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Chapter 7 Gas Chromatograph <ul><li>7.1 Introduction  to Interphase Separations </li></ul><ul><li>Interphase Separations  ...
2. Classification of Chromatography Instrumentation <ul><li>By the types of mobile phase & stationary phase </li></ul><ul>...
<ul><li>By stationary’s forms </li></ul><ul><li>Column  </li></ul><ul><li>Paper </li></ul><ul><li>thin layer </li></ul><ul...
3. Typical GCS Progresses Carrier gas Column Injector Sample Detector Chromatogram
7.2 Principle of GC <ul><li>1. The Interphase Partition of One Substance </li></ul>C(m)  C(s) (1)   Partition  Coefficient...
(2)   Partition Ratio  k p, q :  mass fraction in the stationary  and mobile phase k :   Partition Ratio or Capacity facto...
2.Theoretical Plate (1) Some common relationship (2) Theoretical Plate Model: <ul><li>Height Equivalent to a Theoretical P...
 
 
Binomial distributing 7-7 7-6
3. Export Curve Equation <ul><li>Export Curve Equation   </li></ul><ul><li>  (Gauss distribution) </li></ul>7-8
(2) The Shape of  Export curve t m  (t air ):  unreteined time  t R : retention time T’ R : adjusted retention time V m  (...
h:  Peak of zone   : Standard deviation Y: Width of zone  Y 1/2 : Half peak width 7-9 7-10 7-11 7-12 7-13
(3) The Number of theoretical plate and HETP L: length of the column 7-14 7-15 7-15 7-17
4.Van Deemter Equation <ul><li>u : velocity of the carrier gas </li></ul><ul><li>A, B and  C are the constants for a given...
7.3 Separation of Components <ul><li>Separation for tow components </li></ul><ul><li>(1) Resolution R </li></ul>(2) Separa...
2. Separation Equation of GC Assume:   Y 1 =Y 2 =Y, k 1 ≈k 2 =k 7-21 7-22 7-23
3. Three Separation factor (1) Column effect factor  n (2) Capacity  factor  k (3) Selective  factor  
4. The Choice of experimental qualification (1) Flow rate of carrier gas 7-24 7-25 7-26 7-27
(2) Column temperature <ul><li>(3) Column types  </li></ul><ul><li>Stationary type </li></ul><ul><li>Stationary Liquid and...
7.4 GC  Instrument
<ul><li>Gas Supply </li></ul>Carrier Argon Carrier Helium Carrier Nitrogen Carrier, Fuel gas Hydrogen Function Type
2. Sample Injector
3. Column System <ul><li>(1)Capillary GC Columns   </li></ul>
(2)  stationary phases   Polysiloxanes
4. Detector (1) Two Kinds of Detectors <ul><li>Thermal conductivity detector (TCD) </li></ul>While equilibrium: R 1 R 3 =R...
Electron capture detector (ECD)
Flame ionization detector (FID)
 
Flame photometric detector (FPD)
(2) Behavior of Detector <ul><li>Sensitivity </li></ul>a) for concentration types 7-28 7-29 7-30
b) For mass types <ul><li>Detect limit </li></ul>N: noise of detector(mV)  A: area of the signal 7-31 7-32 7-33
<ul><li>Minimum detect quantity Q 0 </li></ul><ul><li>Response time </li></ul><ul><li>Linear response range </li></ul>For ...
7.5 Qualitative analysis <ul><li>Comparison with pure maters </li></ul><ul><li>Work as a part of analysis system </li></ul...
 
 
7.6 Quantitative analysis <ul><li>Quantitative Equation </li></ul><ul><li>For  same detector,  different substance have di...
2. Determination of zone area (1) By calculation (2) Numerical integral  by computer (3) By instrumental integral
3. Normalization Methods <ul><li>Assume the zones of every substance m j  in sample have obtained, so:   </li></ul>7-39
4. Internal standard Methods <ul><li>Use a internal standard sample its mass is a constant known as m s  and its zone area...
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Chapter 7 gas chromatograph

