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UV spectroscopy
UV spectroscopy is a type of absorption spectroscopy where UV lights are
absorbed by the electrons that causes them to excite to a high energy state.
Principle of UV spectroscopy
In UV spectroscopy, the UV rays passed to the sample are absorbed by the
electrons, which increases the energy of the system.
This causes the excitation of an electron from a lower energy state to a higher
energy state.
This excitation forms an absorption spectrum that can be detected by the
detectors in the spectrometer.
The amount of photon (radiation) absorbed results in an absorption spectrum
which can then be measured in terms of absorbance.
The absorbance of a sample is dependent on the number of excited electrons
which in turn is dependent on the concentration of molecules in the sample.
Steps of UV spectroscopy
Two samples of known and unknown concentrations are taken in a transport
vessel, also termed as a cuvette.
The vessels are then placed, one after the other, in the spectrophotometer
that is provided with light source and detectors.
The spectrophotometer is operated that passes light of a particular
wavelength through the sample.
The photosensitive detectors present in the spectrophotometer detect the
light passing through the sample, which is then converted into digital values.
A graph of the absorbance measured against the concentration of the sample
is plotted, which can then be used for the determination of the unknown
concentration of the sample.
Uses of UV spectroscopy
UV spectroscopy is a technique used for the detection of impurities in organic
substances.
This can also be used for the quantitative determination of compounds that
can absorb UV radiation.
It can also be used for the study of the kinetics of a reaction where the UV
rays are passed through the reaction cell, and the changes in absorbance are
studied.
21. Ultraviolet and visible (UV/Vis) spectroscopy
Ultraviolet and visible spectroscopy is an absorption spectroscopy technique
which uses the radiation in the UV range and the adjacent visible range of the
electromagnetic radiation.
Principle of UV/Vis spectroscopy
UV/Vis spectroscopy is based on the principle that materials produce an
absorption spectrum which is a range of absorbance resulting from the
radiation absorbed by the material at different frequencies.
The absorption spectrum of materials depends on the atomic and molecular
composition of that material.
The frequency of light radiation absorbed by a material is dependent on the
energy difference between the two energy states of the molecules.
The absorption results in the formation of the absorption line, which, together
with other lines, form an absorption spectrum.
The incident light in this spectrometer is in the range of UV and visible
spectrum of the electromagnetic spectrum.
Thus, when a photon with sufficient energy reaches an object, the energy is
absorbed by the electrons causing them to bump into a higher energy state.
The amount of photon (radiation) absorbed results in an absorption spectrum
which can then be measured in terms of absorbance.
The absorbance of a sample is dependent on the number of excited electrons
which in turn is dependent on the concentration of molecules in the sample.
Steps of UV/Vis spectroscopy
Solvent liquid and the sample solution are taken in two transport vessels, also
termed as cuvettes.
The vessel with solvent liquid is then placed in the spectrometer to determine
the light loss due to scattering and absorbance by the solvent. Any
absorbance observed in this process is to be subtracted from the absorbance
of the sample.
The cuvette with the sample solution is then placed in the spectrometer.
The absorbance of the sample is noted in different frequencies which usually
ranges from 200-800 nm.
A similar spectrum is formed from the different concentrations of the
samples.
A graph of the absorbance measured against the concentration of the sample
is plotted, which can then be used for the determination of the unknown
concentration of the sample.
Uses of UV/Vis spectroscopy
Qualitative analysis may be performed in the UV/Vis regions to identify
certain classes (proteins and nucleic acids) of compounds both in the pure
state and in biological mixtures.
This type of spectroscopy is used for the quantification of biological samples
either directly or via colorimetric assays.
22. X-ray photoelectron spectroscopy
X-ray photoelectron spectroscopy is a sensitive, quantitative spectroscopic
technique based on the photoelectric effect used for the identification of
electrons inside a compound, on the surface as well as the chemical state and the
electronic configuration of the compound.
Principle of X-ray photoelectron spectroscopy
Photoelectron spectroscopy utilizes the principle of the photoelectric effect.
The sample is exposed to X-rays with specific wavelengths that induce
photoionization of the substances.
The emitted photoelectrons have energies that are characteristic of their
original energy states and the vibrational and rotational level of the electrons.
The energy of these electrons is used to determine the binding energy of the
electrons in the atoms by the given formula:
BE= hν- KE where hν is the incident radiation, and KE is the energy of the emitted
photoelectrons.
A graph of BE against KE is then plotted.
