1. GBH Enterprises, Ltd.Plant Analytical Techniques BENFIELD LIQUOR: DETERMINATION OF IRONInformation contained in this publication or as otherwise supplied to Users is believed to be accurate and correct at time of going to press, and is given in good faith, but it is for the User to satisfy itself of the suitability of the information for its own particular purpose. GBHE gives no warranty as to the fitness of this information for any particular purpose and any implied warranty or condition (statutory or otherwise) is excluded except to the extent that exclusion is prevented by law. GBHE accepts no liability for loss or personnel injury caused by or resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed.Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com

2. Benfield Liquor: Determination of Iron1SCOPE AND FIELD OF APPLICATION This method is suitable for the determination of the total iron in Benfield liquor samples up to a concentration of approximately 100 ppm m/v.2PRINCIPLE A solution containing a compound of the metallic element under investigation is aspirated into the flame of an atomic absorption spectrophotometer, causing evaporation of the solvent and leaving a solid residue. This process is rapidly followed by vaporization of the solid residue with concomitant molecular dissociation into its constituent atoms which are capable of absorbing radiant energy. The absorption of the radiation from the light source by the atomic vapor is measured and displayed by the spectrophotometer, in graphical format.3REAGENTS During the analysis, use only reagents of analytical reagent grade, unless otherwise specified, and water which has been deionized and then distilled from an all glass apparatus, or water of equivalent purity. 3.1Hydrochloric acid (SG 1.18)THIS REAGENT CAUSES BURNS AND PRODUCES A HARMFUL VAPOR. 3.2Ferric nitrate, standard spectroscopic solution in approximately 0.5 mol/L nitric acid. 1 mL = 1.00 mg iron3.3Stock standard iron solution: dilute 10 mL of the ferric nitrate solution (3.2) to 100 mL with water in a one-mark volumetric flask. 1 mL = 100 g IronRefinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 3. 3.44Working standard iron solutions: dilute 2.5 and 5.0 mL of the stock standard iron solution (3.3) to 100 mL with water in four one-mark volumetric flasks. These working standard solutions will be equivalent to 2.5 and 5.0 g/m.l (ie ppm m/v) iron respectively.APPARATUS 4.1Standard volumetric glassware, class A.4.2Atomic absorption spectrophotometer. A Philips PU 9400 model,or similar, is suitable.Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 4. 5PROCEDURE 5.1Test portion, and preparation of the test solution. Pipette 5.0 ml of test sample into a glass beaker then add 15 ml of hydrochloric acid (3.1). Heat to dissolve any precipitate, if evident, then allow to cool and transfer to a 100 ml one-mark volumetric flask Dilute to the mark with water.5.2Blank solution Prepare a blank solution, using the same reagent quantities as for the test solution (5.1), but omitting the test portion.5.3DeterminationRefinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 5. 5.3.1 The operating conditions for the atomic absorption spectrophotometer (4.2) are as follows: Lamp - iron hollow cathode; Wavelength - 248.3 nm; Band pass - 0.2-0.5 nm; Flame - air/acetylene, fuel lean, blue. 5. 3.2 Aspirate, the lowest concentration working standard solution (3.4), the blank solution (5.2), the rest of the working standard solutions, and the test solution (5.1). consecutively into the atomic absorption spectrophotometer (4.2). in accordance with the manufacturer's instructions.ASPIRATE THE WORKING STANDARD SOLUTIONS CONSECUTIVELY FROM THE LOWEST TO THE HIGHEST CONCENTRATION. TEST SAMPLES OF IRON CONCENTRATION > 50 PPM M/V MUST BE FURTHER DILUTED TEN-FOLD PRIOR TO ASPIRATION. 5. 3.3 The atomic absorption spectrophotometer will establish the absorbance-concentration relationship to give the concentration equivalent of the measured test solution absorbance. 6EXPRESSION OF RESULTS 6.1 The iron in the test solution (5.l), expressed as ppm m/v, is given by automated interpolation from the standard curve displayed on the atomic absorption spectrophotometer. 6.2 As dilution of the test portion is necessary, the iron in the test sample, expressed as ppm m/v, is given by the expression C1 x V2 V1Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 6. Where C1 is the concentration of iron in the test solution (in ppm m/v) derived automatically from the standard curve; V2 is the volume of the test solution n (in mL, ie 100 mL); V1 is the volume of the test portion taken for dilution (in mL; ie 5.0 mL.); 6.3 For test samples of iron concentration > 50 ppm m/v, a further tenfold dilution of the test solution will be necessary. The iron, expressed as ppm m/v, is given by the expression C1 x V2 x 10 V1Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 7. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com