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    Gas Chromatography: CBB4032 Analytical Chemistry Asna M.Z

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    Maziah Muhamad Nordin
    Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized. It works by carrying a gas mobile phase and sample through a column coated with a liquid or solid stationary phase. Compounds elute from the column at different rates and are detected. GC is used with detectors like FID, NPD, and MS for both qualitative and quantitative analysis of organic compounds in areas like environmental testing.

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    Gas Chromatography: CBB4032 Analytical Chemistry Asna M.Z

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    Maziah Muhamad Nordin
    76 views37 pages
    Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized. It works by carrying a gas mobile phase and sample through a column coated with a liquid or solid stationary phase. Compounds elute from the column at different rates and are detected. GC is used with detectors like FID, NPD, and MS for both qualitative and quantitative analysis of organic compounds in areas like environmental testing.

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    Gas Chromatography

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    Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized. It works by carrying a gas mobile phase and sample through a column coated with a liquid or solid stationary phase. Compounds elute from the column at different rates and are detected. GC is used with detectors like FID, NPD, and MS for both qualitative and quantitative analysis of organic compounds in areas like environmental testing.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    76 views37 pages

    Gas Chromatography: CBB4032 Analytical Chemistry Asna M.Z

    Uploaded by

    Maziah Muhamad Nordin
    Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized. It works by carrying a gas mobile phase and sample through a column coated with a liquid or solid stationary phase. Compounds elute from the column at different rates and are detected. GC is used with detectors like FID, NPD, and MS for both qualitative and quantitative analysis of organic compounds in areas like environmental testing.

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    of 37

    Gas Chromatography

    CBB4032 Analytical Chemistry Asna M.Z.

    Content: Intro to GC Column Detector GCMS Qualitative and Quantitative Application Video session -GCMS

    Introduction

    A physical separation method Involve distribution of component between two phases


    Stationary solid (10%) -liquid (90%) Mobile gas

    What compound can be determine by GC?


    Compound vaporise up to 450 C can be analyze by GC Compound that do not decompose at the T when vaporise Compound that quantitatively generate decompose product even if decomposed when vaporised

    Objective

    Separate a mixture containing organic Detect the individual analyte To identify and quantify the analyte base on the reference standard

    A GC system contain:
    Flow controller Injection port Column and column oven Detector Data processor

    The differential migration rate of analyte Mobile phase help sample to move through fixed phase. Column equilibrium: Xm Xs Linear velocity U = L/t

    (L=column length, t = ret. time for unretained peak)

    Flow rate(ml/min), F = 3.142r2L/t


    R is column radius

    Component of a GC

    Shimadzu QP2010Plus

    Method for GC analysis


    EPA 502.2 VOCs compound EPA 551.1 Chlorinated disinfection byproduct EPA 604 Phenol EPA 625 SVOCs Base neutrals, acid, pesticides SW-846 8260b Volatile organic 8270 Semivolatile organics

    Injection port
    Manual by direct injection Automated Autosampler - purge and trap

    Column oven
    Temperature control by Isothermal Gradient

    240 200

    Temp (deg C)

    160 120 80 40 0 0 10 20 30 Time (min) 40 50 60

    Column

    Packed
    Length 0.5-20m I.D. 2-4 mm Inj Vol-0.5-50 (gas) Or 0.1-1 ml (liq)

    Capillary column
    Length 10-100 m I.D. 0.1-0.53 mm Inj Vol-0.1-1 ml (gas) Or 0.004-2.0 ml

    Injection Mode
    Packed column injector Capillary column injector:

    Split adjust injection vol to column Splitless use for analysis of compound with high boiling points with low concentration samples Programming temperature vaporiser Cool on column injector

    Capillary column

    Fused silica

    Material for capillary column


    Fused silica material column activity attributed to expose silanol group and metal ions activity on surface of a glass capillary Treated with dilute hydrofluoric acid to remove imperfections

    Detector
    Mass Spectral Detector -MSD Flame Ionization FID Nitrogen-Phosphorus NPD Flame Photometric FPD

    Thermal Conductivity TCD Electron Capture ECD Photo Ionization - PID

    Detector principles and characteristics

    FID
    Most widely used GC detector Good sensitivity to almost all organic compounds Utilizes air-hydrogen flame that burn between two electrodes Separated component from GC column flow into the flame carbon containing compounds are burned producing charged ionsCH CHO + e

    + Oxidation

    NPD
    The NPD has a heated rubidium bead positioned between two electrodes A separated component from column flow across the bead and compounds containing N and P cause a current to flow between two electrodes The current is amplified and FED into the GC data system.

