................... 3 2 SAFETY & PRECAUTIONS...................................................................... 3 3 ASSOCIATED DOCUMENTS................................................................... 4 4 REQUIREMENTS...................................................................................... 4 4.1 Equipment 4 4.2 Reagents 4 5 PROCEDURE............................................................................................ 5 5.1 Pre-Start Checks 5 5.2 Filling Retorts 6 5.3 Assembling Glassware 7 5.4 Connecting Glassware to the Retorts 7 5.5 Operating MFA Bench 8 5.6 Removing and Weighing Glassware after Retorting Process 10 5.7 Weighing Retort for Final Weight and Coking Tendency Analysis 12 6 CALCULATIONS .................................................................................... 12 7 REPORTING ........................................................................................... 13 8 APPENDICES ......................................................................................... 15 8.1 Modified Fischer Assay Apparatus 15 8.2 Control Panel, Main Power Switch, Control Power Switch & Emergency Stop Button on MFA Bench - 16 - 9 REFERENCES .................................................................................... - 16 - 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 2 Queensland Energy Resources Limited Commercial and in Confidence 1 SCOPE This procedure follows ASTM D 3904-90, Oil from Oil Shale (Resource Evaluation by the Fischer Assay Procedure) and determines the amount of oil, water and spent shale obtained upon heating of a representative oil shale sample that has been crushed to an appropriate size. The amount of gas evolved is calculated from data obtained from following this procedure. The coking tendency of shale is also determined by this procedure. 2 SAFETY & PRECAUTIONS • Safety glasses must be worn at all times in designated areas. • Latex examination gloves must be worn when handling the shale samples. • The exit fan must be turned on and working when running the Modified Fischer Assay (MFA) bench to extract the gases produced during retorting. • Heat resistant gloves capable of protecting against 500oC must be worn when removing the retorts after a MFA analysis run. • Take care when assembling and disassembling the glassware to prevent breakages and cuts and inspect before use. Wearing leather gloves or similar is recommended when assembling glassware. • During the MFA run the glassware may drop off from the rubber stopper on the retort stem. Wearing leather gloves or similar is recommended when fitting the glassware back on to the rubber stopper on the retort stem as the stem of the retort gets hot during the MFA run. • Leather gloves should be worn when handling the slide hammer to minimise injury from pinch points. • If there isn’t sufficient extraction, a dust mask must be worn when packing or emptying the retorts due to the dust created from the oil shale and/or spent shale. • In the event of an emergency, the MFA bench is fitted with an emergency stop button which will shut down the bench causing it to trip. The MFA bench can be re started once it is confirmed the bench is operating correctly. If the Main Power switch has flicked to ‘Trip’, the switch must be turned to the left to ‘Reset’ and then switched to ‘On’. • Acetone and Toluene are flammable liquids. Acetone and Toluene must be stored in the flammable storage cabinet when not in use. Labelled wash bottles must be used for dispensing Acetone and Toluene in the laboratory. Inhalation of vapour and contact with skin and eyes should be avoided. The relevant MSDS should be consulted prior to handling these chemicals. All Acetone and Toluene waste must be contained in safety containers located in the fume cupboard and once full, the waste is transported to Transpacific for disposal as per LP 1.1 Laboratory Management Procedure. • Do not leave the MFA bench unattended when it is running the ASTM method or when the antifreeze/water solution is circulating through the tray. 