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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