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III.a. Analytical Technology |
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III.b. Sample Preparation |
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III.c. Monitoring (Air, Water, and Waste) |
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III.d. Quality assurance & Method
Development |
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III.e. Endocrine disrupting chemicals |
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III.f. Dioxin & PCBs |
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III.g. Pesticides |
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III.h. Future trend on monitoing technique |
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Ion-Selective Electrode |
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Respond selectively toward one particular ion in
the solution |
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Consists of a silver/silver chloride electrode
in d. HCl which is enclosed in an envelope of electrically conductive glass |
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Mobil phase |
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- Isocratic mode |
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- Gradient mode single pump |
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multiple pump |
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Normal phase(adsorption mode) : silica phase |
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bonded phase |
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Reverse phase(distribution mode) : C18
column |
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Ion exchange(ion exchange mode) : cation column |
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anion column |
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Size exclusion(molecular mode) : GPC |
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Optical Detector |
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- UV/Visible Detector |
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- Fluorescence Detector |
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- Refractive Index Detector |
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Electrochemical Detector |
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- Conductivity Detector |
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- Electrochemical Detector |
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A = ebc : Lambert-Beer’s Law |
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A : absorbance e : molar absorptivity |
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b : cell length c: conc. |
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Fixed type |
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Variable type |
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Photodiode array type |
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Carrier gas and injector |
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- Split |
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- Splitless |
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- On column |
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Column and column oven |
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Detector |
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Column Selection |
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Film Thickness |
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Temperature Limits |
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Polarity/Structures |
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McReynold’s Constants |
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Column Behavior |
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Test Mixtures |
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Dead Volume |
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Thermal Gradients |
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Equilibrium Time |
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Cool Down Time |
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Installation |
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Column Bleed |
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What is the Effect of Phase Type on Separation? |
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How
Do I Choose a Column |
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for My Separation? |
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Consult literature for what other’s have used
successfully |
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Call column manufacturers for their advice |
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Consider : |
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Influence of I.D. on resolution |
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0.20 or 0.25 mm I.D. usually best choice |
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Choosing thin or thick films |
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For high boiling compounds use thin film(0.25m or smaller) |
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For low boiling compounds use thick film(1 m or larger) |
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Influence of column length |
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30 meters usually best choice |
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Increase carrier gas flow rate |
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Increase temperature program ramp rates |
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Use hydrogen as a carrier gas |
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Reduce column length |
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Reduce column diameter |
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Reduce thickness of stationary phase |
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Detector Characteristics |
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- Sensitivity |
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- Noise |
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- Linearity |
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- MDQ |
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- Drift |
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- Classification |
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TCD |
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FID |
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ECD |
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NPD |
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PID |
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FPD |
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Response |
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Sensitivity |
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- Signal/Noise |
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- MDQ(minimum detectable quantity) |
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Selectivity |
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Dynamic Range |
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Linear Range |
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Mechanism of Operation |
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- Ionization Detectors(FID, ECD, NPD, PID) |
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- Physical Property(TCD, Gas Density) |
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Chemical Reaction(Hall Detector) |
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Response to Carrier Gas Flow |
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Mass Sensitive(FID, FPD, MS) |
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Concentration Sensitive(TCD, ECD, PID, IR) |
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Responsive |
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Specific |
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Selective |
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Universal |
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Destructive : FID, NPD, MS |
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Nondestructive : TCD, IR, PID |
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How are Typical Nitrogen Phosphorous
