Determination of Residue and Oil in Anhydrous Ammonia

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Plant Analytical Techniques …

Plant Analytical Techniques

Determination of Residue and Oil in Anhydrous Ammonia

This method is suitable for the determination of residue and oil in anhydrous ammonia.

FIELD OF APPLICATION
This method may be applied to standard and premium grade anhydrous ammonia having residue content in the range 10-5000 micrograms per gram and oil content in the range l-500 micrograms per gram

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  • 1. GBH Enterprises, Ltd. Plant Analytical Techniques ANHYDROUS AMMONIA: DETERMINATION OF RESIDUE AND OIL 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. ANHYDROUS AMMONIA: DETERMINATION OF RESIDUE AND OIL WARNING AND SAFETY PRECAUTIONS: VAPOR: CONCENTRATED VAPOR CAN CAUSE SKIN IRRITATION AND HIGH CONCENTRATIONS MAY GIVE SERIOUS BURNS TO EYES, RESPIRATORY PASSAGES AND LUNGS. CAN FORM EXPLOSIVE COMPOUNDS WITH CHLORINE, HYPOCHLORITE OR MERCURY. 1 SCOPE This method is suitable for the determination of residue and oil in anhydrous ammonia. 2 FIELD OF APPLICATION This method may be applied to standard and premium grade anhydrous ammonia having residue content in the range 10-5000 micrograms per gram and oil content in the range l-500 micrograms per gram. 3 PRINCIPLE Total residue (comprising water and involatile contaminants) is determined gravimetrically after evaporation of ammonia. Oil is extracted from the residue using a non-hydrocarbon solvent and its concentration determined by comparison of infra-red absorption with that of a standard oil solution. 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. 4 REAGENTS AND MATERIALS 4.1 1,1,2 -Trichlorotrifluoroethane : Analytical reagent grade, having < 15 micrograms per gram residue on evaporation. 4.2 Stock standard oil solution: weigh 0.500 + 0.001 g of lubricating oil or liquid paraffin into a 50 mL beaker. Add approximately 25 mL of 1,1,2-Trichlorotrifluoroethane (4.1), stir to dissolve and quantitatively transfer to a 250 mL volumetric flask. Dilute to the mark with 1,1,2-Trichlorotrifluoroethane (4.1) and mix. This stock solution is stable for a period not exceeding 2 months (1 mL = 2 mg oil). 5 APPARATUS 5.1 Infra-red spectrophotometer: A double beam ratio - recording instrument capable of scanning between 2000-4000 wave numbers (cm-l) and having a resolution better than 8 cm-l at 3000 cm-l is suitable eg PHILIPS PU9706 Infra-red Spectrophotometer is suitable 5.2 Optical cells, of path length 30 mm 5.3 Standard volumetric glassware : Class A. 6 SAMPLING Take 100 g (147 mL) of anhydrous ammonia into a 250 mL conical flask in accordance with Sampling procedure S2/2/1 of Sampling Procedures Manual SPL-FE. 7 PROCEDURE 7.1 Analysis for residue Immerse the sample flask in a continuous stream of cold water and allow the ammonia to evaporate slowly. When evaporation is complete, with a fixed air rate of 100 f 5 litres per hour, blow out traces of ammonia for 30 f 5 seconds. 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. Allow 30 minutes for the flask to equilibrate to room temperature, dry the outside of the flask, and weigh to the nearest 0.001 g; record this weight as 'A'g. Place the flask in an oven heated to 100 + 5OC for 20 minutes. Cool to room temperature, rinse the flask with several small (approx 5 mL) portions of 1,1,2-Trichlorotrifluoroethane. Transfer the washings to a clean dry 25 mL volumetric flask and dilute to the mark with 1,1,2-Trichlorotrifluoroethane. Retain this solution (solution 'A') for the determination of oil. Rinse the sample flask with 50 % v/v hydrochloric acid, with water and then with methanol. Heat in an oven at 100 + 5OC for 20 minutes, cool to room temperature and reweigh. Record this weight as 'B'g. 7.2 Analysis for oil Measure the absorbance of Solution 'A' from 7.1 at 2990 cm-1 on a scanning spectrophotometer. Similarly determine the absorbance of a solution prepared by diluting 0.5 mL of the stock standard solution (4.2) to 25 mL with 1,1,2-Trichlorotrifluoroethane (4.1) which contains 40 µg oil per mL. 8 EXPRESSION OF RESULTS 8.1 Method of calculation The residue, expressed as micrograms per gram, is given by the formula: Where: A is the weight, in grams, of the sample flask and residue: B is the weight, in grams, of the clean, dry sample flask: 100 is the weight, in grams, of anhydrous ammonia taken for analysis. 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. The residue should be expressed to the nearest 10 micrograms per gram for results up to 1000 micrograms per gram and to the nearest 100 micrograms per gram for results between 1010 and 5000 micrograms per gram. The oil content, expressed in micrograms per gram, is given by the formula: Where: A is the absorbance of the standard: B is the absorbance of the sample, corrected by subtracting the blank: 100 is the weight in grams of the anhydrous ammonia sample taken for analysis. The oil content should be expressed to the nearest microgram per gram for results between 0 and 30 micrograms per gram, to the nearest 5 micrograms per gram for results between 31 and 100 micrograms per gram, and to the nearest 10 micrograms per gram for results between 101 and 500 micrograms per gram. Note: If the absorbance of solution 'A' lies outside the range of calibration ie> 40 µg oil per mL, dilute a volume V1 mL of solution 'A' to V2 mL with 1,1,2-Trichlorotrifluoroethane (4.1). such that the absorbance of the diluted solution is within the range of calibration. 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. 8.2 Precision data 8.2.1 Repeatability The following data was obtained by the analysis of a solution containing 40 tig oil per mL on an infra-red spectrophotometer. Run Number Absorbance 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0.205 0.205 0.205 0.205 0.205 0.210 0.200 0.210 0.210 0.205 0.210 0.205 0.205 0.210 0.205 0.205 0.210 0.205 0.205 0.205 MEAN STD. DEVIATION % R.S.D. 0.206 0.0027 1.33 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
  • 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