    FPD

    A miniaturized version of flame emission spectrophotometer Applied to Sulfur or Phosphorus containing compounds that burned in a small flame S and P wavelength are selected by filter in the light path

    S: (S-S)* (S-S) + hv (394 nm) P: (PHO)* (PHO) + hv (526 nm)

    TCD
    One of earliest GC Low sensitivity Use heated wire or semiconductor Resistance of wire changes with analyte vs carrier

    ECD

    Electron capture detector contain radioisotope of Nickel, 63N or 3H adsorbed on Pt or Ti foil that emit beta particle as its decay particle hit carrier gas cause electron burst to be released constant current Separated component flow in column to ECD and those with an affinity for electrons acquire negative charge. Cause current reduce = signal Most sensitive and selective GC Respond to compound contain halogen Chlorine, Bromine, Fluorine and Iodine ray and nitro groups. N N + + ePCB + e- PCBPCB + N2+ Neutral compounds
    2 2

    PID
    Column effluent irradiated with intense UV light source Ionizes molecules Measure ions with electrodes in detector cell

    GC-MS interphase
    Powerful tool for separation and quantitation Interphase of GC and MS require special jet separator or membrane separator for packed column MS operate under high vacuum

    Mass Spectral -GCMS


    Commonly Quadrupole or ion trap Time of flight/magnetic Use ion multiplier Require ion source
    Electron ionization-EI Chemical ionization-CI

    EI

    thermal electron (70eV) hit molecules and ionize them Ample fragment ion = ample structure info fingerprint

    CI

    Yield ionization in 2 stage:


    Reactive gas (methane) ionized by thermoelectron The primer ionize ion of reactive gas react with sample gas molecule to generate secondary ionize ion No fragment as molecule react in low energy state

    Ion trap

    Ion trap uses radio frequency to trap ions, hold or store them, then ejects them to detector

    Mode of GCMS operation


    Spectral mode display chromatogram at every second Total ion chromatography (TIC) all ions formed a high intensity signal Selective ion monitoring focus to certain mass/charge ratio, m/z of interest compounds only, very sensitive

    Qualitative
    Direct comparison of retention time Log plotting of homologues series Retention Index

    Qualitative analysis

    Identification by log plotting of homologues series


    A. a semilog plotting, one column Log Rt vs Cn or Bp or (CH2)n B. Log-log plotting, two column Log Rt (nonpolar) vs Log Rt (polar)

    Qualitative analysis

    Retention Index
    n-paraffin are chosen as standard components The retentian times of n-paraffin eluting before and after a target component are used to calculate the retention index

    Qualitative analysis

    Direct comparison of retention time


    Simplest method A known standard is first analyze under specific GC condition Unknown is then run under the same GC condition The difference in the retention times should not be more than +/- 0.1 min for proper identification

    Quantitative analysis
    Normalization Corrected area normalization Absolute calibration zero

    Quantitative analysis

    Absolute calibration curve method


    A relationship between the concentration of an analyte and its peak area (or height) Concentration of unknown can be calculated from this relationship External and internal standard

    Quantitative analysis

    External standard
    Concentration of an unknown A CA=C1/A1 x AA C- concentration, A- peak area

    Internal standard
    Concentration of unknown X Cx = (CA/Cs)(AA/As) x Ax/AIS x WIS IS- internal standard

    Calibration curve
    A ideal case B error in standard or impurity C Loss onto column D Error in standard or constant lost of analyte

    Linear equation calibration plot

    Y = a + bX, Y is peak response of analyte


    X is the concentration of analyte a is the intercept b is the slope

    Concentration X = (Y-a)/b If a = 0, b = 2x 106, the concentration of unknown U which shows a peak response of Y = 500,000 is determined to be 0.25 mg/mL Alternatively after the calibration range has been established, the concentration of unknown can be determined by response factor
    RF = Standard peak response/ standard concentration

    If two or more than one standard of different concentration within a linear range are measured, use average RF

    Normalization

    This method is simple, provided that each solute, i, the analytical signal lies within the linearity range, the peak area is proportional to the weight of solute pass through the detector cell, thus present in the injected volume Mi = KiAi here Ai is the peak area of solute I And Ki is the response coefficient Percentage in weight of each analyte %i = (Ki Ai)/(iKi Ai) x 100

    Application of GCMS
    Ideally suited to screen environmental samples with large variety of contaminant Ionize molecules and fragment products can be used to identify the compounds Produce mass spectrum based on the mass to charge ratio (m/z)

    References

    Jack Cazes (Ed) Encyclopedia of Chromatography, Marcel Dekker Inc. 2001 Perkin Elmer GC course note Nealk Osther and Patric K., Sampling and Analysis, Vol 4 K.H. Altgelt and T.H. Gouw (Eds), Chromatography in Petroleum Analysis, Marcell Dekker Inc Vol II Marco Pellie et al, Characterization of Contaminate Sediment, Battelle Press 2002

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