The peaks in the spectrum indicate the electrons in different subshells of an
atom. The lowest peaks indicate the valence electrons, whereas the highest
peaks correspond to the core electrons.
Steps of X-ray photoelectron spectroscopy
The sample is placed in the spectrometer, which is exposed to the ionizing
radiation from the radiation source.
The emitted electrons strike the detectors, which then converts the energy
into an electric signal.
The signal is transferred to the analyzer to obtain the analog data from the
signal.
Then a graph is plotted of the kinetic energy of the emitted electrons and the
binding energy.
Based on the peaks formed in the graph, the unknown element can be
detected.
Uses of X-ray photoelectron spectroscopy
X-ray photoelectron spectroscopy is commonly used for the measurement of
composition, chemical state, and electronic configuration of various organic
and inorganic substances.
This also assists in the surface analysis of various compounds.
References
X-Ray Spectroscopy- Principle, Instrumentation and
Applications
December 22, 2018 by Sagar Aryal
Table of Contents
Principle of X-Ray Spectroscopy
Working of X-Ray Spectroscopy
Instrumentation of X-Ray Spectroscopy
Applications of X-Ray Spectroscopy
Advantages of X-Ray Spectroscopy
Limitations of X-Ray Spectroscopy
References
X-rays make up X-radiation, a form of electromagnetic radiation.
Most X-rays have a wavelength ranging from 0.01 to 10 nanometers,
corresponding to frequencies in the range 30 petahertz to
30 exahertz (3×1016 Hz to 3×1019 Hz) and energies in the range 100 eV to
100 keV, produced by the deceleration of high-energy electrons.
X-ray spectroscopy is a general term for several spectroscopic techniques for
characterization of materials by using x-ray excitation.
Source: University College Cork
Principle of X-Ray Spectroscopy
XRF works on methods involving interactions between electron beams and x-
rays with samples.
It is made possible by the behavior of atoms when they interact with
radiation.
When materials are excited with high-energy, short wavelength radiation (e.g.,
X-rays), they can become ionized.
When an electron from the inner shell of an atom is excited by the energy of
a photon, it moves to a higher energy level.
When it returns to the low energy level, the energy which it previously gained
by the excitation is emitted as a photon which has a wavelength that is
characteristic for the element (there could be several characteristic
wavelengths per element).
Thus atomic X-rays emitted during electronic transitions to the inner shell
states in atoms of modest atomic number.
These X-rays since have characteristic energies related to the atomic number,
and each element therefore has a characteristic X-ray spectrum which can be
used to identify the element.
Working of X-Ray Spectroscopy
1. An XRF spectrometer works because if a sample is illuminated by an intense
X-ray beam, known as the incident beam, some of the energy is scattered, but
some is also absorbed within the sample in a manner that depends on its
chemistry.
2. The incident X-ray beam is typically produced from a Rh target, although W,
Mo, Cr and others can also be used, depending on the application.
3. When x-ray hits sample, the sample emits x-rays along a spectrum of
wavelengths characteristic of the type of atoms present.
4. If a sample has many elements present, the use of a Wavelength Dispersive
Spectrometer allows the separation of a complex emitted X-ray spectrum into
characteristic wavelengths for each element present.
5. Various types of detectors used to measure intensity of emitted radiation.
6. The intensity of the energy measured by these detectors is proportional to
the abundance of the element in the sample.
7. The exact value for each element is derived from standards from prior
analyses from other techniques.
Instrumentation of X-Ray Spectroscopy
Components for X-ray spectroscopy are:
1. X-ray generating equipment (X-ray tube)
2. Collimator
3. Monochromators
4. Detectors
A. X-ray generating equipment (X-ray tube)
X-rays can be generated by an X-ray tube.
X-rays tube is a vacuum tube that uses a high voltage to accelerate the
electrons released by a hot cathode to a high velocity.
The high velocity electrons collide with a metal target, the anode, creating the
X-rays.
B. Collimators
A collimator is a device that narrows a beam of particles or waves.
Narrow mean to cause the directions of motion to become more aligned in a
specific direction (i.e., collimated or parallel).
Collimation is achieved by using a series of closely spaced ,parallel metal
plates or by a bundle of tubes ,0.5 or less in diameter.
C. Monochromator
Monochromator crystals partially polarize an unpolarized X-ray beam.
The main goal of a monochromator is to separate and transmit a narrow
portion of the optical signal chosen from a wider range of wavelengths
available at the input.
Types of Monochromator