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Chapter 7 gas chromatograph

  1. 1. Chapter 7 Gas Chromatograph <ul><li>7.1 Introduction to Interphase Separations </li></ul><ul><li>Interphase Separations </li></ul>Mixed Substances Separated Components Stationary Phase Mobile Phase
  2. 2. 2. Classification of Chromatography Instrumentation <ul><li>By the types of mobile phase & stationary phase </li></ul><ul><li>Gas - Liquid GLC </li></ul><ul><li>Gas - Solid GSC </li></ul><ul><li>Liquid - Liquid LLC </li></ul><ul><li>Liquid - Solid LSC </li></ul>
  3. 3. <ul><li>By stationary’s forms </li></ul><ul><li>Column </li></ul><ul><li>Paper </li></ul><ul><li>thin layer </li></ul><ul><li>By separation mechanism </li></ul><ul><li>absorption </li></ul><ul><li>partition </li></ul><ul><li>exchange </li></ul>
  4. 4. 3. Typical GCS Progresses Carrier gas Column Injector Sample Detector Chromatogram
  5. 5. 7.2 Principle of GC <ul><li>1. The Interphase Partition of One Substance </li></ul>C(m) C(s) (1) Partition Coefficient K 7-1
  6. 6. (2) Partition Ratio k p, q : mass fraction in the stationary and mobile phase k : Partition Ratio or Capacity factor  : phase ratio 7-2 7-3 7-4
  7. 7. 2.Theoretical Plate (1) Some common relationship (2) Theoretical Plate Model: <ul><li>Height Equivalent to a Theoretical Plate(HETP) </li></ul><ul><li>Gas Flow rate is 1 plate Volume per time </li></ul><ul><li>K is a constant </li></ul><ul><li>Sample come into the plate only by the plate No. 0 </li></ul>7-5
  8. 10. Binomial distributing 7-7 7-6
  9. 11. 3. Export Curve Equation <ul><li>Export Curve Equation </li></ul><ul><li> (Gauss distribution) </li></ul>7-8
  10. 12. (2) The Shape of Export curve t m (t air ): unreteined time t R : retention time T’ R : adjusted retention time V m (V air ): unreteined volume V R : retention volume V’ R : adjusted retention volume
  11. 13. h: Peak of zone  : Standard deviation Y: Width of zone Y 1/2 : Half peak width 7-9 7-10 7-11 7-12 7-13
  12. 14. (3) The Number of theoretical plate and HETP L: length of the column 7-14 7-15 7-15 7-17
  13. 15. 4.Van Deemter Equation <ul><li>u : velocity of the carrier gas </li></ul><ul><li>A, B and C are the constants for a given system </li></ul>7-18
  14. 16. 7.3 Separation of Components <ul><li>Separation for tow components </li></ul><ul><li>(1) Resolution R </li></ul>(2) Separation Factor 7-19 7-20
  15. 17. 2. Separation Equation of GC Assume: Y 1 =Y 2 =Y, k 1 ≈k 2 =k 7-21 7-22 7-23
  16. 18. 3. Three Separation factor (1) Column effect factor n (2) Capacity factor k (3) Selective factor 
  17. 19. 4. The Choice of experimental qualification (1) Flow rate of carrier gas 7-24 7-25 7-26 7-27
  18. 20. (2) Column temperature <ul><li>(3) Column types </li></ul><ul><li>Stationary type </li></ul><ul><li>Stationary Liquid and Temperature </li></ul><ul><li>Supporter </li></ul>(4) Injection time and volume 300 ~ 400 ℃ 200 ~ 300 ℃ 100 ~ 200℃ high mid low
  19. 21. 7.4 GC Instrument
  20. 22. <ul><li>Gas Supply </li></ul>Carrier Argon Carrier Helium Carrier Nitrogen Carrier, Fuel gas Hydrogen Function Type
  21. 23. 2. Sample Injector
  22. 24. 3. Column System <ul><li>(1)Capillary GC Columns </li></ul>
  23. 25. (2) stationary phases Polysiloxanes
  24. 26. 4. Detector (1) Two Kinds of Detectors <ul><li>Thermal conductivity detector (TCD) </li></ul>While equilibrium: R 1 R 3 =R 2 R 4
  25. 27. Electron capture detector (ECD)
  26. 28. Flame ionization detector (FID)
  27. 30. Flame photometric detector (FPD)
  28. 31. (2) Behavior of Detector <ul><li>Sensitivity </li></ul>a) for concentration types 7-28 7-29 7-30
  29. 32. b) For mass types <ul><li>Detect limit </li></ul>N: noise of detector(mV) A: area of the signal 7-31 7-32 7-33
  30. 33. <ul><li>Minimum detect quantity Q 0 </li></ul><ul><li>Response time </li></ul><ul><li>Linear response range </li></ul>For mass: For concentration: 7-34 7-35 7-36
  31. 34. 7.5 Qualitative analysis <ul><li>Comparison with pure maters </li></ul><ul><li>Work as a part of analysis system </li></ul><ul><li>GC-IR GC-MS </li></ul><ul><li>3. Retention Index </li></ul>
  32. 37. 7.6 Quantitative analysis <ul><li>Quantitative Equation </li></ul><ul><li>For same detector, different substance have different response sensitivity. </li></ul>Is called as Quantitative correction factor The equation Is Quantitative Equation. 7-37 7-38
  33. 38. 2. Determination of zone area (1) By calculation (2) Numerical integral by computer (3) By instrumental integral
  34. 39. 3. Normalization Methods <ul><li>Assume the zones of every substance m j in sample have obtained, so: </li></ul>7-39
  35. 40. 4. Internal standard Methods <ul><li>Use a internal standard sample its mass is a constant known as m s and its zone area is A s </li></ul>7-40 7-41

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