Detectors(NPD) Designed? |
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Operates Similar to an FID |
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Alkali Salt Bead ElectronicallyHeated to 600-800℃ |
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Alkali metal ions are emitted from bead which
interact with |
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Nitrogen and phosphorous containing column effluent
increasing detector current flow |
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Ionization process |
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Ionization : ABC + e ’ ABC+
+ 2e |
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Fragmentation : ABC+ ’ AB +
C + |
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AB+ + C¬(loss
of neural) |
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AC+ + B¬(rearrangement) |
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etc. |
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Electron ionization |
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Chemical ionization |
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m B2R2 |
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= |
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e 2U |
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Magnetic Sector Mass Spectrometry(MSMS) |
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Quadrupole Mass Spectrometry(QTMS) |
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Ion Trap Quadrupole Mass Spectrometry(ITMS) |
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Time of Flight Mass Spectrometry(ToFMS) |
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Ion Cycloton Resonance Mass Spectrometry(ICRMS) |
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Ion Mobility Mass Spectrometry(IMMS) |
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Isotope Ratio Mass Spectrometry(IRMS) |
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Gas Chromatography-Mass Spectrometry(GC-MS) |
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Liquid Chromatography-Mass Spectrometry(LC-MS) |
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Scan Mode Detection |
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Single Ion Monitoring Mode Detection |
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Radio immunoassay(2H, 13C,
125I) |
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Enzyme immunoassay |
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Heterogeneous assay |
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(Enzyme Linked Immuno Sorbent Assay : ELISA) |
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Homogeneous assay |
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(Enzyme Multiplied Immunoassay : EMIT) |
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Remove Matrix Effects |
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Achieve Partial Separation |
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MW |
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Group or Class |
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Reduction of Interferences in the Separation
Step |
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Ionic leachables – IC |
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Quench bacterial activity |
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Particulate matter – HPLC |
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Nonvolatile material – GC |
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Coeluting compounds |
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Preconcentrate Analyte(s) |
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Get Analyte(s) Into Solution |
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Get Analyte(s) Into a Phase Compatible with the
Separation Mobile Phase |
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Reduce the Requirements for a &/or N
in the Separation |
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Make the Analyte(s) Compatible w/Detector |
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Enhance the Sensitivity of the Detector |
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Filtration(whole air, size select and
Dichotomous) |
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Cellulose Fiber |
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Glass or Quartz Fiber |
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Teflon Coated Glass Fiber |
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Membranes |
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Centrifugal Collection(Cyclones, etc.) |
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Impaction |
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Electrostatic Precipitation |
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Continuous |
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Solid Adsorbents |
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Organic Polymers(Tenax, XAD-2, Carbotrap) |
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Inorganic (Silica gel, Florisil) |
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Carbon(Activated Carbon, Carbon Molecular
Sieves) |
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Cryogenic Trapping |
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Impingers |
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Whole Air Collection(Canisters, Glass Bulbs) |
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Derivatization Techniques |
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Remote Monitoring |
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Semi-continuous(Chrompack, Minicams etc.) |
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Primary source |
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Chemical Synthesis by product |
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Waste incenerator |
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Paper manufactoring |
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Car emission |
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Natural causes(forest fire, lighting etc) |
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Secondary source |
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Food intake |
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Inhalation |
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Skin contact |
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Estimation of Relative
Toxicities(TCDD-Equivalents) of Various Chlorinated Dibenzo-p-dioxins and
Dibenzofurans* |
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Range of contents, expressed as TEQ, in pg/g of
fats contained (except for fruit and vegetables), for various categories of
food. |
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PCDD and PCDF contents in breast milk in various
countries, expressed in pg/g fat. |
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Fungicide |
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Insecticide |
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Miticide |
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Nematocide |
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Heribcide |
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Growth Regulator |
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Dual GC/ECD(I) and NPD(II) chromatograms of
standard 25 pesticides. Peak
identity;
1. Isoprocarb, 2. Dimethoate, 3. a-BHC, 4. b-BHC, 5. g-BHC, 6. Diazinon, 7. Carbaryl, 8. Fenitrothion, 9.
Malathion, 10. Fenthion, 11. Parathion, 12. Aldrin, 13. Captan, 14.
Phenthoate, 15. o,p’-DDE, 16. p,p’-DDE, 17. o,p’-DDD, 18. Dieldrin, 19. m,p’-DDD,
20. Endrin, 21. p,p’-DDD, 22. o,p’-DDT, 23. p,p’-DDT, 24. Captafol, 25. EPN
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Total ion chromatogram of standard 25
pesticiides using SIM mode. Peak identity;
1. Isoprocarb, 2. a-BHC, 3. Dimethoate, 4. b-BHC, 5. g-BHC, 6. Diazinon, 7.
Carbaryl, 8. Fenitrothion, 9. Aldrin,
10. Malathion, 11. Fenthion, 12. Parathion, 13. Captan, 14. Phenthoate, 15. o,p’-DDE,
16. Dieldrin, 17. p,p’-DDE,
18. o,p’-DDD, 19. Endrin, 20. m,p’-DDD,
21. p,p’-DDD, 22. o,p’-DDT, 23. p,p’-DDT, 24. Captafol, 25. EPN
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슬라이드 노트