1. Chapter 10 Atomic Emission Spectrometry

2. 10A EMISSION SPECTROSCOPY BASED ON PLASMA SOURCES

3. Inductively coupled plasma (ICP)
Direct current plasma (DCP)
Microwave induced plasma (MIP)

4. 10A-1 The Inductivity Coupled Plasma Source

5. FIGURE 10-1 A typical ICP source. Position A shows radial viewing of
the torch, and position B
shows axial viewing.

9. Sample introduction

10. FIGURE 10-2 The Meinhard nebulizer. The nebulizing gas flows
through an opening that surrounds the capillary concentrically. This
causes a reduced pressure at the tip and aspiration of the sample.
The high-velocity gas at the tip breaks up the solution into a mist.

11. Plasma Appearance and Spectra
Analyte Atomization and Ionization

12. FIGURE 10-3 Device for electrothermal vaporization.

13. FIGURE 10-4
Temperatures in
a typical ICP
course.

14. 10A-2 The Direct Current Plasma Source

15. FIGURE 10-5
A three-electrode DC plasma jet.

16. 10A-3 Plasma Source
Spectrometers

17. Instruments for emission spectroscopy are of three
basic types: sequential, simultaneous multichannel, and
Fourier transform.

18. TABLE 10-1 Desirable Properties of an Emission Spectrometer

19. Sequential Instruments
Slew-Scan Spectrometers
Scanning Echelle Spectrometers

20. FIGURE 10-6 Optical diagram of a sequential ICP optical emission spectrometer. All
moving parts are under computer control, and their modes of motion are indicated by
the three-dimensional arrow. Moving parts include the grating, a mirror for transducer
selection, a refractor plate for optimizing signal throughput, and a viewing mirror to
optimize the plasma viewing position. The spectrometer contains a mercury lamp for
automatic wavelength calibration. Notice the axial viewing geometry.

22. FIGURE 10-7 Schematic of an echelle spectrograph system.

23. Multichannel Spectrometers
Polychromators.

24. FIGURE 10-8 Direct- reading ICP emission spectrometer. The
polychromator is of the
Paschen-Runge design.
It features a concave
grating and produces a
spectrum around a
Rowland circle.
Separate exit slits
isolate each spectral line,
and a separate
photomulitiplier tube
converts the optical
information from each
channel into an electrical
signal. Notice the radial
viewing geometry. PMT=
photomultiplier tube.

25. ICP-AES

26. A Charge-Injection Device Instrument

27. FIGURE 10-9 Optical diagram of an echelle spectrometer
with a charge-injection detector.

28. FIGURE 10-10

29. FIGURE 10-10(a) Schematic representing the surface of a CID. The short
horizontal lines represent the read windows. A magnified image of one of
the read windows is also shown. The nine central elements form the
examination window, where a line is positioned.

30. FIGURE 10-10(b)
Intensity profile for an iron
line. All of the radiation
from the line falls on the
3 × 3 examination window.

31. A Charge-Coupled Device Instrument
A Combination Instrument

32. FIGURE 10-11 An echelle spectrometer with segmented
array of CCDs.

33. FIGURE 10-12 Schematic of an array segment showing
phototransducers, storage and output registers, and readout
circuitry.

34. Fourier Transform Spectrometers
Fourier, Joseph

35. 10A-4 Applications of Plasma Sources

36. Sample Preparation
Elements Determined

37. Line Selection
Calibration Curves

38. FIGURE 10-13 Periodic table characterizing the detection power and number of
useful emission lines of ICP by using a pneumatic nebulizer. The color and degree of
shading indicate the range of detection limits for the useful lines. The area of
shading indicates the number of useful lines.

39. FIGURE 10-14 Typical calibration curves in ICP emission
spectrometry.

40. FIGURE 10-15 Internal standard calibration curves with an ICP
source. Here, an yttrium
line at nm served
as an internal standard.
Notice the lack of
interelement
interference.

41. Interferences
Detection Limits

43. 10B EMISSION SPECTROSCOPY BASED ON ARC AND SPARK SOURCES

44. These spectra permitted the qualitative and quantitative determination of metallic elements in
a variety of sample types, including metals and alloys,
soils, minerals, and rocks,

45. TABLE 10-2 Effect of Standardization Frequency on Precision of ICP Data

46. 10B-1 Sample Types and Sample Handling

47. Metals
Nonmetallic Solids

48. TABLE 10-3 Comparison of Detection Limits for Several Atomic spectral Methods

49. FIGURE 10-16 Some typical graphite electrode shapes.
Narrow necks are to reduce thermal conductivity.

50. 10B-2 Instruments for Arc and
Spark Source Spectroscopy

51. Spectrographs

52. FIGRUE 10-17 The Eagle mounting for a grating spectrograph.

53. Multichannel Photoelectric Spectrometers
Multichannel Photomultiplier Instruments.
Array-Based Multichannel Instruments.

54. 10B-3 Arc Source Emission Spectroscopy

55. Characteristics of Arc Sources
Cyanogen Spectral Bands.
Rates or Emission.

56. Applications of Arc Sources

59. 10B-4 Spark Sources and Spark Spectra

60. Applications of Spark Source Spectroscopy

61. 10C MISCELLANEOUS SOURCES FOR OPTICAL EMISSION SPECTROSCOPY

62. 10C-1 Flame Emission Sources

63. 10C-2 Glow-Discharge Sources

64. 10C-3 Laser Microprobe Sources