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Chapter: Modern Analytical Chemistry: Spectroscopic Methods of Analysis

Spectroscopic Methods of Analysis

Before the beginning of the twentieth century most quantitative chemical analyses used gravimetry or titrimetry as the analytical method.

Spectroscopic Methods of Analysis

Before the beginning of the twentieth century most quantitative chemical analyses used gravimetry or titrimetry as the analytical method.

With these methods, analysts achieved highly accurate results, but were usually limited to the analysis of major and minor analytes. Other methods developed during this period extended quantitative analysis to include trace level analytes. One such method was colorimetry.

One example of an early colorimetric analysis is Nessler’s method for ammonia, which was first proposed in 1856. Nessler found that adding an alkaline solution of HgI2 and KI to a dilute solution of ammonia produced a yellow to reddish brown colloid with the color determined by the concentration of ammonia. A comparison of the sample’s color to that for a series of standards was used to determine the concentration of ammonia. Equal volumes of the sample and standards were transferred to a set of tubes with flat bottoms. The tubes were placed in a rack equipped at the bottom with a reflecting surface, allowing light to pass through the solution. The colors of the samples and standards were compared by looking down through the solutions. Until recently, a modified form of this method was listed as a standard method for the analysis of ammonia in water and wastewater.

Colorimetry, in which a sample absorbs visible light, is one example of a spectroscopic method of analysis. At the end of the nineteenth century, spectroscopy was limited to the absorption, emission, and scattering of visible, ultraviolet, and infrared electromagnetic radiation. During the twentieth century, spectroscopy has been extended to include other forms of electromagnetic radiation (photon spectroscopy), such as X-rays, microwaves, and radio waves, as well as energetic particles (particle spectroscopy), such as electrons and ions.

 

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