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Atomic emission spectroscopy


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Atomic emission spectroscopy

  3. 3. • Used as standard method for the metal analysis • In atomic emission small part of sample is vaporized forms free atom that attain energy form excitation source results in transition from lower to higher energy state on returning back emit a photon of radiation
  4. 4. • Ancient: atomic emission was only based on flame , arc or spark excitation sources. • Modern era: advancement is made by the introduction of non combustion plasma sources
  5. 5. • Consist of discrete irregularly spaced lines • Spectra obtained from plasma ,arc or spark excitation source are often highly complex
  7. 7. Principle • The electrons of an atom moves from higher energy level to lower energy level, they emit extra amount of energy in the form of light which is consist of photons.
  8. 8. Instrumentation Comprises on: • Source & Sample • Atomizer • Monochromator • Detector & readout device
  9. 9. Schematic Diagram Of Instrumentation
  10. 10. Spectra
  11. 11. COMPONENTS 1. Light source a. Inductively coupled plasma (ICP) b. Direct current plasma (DCP) c. Flame d. Arc and spark BY GHOUSIAAROOJ (1416984)
  12. 12. Plasma Source “ Plasma is defined as a neutral gas containing significant number of both positive and negative ions or free electrons”
  13. 13. Mechanism Of Inductively Coupled Plasma • The inductively coupled plasma torch consist of 3 concentric silica quartz tube. • Argon stream that carries the sample in the form of an aerosol, passes through the central tube. • Plasma is initiated by a spark from a tesla coil. Argon gas ionized and emission is measured.
  14. 14. Flame Source Mechanism: • It consist of total consumption burner in which sample is drawn through a capillary tube which injected directly into flame and flame is high temperature source that is used to desolvate and vaporize a sample and generate free atom for spectroscopic study.
  15. 15. Spark source Mechanism: • It consist of the primary circuit a voltage of 110-220V is maintained. The high voltage is obtained from setup transformer which convert the line power to 15000-40000V which then charge the capacitor. When energy stored in the capacitor, synchronous trigger the spark between the electrodes.
  16. 16. Continue Light source e. Arc and spark f. Laser induced breakdown g. Laser induced plasma h. Microwave induced plasma BY HIRA BILAL (1416992)
  17. 17. Arc Discharge DC ARC AC ARC • Used for quantative analysis. • Also used for quantative analysis. • Source is regulate supply is 110 to 220 V(tem p 4000 t0 8000K). • In this alteration at a frequency of 60 HZ (2000 to 5oooV) that maintain by transformer. • When the sample (solid and liquid ) is kept on the lower electrode in the arc gap then start the current flow in the gap & electrical arced is established which responsible excitation. • Once arc is picks out in the gap, current flow start which arced the sample and create excitation. • Graphite electrodes is used and Less sensitive. • More sensitive.
  18. 18. Laser Induced Plasma • In this source highly energetic laser pulse used to generated optical sample excitation. • When laser beam focused on the small spot on a sample(liquid, solid and gases). • The temperature of heated region is rise rapidly that vaporized the sample material & induced plasma formed . • vaporized material excited & emit radiation.
  19. 19. Laser Beam Excitation
  20. 20. Microwave Induced Plasma • Used for multi-analytic determination of major to minor elements. • Employed microwave energy to produced plasma. • MIP generated from few hundred watts of radiation source • Atomized sample pass through plasma & promote electron excitation .
  22. 22. Atomizer • Elements to be analyzed needs to be in atomic state. • Atomization; Conversion of sample (maybe; solid or liquid) into free gaseous atom. • Atomizer; Device used for atomization
  24. 24. 1. Flame Atomizer • To produce flame, required oxidant gas and flame gas. • Mostly the air-acetylene flame or nitrous oxide- acetylene flame is used. • Liquid or dissolved samples are typically used with flame atomizer.
  25. 25. Flame Atomization
  26. 26. Sub-types Of Flame Atomization a. Continuous Atomization; sample penetrate the atomizer at constant speed. a. not used for dissolved solid.* b. Discrete Atomization; measured amount of sample enters atomizer. –effective when sample volume is limited.
  27. 27. Advantages; • Reproducibility of sample and result. Disadvantages; • Only 5-15% of the nebulized sample reaches the flame. • A minimum sample volume of 0.5-1.0 ml is needed to give a reliable reading. • Viscous samples require dilution with a solvent.