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 3 Queensland Energy Resources Limited Commercial and in Confidence 3 ASSOCIATED DOCUMENTS • LP 1.1 Laboratory Management Procedure • LP 2.2 Laboratory Database Procedure • LP 3.1 Shale Sample Preparation – Splitting Procedure • LP 3.2 Laboratory Sample Management Procedure • LP 4.3 Density by Digital Density Meter Procedure • LP 4.4 Centrifuge Operating Procedure • LF4201 Oven Dried Moisture in Shale & Modified Fischer Assay Worksheet 4 REQUIREMENTS 4.1 Equipment • MFA bench (including ovens) with controller • VWR recirculation chiller, 1/3 HP Model 1173MD • Aluminium retorts with vent tube and 4 discs • Slide Hammer for tamping retort plug before retorting and removing plug after retorting • Steel Rod used with slide hammer to remove retort plug • Glassware – Insulated Allihn Condensers, Y Adapters, 100mL Centrifuge Tubes, Glass Beads 3mm • Rubber insulating electrical tape for wrapping Y adapters • Rack to hold centrifuge tubes and Y adapters • Rubber Stoppers, Retort Stems 25mm Bottom 29mm Top 25mm Height, Centrifuge Tubes 16mm Bottom 19mm Top 19mm Height • Cork Borer or similar tool to bore holes in rubber stoppers • Trolley for cooling hot retorts • Mettler Toledo Balance, 8100g capacity • Mettler Toledo Balance, 610g capacity • Holder for centrifuge tube and Y adapter assembly when weighing • Heat resistant gloves rated for 500oC • Drying tubes filled with silica gel • Kim Wipes • Latex Examination Gloves • Spatula • Screwdriver • Safety cans to collect Acetone and Toluene waste 4.2 Reagents • 50% Antifreeze/Water solution for chillers • Alconox detergent, Acetone and Toluene for cleaning glassware • Stopcock grease 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 4 Queensland Energy Resources Limited Commercial and in Confidence 5 PROCEDURE 5.1 Pre-Start Checks • Turn the MFA bench on by switching the Main Power switch to On. This will start the chiller running automatically. Switch the Control Power switch to On. This will start the exhaust fan running automatically. Refer to Appendix 8.2 for a photo of the control panel on the MFA bench showing the power switches, touch screen and emergency button. Refer to the chiller operating manual for further operating instructions. • Once the touch screen lights up, select the Bench Control button. Figure 5.1: Main Screen • When the temperature appears in the Cooling Water Input and the Cooling Water Output, start the pump by pushing the Start button under Cooling Pump Control. NOTE: The pump must be started as soon as possible to start the Antifreeze/Water solution circulating through the chiller otherwise the chiller will run dry and may be damaged. 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 5 Queensland Energy Resources Limited Commercial and in Confidence Figure 5.2: Bench Control Screen • Enable the ovens by pressing the Main button on the touch screen (Figure 5.2) and selecting the Disabled button for each oven (Figure 5.1) which will Enable each oven allowing them to be used. • Wait until the chiller gets down to 3oC before opening the inlet valve on the tray. The temperature can be read by pushing the Bench Control button (Figure 5.1). • Set the flow so the tray fills up, regulating with the inlet and exit valve to ensure there is no overflow. • Check there is sufficient grease on the bottom fitting of the condensers to prevent leakage in use and facilitate separation. If there isn’t sufficient grease use silicone free laboratory grease and apply a light coat completely around the condenser fitting. 5.2 Filling Retorts • Record data on LF4201 Oven Dried Moisture in Shale & Modified Fischer Assay Worksheet including sample identification, sample date, sample time, retort number, oven position, centrifuge tube number, technician’s name and current date. • At ambient temperature, obtain a tare weight to the nearest 0.1g for the empty retort, four discs, vent tube, and retort plug. Record on LF4201. • Obtain labeled sample bag containing representative shale sample requiring MFA analysis. Refer to LP 3.2 Laboratory Sample Management Procedure for process of analysing samples. • Before filling the retort with the shale sample, place the vent tube in the middle of the retort. 2008 Stuart Annual Report EPM 3215, MDL 177, MDL 225 6 Queensland Energy Resources Limited Commercial and in Confidence • Using the first two fingers of one hand, cover the top of the vent tube and the retort stem hole to prevent sample from collecting in those areas. • Obtain the sample and pour 1/5 of the sample into the retort, smooth with spatula and place first disc on top of that layer. NOTE: A dust mask must be worn if there isn’t sufficient extraction when packing the retorts due to the dust created from the oil shale. • Tamp top of disc with spatula to pack shale. • Repeat the process,