Instruments for Optical Spectrometry

Instrument components Most spectroscopic instruments for use in the UV/Visible and IR regions are made up of 5 components: 1. a stable source of radiant energy 2. a wavelength selector that isolates a limited region of the spectrum for measurement 3. one or more sample containers 4. a radiation detector, which converts radiant energy to a measurable electrical signal 5. a signal processing and readout unit Optical materials The cells, windows, lenses, mirrors, and wavelength-selecting elements in an optical spectroscopic instrument must transmit radiation in the wavelength region being investigated. Ordinary silicate glass is completely adequate for use in the visible region and has the considerable advantage of low cost. In the UV region at wavelengths shorter than about 380 nm, glass begins to absorb, and fused silica or quartz must be substituted. Also, in the IR region, glass, quartz, and fused silica all absorb at wavelengths longer than 2.5 m. Hence, optical elements for IR spectrometry are typically made from halide salts or, in some cases, polymeric materials. Spectroscopic Sources A source must generate a beam of radiation that is sufficiently powerful to allow easy detection and measurement. The output power should be stable for reasonable periods of time. A well-regulated power supply must provide electrical power for the source. Spectroscopic sources are of only two types: 1. Continuum sources which emit radiation that changes in intensity only slowly as a function of wavelength. 2. Line sources emit a limited number of spectral lines, each of which spans a very limited wavelength range. A continuum source provides a broad distribution of wavelengths within a particular spectral range. This distribution is known as a spectral continuum. Sources can also be classified as continuous sources, which emit radiation continuously with time, or pulsed sources, which emit radiation in bursts. Continuum Sources in the UV/Visible Region Skoog, West et al, Fundamentals of analytical chemistry, 8th ed, ISBN-13: 978-0-03-035523-3

An ordinary tungsten filament lamp provides a distribution of wavelengths from 320 to 2500 nm. Generally, these lamps are operated at a temperature of around 2900K, which produces useful radiation from about 350 to 2200 nm. Tungsten/halogen lamps, also called quartz/halogen lamps, contain a small amount of iodine within the quartz envelope that houses the filament. Quartz allows the filament to be operated at a temperature of about 3500K, which leads to higher intensities and extends the range of the lamp well into the UV region. These lamps are finding ever-increasing use in modern spectroscopic instruments because of their 1. extended wavelength range 2. greater intensity 3. longer life

Illustration 1: A close up of a halogen lamp

Deuterium (and also hydrogen lamps) Most often used to provide continuum radiation in the UV region. A deuterium lamp consists of a cylindrical tube containing deuterium at low pressure, with a quartz window from which the radiation exits. Other Ultraviolet/Visible Sources Low-pressure mercury arc lamps are very common sources that are used in liquid chromatography detectors. The dominant line emitted by these sources Illustration 2: is the 253.7 nm Hg line. Deuterium lamp Hollow-cathode lamps are also common line sources that are specifically used for atomic absorption spectroscopy. Continuum Sources in the Infrafred region The continuum sources for IR radiation are normally heated inert solids. A Globar source is a silicon carbide rod; infrared radiation is emitted when the Globar is heated to about 1500 C by the passage of electricity. A Nernst glower is a cylinder of zirconium and yttrium oxides that emits IR radiation when heated to a high temperature by an electric current. Electrically heated spirals of nichrome wire also serve as inexpensive IR sources.

Skoog, West et al, Fundamentals of analytical chemistry, 8th ed, ISBN-13: 978-0-03-035523-3