  28. 28. 2. Electro-thermal Atomizer • Also known as “Graphite Furnace Atomizer” • More convenient to uses a non-flame method i.e. electrically heated graphite tube.
  29. 29. Construction • Serves as a sample cellGraphite Tube • Metal jacket by which the water is circulated Enclosed Water Cooled Housing • Made of quartz allow light to pass through the tube Transparent Window • Protect graphite tube from oxidation Inert Pure Gas Control • Heating of graphite tubeElectrical Contact
  30. 30. Atomization Of Sample DRYING • drying of sample into solid deposit. • by heating graphite tube at 110 ºC. ASHING • conversion of organic matter in CO2 and H2O &volatilization of inorganic matter. • by heating graphite tube at 350-1200 ºC. ATOMIZATION • leads to gaseous atom • by raising the temperature up to 2000-3000 ºC.
  31. 31. Advantages; • Small sample size • Little or no sample preparation required • Enhanced sensitivity • Direct analysis of solid samples Disadvantages; • Loss of analyte during ashing stage • Incomplete atomization
  32. 32. Sample Handling • The droplets of sample introduced in atomizer should be of constant size. • The temperature should be maintained to obtain good reproducibility. • The speed of introducing sample must be equal to certain permissible band values. • Sufficient sample volume should be available for maximum efficiency
  33. 33. MONOCROMATORS a. Prism b. Diffraction grating UROOSA FATIMA (1417050)
  34. 34. Monochromator • It is a device use to transmit narrow band of wavelength which is chosen from wavelength of wider range available. • Types of monochromator: • Prism Monochromator • Grating Monochromator
  35. 35. a. Prism • When the light pass through prism it emerges out in form of two lines or beam. • To overcome this drawback two half prism are placed. • When light pass through first prism it splits into two beams, when it reaches second half prism recombines two beam into single beam
  36. 36. b. Diffraction grating • It gives better result and resolution. • It replaced prism give linear dispersion. • Problem occurred during the identification of wavelength of emission lines on photographic plate solved through grating monochromator. • Once we identify known reference line and other lines identified automatically.
  37. 37. DETECTORS BY NIMRAAZHER (1417024)
  38. 38. Phototube (Photo Electric Cell) • Glass filled or vacuum tube • Sensitive to light • Depend on frequency and intensity of incoming photon • Need amplifier. But are replaced by photomultiplier detectors.
  39. 39. Photo Multiplier Detector • Vacuum phototubes, are extremely sensitive detectors of light in the ultra violet, visible, and near-infrared region ranges of the electromagnetic spectrum.
  41. 41. Atomic Emission Spectrometers • Sensitivity is limited by noise. • High luminosity and high resolution monochromators necessary to isolate spectral lines. • Concave and plane grating use as dispersive element. • Echelle grating system use for high resolution spectrograph.
  42. 42. Concave Grating • Use for non scanning multi elements. • Entrance and exit slit mounted on a Rowland circle. • Secondary optics consist of mirror behind exit slit. • Exit slit only pass spectral wavelengths.
  43. 43. • Large wavelengths cover by Paschen- Runge mounting. • To illuminate concave grating Wadsworth mounting commonly use.
  44. 44. Plane Grating • It is mostly use in AES instruments. • Grating serve as dispersive element. • Ebert mounting is use in large spectrometers in which plane grating present. • Standard grating has 600-1200lines/mm. • Current AES has plane grating scanning monochromators have 1500 lines/mm.
  45. 45. Echelle Grating • Provide excellent dispersion and resolution. • Longest wavelength of lowest order appear at bottom higher order at top. • Two dimension permits high dispersion as compare to one dimension. • Spectral interference eliminated by echelle grating.
  46. 46. • Spectral interference eliminated by echelle grating. • Special camera attach to instrument and they provide widespread application of multi element analysis.
  48. 48. Applications • It is used for rapid analysis of multi-component pharmaceutical tablet. • It is used for elemental analysis. • It is used primarily for the identification and determination of metals in traces amount.
  49. 49. • It is used for determination of mineral composition of igeous and metamorphic rock. • It is used for routine analysis of wear metals in lubricating oils. • It is used for the analysis of sodium, potassium and lithium.
  50. 50. CONCLUSION • Introduction • Principle • Instrumentation • Spectrometers • Applications SOOFIA BINT-E IRFAN (1417042)