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Chapter 7 gas chromatograph
 

Chapter 7 gas chromatograph

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    Chapter 7 gas chromatograph Chapter 7 gas chromatograph Presentation Transcript

    • Chapter 7 Gas Chromatograph
      • 7.1 Introduction to Interphase Separations
      • Interphase Separations
      Mixed Substances Separated Components Stationary Phase Mobile Phase
    • 2. Classification of Chromatography Instrumentation
      • By the types of mobile phase & stationary phase
      • Gas - Liquid GLC
      • Gas - Solid GSC
      • Liquid - Liquid LLC
      • Liquid - Solid LSC
      • By stationary’s forms
      • Column
      • Paper
      • thin layer
      • By separation mechanism
      • absorption
      • partition
      • exchange
    • 3. Typical GCS Progresses Carrier gas Column Injector Sample Detector Chromatogram
    • 7.2 Principle of GC
      • 1. The Interphase Partition of One Substance
      C(m) C(s) (1) Partition Coefficient K 7-1
    • (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
    • 2.Theoretical Plate (1) Some common relationship (2) Theoretical Plate Model:
      • Height Equivalent to a Theoretical Plate(HETP)
      • Gas Flow rate is 1 plate Volume per time
      • K is a constant
      • Sample come into the plate only by the plate No. 0
      7-5
    •  
    •  
    • Binomial distributing 7-7 7-6
    • 3. Export Curve Equation
      • Export Curve Equation
      • (Gauss distribution)
      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 (V air ): unreteined volume V R : retention volume V’ R : adjusted retention volume
    • 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
      • u : velocity of the carrier gas
      • A, B and C are the constants for a given system
      7-18
    • 7.3 Separation of Components
      • Separation for tow components
      • (1) Resolution R
      (2) Separation Factor 7-19 7-20
    • 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
      • (3) Column types
      • Stationary type
      • Stationary Liquid and Temperature
      • Supporter
      (4) Injection time and volume 300 ~ 400 ℃ 200 ~ 300 ℃ 100 ~ 200℃ high mid low
    • 7.4 GC Instrument
      • Gas Supply
      Carrier Argon Carrier Helium Carrier Nitrogen Carrier, Fuel gas Hydrogen Function Type
    • 2. Sample Injector
    • 3. Column System
      • (1)Capillary GC Columns
    • (2) stationary phases Polysiloxanes
    • 4. Detector (1) Two Kinds of Detectors
      • Thermal conductivity detector (TCD)
      While equilibrium: R 1 R 3 =R 2 R 4
    • Electron capture detector (ECD)
    • Flame ionization detector (FID)
    •  
    • Flame photometric detector (FPD)
    • (2) Behavior of Detector
      • Sensitivity
      a) for concentration types 7-28 7-29 7-30
    • b) For mass types
      • Detect limit
      N: noise of detector(mV) A: area of the signal 7-31 7-32 7-33
      • Minimum detect quantity Q 0
      • Response time
      • Linear response range
      For mass: For concentration: 7-34 7-35 7-36
    • 7.5 Qualitative analysis
      • Comparison with pure maters
      • Work as a part of analysis system
      • GC-IR GC-MS
      • 3. Retention Index
    •  
    •  
    • 7.6 Quantitative analysis
      • Quantitative Equation
      • For same detector, different substance have different response sensitivity.
      Is called as Quantitative correction factor The equation Is Quantitative Equation. 7-37 7-38
    • 2. Determination of zone area (1) By calculation (2) Numerical integral by computer (3) By instrumental integral
    • 3. Normalization Methods
      • Assume the zones of every substance m j in sample have obtained, so:
      7-39
    • 4. Internal standard Methods
      • Use a internal standard sample its mass is a constant known as m s and its zone area is A s
      7-40 7-41