BENFIELD LIQUOR:Determination of Diethanolamine Using an Auto Titrator
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BENFIELD LIQUOR:Determination of Diethanolamine Using an Auto Titrator

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BENFIELD LIQUOR:Determination of Diethanolamine Using an Auto Titrator

1 SCOPE AND FIELD OF APPLICATION
This method is suitable for the determination of diethanolamine in Benfield Liquor.

2 PRINCIPLE
Diethanolamine is converted quantitatively into ammonia by boiling in the presence of sulfuric acid and copper sulfate. The ammonia is distilled from an alkaline medium and absorbed into boric acid. The solution is titrated with standard acid.

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  • 1. GBH Enterprises, Ltd. Plant Analytical Techniques BENFIELD LIQUOR: Determination of Diethanolamine - using an auto titrator Information 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: 1 Determination of Diethanolamine – using an auto titrator SCOPE AND FIELD OF APPLICATION This method is suitable for the determination of diethanolamine in Benfield Liquor. 2 PRINCIPLE Diethanolamine is converted quantitatively into ammonia by boiling in the presence of sulfuric acid and copper sulfate. The ammonia is distilled from an alkaline medium and absorbed into boric acid. The solution is titrated with standard acid. 3 Reagents 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. 3.1 Digestion mixture. dissolve 12 g of copper (11) sulfate crystals in 400 mL of water then carefully add 1600 mL of concentrated sulfuric acid (S.G.= 1.84) SULFURIC ACID - REACTS VIGOROUSLY WITH WATER WITH EVOLUTION OF HEAT – CAUSES SEVEREBURNS - DIGESTION MIXTURE IS CORROSIVE. 3.2 Hydrochloric acid. c(HC1) = 0.1 M HYDROCHLORIC ACID - CAUSES BURNS AND HAS A HARMFUL VAPOR 3.3 Boric acid, 1% with bromocresol green / methyl red indicator solution. Dissolve 100 g of boric acid in 10 L of water. Add 100 ml bromocresol green solution (100 mg in 100 ml methanol). Add 70 ml methyl red solution (alcohol soluble grade) (100 mg in 100 ml methanol). Mix thoroughly. 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
  • 3. Transfer 25 ml of the boric acid solution to a receiver flask and add 100 ml of water. If the solution in the flask is still red, titrate with 0.1 M sodium hydroxide solution until a neutral grey color is obtained. Calculate the amount of sodium hydroxide solution necessary to adjust the boric acid solution in the 10 L flask with the formula: ml 1.0 M alkali = ml titre x 40 Add the calculated amount of 1.0 M alkali solution to the boric acid solution. Mix. Check the adjustment result by distilling a new blank sample. METHANOL - TOXIC BY INGESTION - DAMAGING IF SPLASHED IN EYES. HIGH CONCENTRATIONS OF VAPOR MAY CAUSE DIZZINESS, STUPOR, CRAMPS AND DIGESTIVE DISTURBANCE. LOWER LEVELS MAY CAUSE HEADACHE AND NAUSEA. BROMOCRESOL GREEN AND METHYL RED - HARMFUL AVOID CONTACT WITH EYES AND SKIN. SODIUM HYDROXIDE IRRITATING TO EYES AND SKIN. 3.4 Sodium hydroxide solution, 35-40%. SODIUM HYDROXIDE - CAUSES BURNS AVOID CONTACT WITH EYES AND SKIN. 4 APPARATUS 4 .1 Standard volumetric glassware. Class A. 4.2 Digestion system, a Tecator Digestion system 6 1007 Digester is suitable. 4.3 Auto-titrator, a Tecator Kjeltec AUTO 1030 analyzer 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. 5 5.1 Procedure Blank determination Perform a blank determination using 50 ml of water, following the procedure described in sub-section 5.2 from "Connect the distillation tube". 5.2 Calibration Dry ammonium sulfate at 105 deg C for 1 hour. Weigh exactly 0.1000 g. Transfer to the distillation tube of the auto-titrator (4.3), add approximately 50 ml water. Connect the distillation tube to the splash head. Start the run in accordance with the manufacturer's instructions. (see Annex 1 for Parameters and Operational procedure for the Tecator Kjeltec AUTO 1030 analyzer). 5.3 Preparation of the solution. 5.3.1 Weigh 10 g to the nearest 0.001 g of sample and transfer quantitatively into a digestion tube. Add carefully and slowly (dropwise initially) 20 ml of digestion mixture (3.1). Set up the digestion system (4.2) according to the manufacturer's instructions. Place the digestion tube in the digestion system (4.2). Heat the mixture in the digestion system to boiling and continue to digest for 1 hour (following manufacturer's instructions). 5.3.2 Cool the mixture, and then carefully add approximately 40 ml of water. Mix thoroughly. 5.4 Determination Set up the auto-titrator according to the manufacturer's instructions. Transfer the sample as prepared in sub-section 5.3 into the distillation tube of the auto-titrator (4.3). Add approximately 40 mL of water. Continue as described in sub-section 5.2 from "Connect the distillation tube.......". 6 Expression of Results 6.1 Express the results of analysis as a percentage of diethanolamine in the Benfield Liquor as % m/m. 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
  • 5. ANNEX 1 – Parameters Ensure the Tecator Kjeltec AUTO 1030 analyzer is set up as below: A B and C are the front panel settings Where A = Delay time B = Factor for converting mL of 0.1 M HCl to diethanolamine % m/m. [( § is given by the expression 1.05 x 1 )] M 10 where M = mass of sample C = Blank value (* is the current blank value as obtained in sub-section 5.1 e.g. for 0.2 mL the blank value is 0.2 x 10 i.e. 20) Operational After the appropriate parameters have been set up as shown above proceed as follows: 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
  • 6. Close the safety door after completion CYCLE OVER light will come on permanently. Open safety door and wait until CYCLE OVER light comes on permanently. Remove digestion tube (DANGER - HOT SURFACE) and carefully wash six times with water, then wash with dilute sulfuric acid finally wash with water. Result is displayed directly on left of front panel as % m/m. 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