Barium
Basic Theory
Basics cont
modern equipment uses a slightly different set up:-
A diffraction grating is used to produce the spectrum and mirrors focus the radiation onto detectors. Analytical Workshop 2012
Emission Spectra
In the case of optical emission spectroscopy the EM radiation is in the visible\optical region of the EMS which we see as different colours depending on the wavelength\energy of the emitted photon.
The energy of a photon and its wavelength are related by the following equation:-
E = hc
Analytical Workshop 2012
where h is Planck's constant (6.626 10-34 joules) and c is the speed of light (2.998 108 m/s).
Emission spectrum of H
Emission spectrum of Fe
The System
Sample sparked to produce a burn Polychromatic light Emitted Light
Computer
Calculation of results Comparison to Standards Data output and storage
130 800 nm Grating The incoming light is reflected and diffracted, producing the spectrum
Entrance Slit
130 800 nm
The CCD chips simultaneously detect all incident light and determine the intensity of each wavelength. Analytical Workshop 2012
The Sample
Generally speaking the sample is metallic, flat and freshly ground. The sample is clamped in place and sparked to generate a spectrum this leaves burn marks on the sample:-
Burn marks
Sample
If the sample does not burn correctly spurious results can be produced. Poor burning can be caused by poor grinding and rough\uneven surfaces.
Analysis
The Intensity of an emission line (colour) is proportional to concentration allows measurement of how much of each element is present. A number of standards are run first to set up a calibration curve, these take into account any matrix matching difficulties (i.e. overlap of elements in some materials). Take the example of Fe Requires six standards to correctly calibrate the instrument for Fe analysis.
Analysis Continued
Once calibration is completed numerous samples can be analysed. The sample is simply clamped into place, sparked and a spectrum collected. The spectrometer collects the intensity of light at all wavelengths and compares this to the values for the calibration standard. This gives an accurate value of the elements present in the sample. Multiple sparks are collected until concordant results are obtained within an acceptable standard deviation. Further samples of the same alloy type can then be analysed. Different alloys require re-calibration before analysis can occur.
System Types
Spark Optical Emission Spectrometers come in all shapes and sizes for a multitude of uses. Foundry\steel making applications usually floor standing to analyse composition of metals during production quality control. Portable units often used in manufacturing plants to assess metal composition. Portable units to analyse large immovable materials Hand held units to assist in scrap sorting The smaller the unit the less accuracy In the measurements so convenience over quality still useful as analysis can be Performed anywhere.