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Updated: 15 September 2019 1 CEE 772: 9/15/2019 Mohan CEE 772 #5b Aarthi Instrumental Methods in Environmental Analysis LECTURE #5B AARTHI MOHAN ATOMIC SPECTROSCOPY: INSTRUMENT DESIGN (SKOOG, 4

  1. Updated: 15 September 2019 1 CEE 772: 9/15/2019 Mohan CEE 772 #5b Aarthi Instrumental Methods in Environmental Analysis LECTURE #5B AARTHI MOHAN ATOMIC SPECTROSCOPY: INSTRUMENT DESIGN (SKOOG, 4 TH ED., CHAPTER 10; HARRIS 7 TH ED., CHAPTER 21)

  2. 2 Types of optical spectrophotometers  UV-Vis Spectrophotometer  Atomic Spectrophotometer (AS)  Flame atomization  Atomic Absorption Spectroscopy (AAS)  Flame Emission Spectroscopy (FES)  Atomic Fluorescence Spectroscopy (AFS)  Infra-red absorption Spectroscopy (IR)  Raman Spectroscopy  X-Ray spectroscopy  Nuclear Magnetic Resonance (NMR) Spectroscopy CEE 772 #5b Aarthi Mohan 9/15/2019

  3. 3 Atomic Spectrophotometry  Use  Analysis of metals (> 70 elements, ppm to ppb levels)  Very sensitive  Heat treatment for conversion of components into gaseous form (atomization)  Three types  Absorption (AAS)  Flame and electrothermal (furnace)  Emission (AES)  Often used with plasma  Fluorescence CEE 772 #5b Aarthi Mohan 9/15/2019

  4. Atomic Absorption Spectrophotometers 4 Atomizer (in place of sample holder); flame, furnace or plasma (2000-8000K) Amplifier and Wavelength Photoelectric readout selector detector A plasma is a gas hot enough to contain electrons and ions. Elements measured by absorption or emission of UV or Vis by these atoms 9/15/2019 CEE 772 #5b Aarthi Mohan

  5. Atomic Absorption Spectrophotometers 5 - High sensitivity - Ability to distinguish one element from a complex mixture - Multi-elemental analysis - High throughput Molecular Atomic spec. spec. - Ppm-ppt ~100nm 0.001 nm; little over lap, - Equipment are expensive sharp peaks (>>70 elements at once) CEE 772 #5b Aarthi Mohan

  6. Atomic Absorption Spectrophotometers 6 Iron cathode ; Ne+ or Ar+ 2000-3000K Flame pathlength 10cm CEE 772 #5b Aarthi Mohan

  7. Atomic Fluorescence Spectrophotometers 7 0.1 μ s 0.2 nm res PbCO3 1000 times more sensitive than AAS Uncommon equipment CEE 772 #5b Aarthi Mohan

  8. 8 Light (Radiation) Source -Hollow Cathode Lamps  Tungsten anode and cylindrical cathode sealed in glass tube filled with neon or argon 1-5 torr.  Cathode (neg)= metal whose spectrum desired -Most are single element Ar + -Some multi-element lamps are available  Sputtering M o More than one metal in the cathode  Metal atoms are -Currents are optimized dislodged -Short life M *  Excitation M o Moderate cost ($180-$250)  Through contact Ar + -Less suited for volatile elements with fill gas ions   Emission M o M * h CEE 772 #5b Aarthi Mohan 9/15/2019

  9. 9 Electrodeless discharge lamps (EDL)  Radiation intensity 1-2 orders of magnitude greater than hollow- cathode.  No electrode; energized by radio-frequency or microwave  Brighter than hollow cathode (lower detection limits)  Longer life than hollow cathode.  Intensity drift issues have been noted.  Requires a special power supply  Available for 15 or more elements CEE 772 #5b Aarthi Mohan 9/15/2019

  10. Atomization: Flames, furnaces, plasma 10 Flames (decades Furnaces of use) Plasma CEE 772 #5b Aarthi Mohan

  11. Flame AA 11 (Reversible) (Reversible) Fuel Oxidant Temperature (K) H 2 Air 2000-2100 C 2 H Air 2100-2400 2 H 2 O 2 2600-2700 Fuel oxidizer combination acetylene and air, flame C 2 H N 2 O 2600-2800 temperature of 2400-2700 K. 2 Taken from DAR slides For higher temperature acetylene and nitrous oxide CEE 772 #5b Aarthi Mohan 9/15/2019

  12. Temperature 12 CEE 772 #5b Aarthi Mohan 9/15/2019

  13. 13 Instrument Design CEE 772 #5b Aarthi Mohan 9/15/2019

  14. Transitions 14 CEE 772 #5b Aarthi Mohan 9/15/2019

  15. Graphite AA 15 -Electrically heated -More sensitive than flame, less sample 1-100 μ L -Argon used to prevent oxidation of furnace -Sample injection important (too high, low precision) CEE 772 #5b Aarthi Mohan 9/15/2019

  16. Graphite AA 16 2550 C for not more then 7s Charring Analytical uL of 60s at high signal= Furnace sample temperatur time- Sample heated 3-4 Atomizatio Clean out injected at drying to e to integrated times to n for few by heating remove high destroy absorbance atomize seconds furnace temperatur solvents organic during sample e matter atomizatio (pyrolysis) n Purging with Ar or N2 for every step except atomization to avoid analyte blowout and remove other volatile non-organics

  17. 17 Signals (DAR slide) Analysis of Molybdenum A: uncoated tube B: pyro-coated tube CEE 772 #5b Aarthi Mohan 9/15/2019

  18. 18 18 Manganese (DAR slide)  US SMCL - 50 ug/L  EPA does not enforce "secondary maximum contaminant levels" or "SMCLs." They are established only as guidelines to assist public water systems in managing their drinking water for aesthetic considerations, such as taste, color and odor. These contaminants are not considered to present a risk to human health at the SMCL.  New data suggest neurodevelopmental affects in children at or near the SMCL  Env. Health Persp. 9/15/2019 CEE 772 #5b Aarthi Mohan

  19. 19 CEE 772 #5b Aarthi Mohan 9/15/2019

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