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Simdis Course

Simdis Course . AC Analytical Controls January 2001. Simdis - Introduction. Distillation is the most widely used separation process in the petrol industry

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Simdis Course

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  1. Simdis Course AC Analytical Controls January 2001

  2. Simdis - Introduction • Distillation is the most widely used separation process in the petrol industry • Knowledge of the boiling range is essential for quality assurance regulatory compliance refinery process control physical property predictions

  3. Simdis Vs. Physical Distillation • D86, D1160 generates an average boiling point of a mixture at a given point • D 2892, 15 theoretical plate, true boiling point • Time consuming, labor intensive, imprecise

  4. Simdis Vs Physical Distallation • GC analysis simulates a “true boiling point” • Simdis provides TBP of the individual components in a mixture at a given point • Automated • Accurate results • Fast • Detection of contamination or entrainment

  5. Simdis Theory • The technique of simulated distillation is based upon the assumption that individual components of a sample elute from a GC column in order of their boiling point.

  6. Available Simdis Methods Final boiling point • ASTM 3710 260 °C • ASTM 2887 538 °C • 2887 extended 620 °C • Ht 750 750 °C

  7. ASTM D 3710 • Gasoline, naphtha, kerosene • Final boiling point (FBP)<260°C • Packed or capillary column

  8. ASTM D 2887 • Petroleum products • Final boiling point (FBP)<538°C • Packed or capillary column • Cryogenic option

  9. ASTM D 2887 Extended • Petroleum products • Final boiling point (FBP)<620°C • Capillary column • Cryogenic option

  10. Ht 750 • Crude's and crude fractions, petroleum products • Boiling range from 35°C-750°C • Capillary column • Cryogenic option

  11. Requirements • non-polar stationery phase • linear temperature program • compensation of column bleeding

  12. Hardware • Gas chromatograph • Programmable temperature vaporizer (PTV injector) • FID detector • Column

  13. Typical Gas Chromatograph Fixed Mol-Sieve Traps Restrictors Injection Port Regulators Detector Electrometer Flow PC Controller Column Carrier Hydrogen Air Gas

  14. PTV

  15. Flame Ionization Detector Schematic FID Detector Assembly Air Inlet Capillary Column End-Position (1-2 mm from Top of Jet) Jet H2 Inlet + Make-Up Exit End of Column

  16. CO H 0 2 2 + + CHO CHO CO H 0 + 2 2 CHO + The FID is a destructive, mass sensing detector. Cations generated in the flame are counted and produce the detector signal. Analytes that have the greatest number of low oxidation state carbons produce the largest signal. + CHO CHO CO 2 H 0 2 H 0 2 H H 2 2 CH 4 H H 2 2 CH 4 H H CH 2 2 4 H H CH 2 2 4 Column CH H H 4 2 2 Jet CH H H 4 2 2 Flame Ionization Detector

  17. System Startup • Electrical connections • Gas connections – carrier, FID • GC and auto sampler configuration • Installation of liner & column • Installation of septum and syringe • Check flows

  18. Simdis Theory • A n-paraffin standard is analyzed to determine retention times • The times relate to the n-paraffin boiling points • A boiling point calibration curve is created by the software

  19. AC SIMDIS D 2887 Calibration AC SIMDIS Analyzers

  20. Calibration Report AC SIMDIS Analyzers

  21. Calibration Curve AC SIMDIS Analyzers

  22. Boiling Point Curve AC SIMDIS Analyzers

  23. Simdis Theory • Every analysis should be corrected for column bleeding • Analyze a blank in every sequence • The blank signal is automatically subtracted from every sample and reference signal

  24. Simdis Theory • The net signal is used to determine boiling points • IBP at 0.5 % of the total area • FBP at 99.5 % of the total area • The total area lies between start and end elution point • The start and end time are determined by elution algorithms

  25. Simdis Theory • A reference sample is analyzed to check system performance

  26. AC SIMDIS D 2887 Reference AC SIMDIS Analyzers

  27. AC SIMDIS D 2887 reference reports AC SIMDIS Analyzers

  28. AC SIMDIS D 2887 Reference Reports AC SIMDIS Analyzers

  29. Starting Analysis • Make & run a sequence • Calibration • Observe results • Reprocess if necessary

  30. Chromatogram: Boiling point (°C) 100 0 200 300 400 500 600 700 800 70000 65000 60000 55000 50000 45000 40000 35000 Signal 30000 25000 20000 15000 10000 Start Time End Time 5000 FBP IBP 0 0 5 10 15 20 25 30 35 40 45 Retention time (min) Non Fitting Blank

  31. Chromatogram: Boiling point (°C) 200 300 400 500 600 700 800 3000 2800 2600 2400 2200 2000 1800 1600 Signal 1400 1200 1000 800 600 400 Start Time End Time 200 FBP IBP 0 0 5 10 15 20 25 30 35 40 45 50 55 Retention time (min) End Time Found Incorrectly

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