Recogida de contenedores de superficie y soterrados

Infrared spectroscopy is the study of the identification of chemical compounds observing how infrared radiation is absorbed by the chemical bonds within the compounds [67]. When applied to a molecule, infrared radiation encourages transitions between vibrational and rotational energy levels of the ground (lowest) electronic energy state [21]. Atoms in molecules are constantly vibrating with respect to one another. This happens as long as the temperature of the molecule is above zero [68]. When infrared radiation is directed on a molecule, and the frequency of a specific vibration is equal to the frequency of the infra-red radiation, the molecule absorbs the radiation. This absorption will be represented on the infrared spectrum as a peak [22].

There are two types of vibration modes; the stretching and the bond vibration modes. When infrared radiation is absorbed, the energy associated with the absorption is converted to either of the vibration modes [22]. The only vibration that can occur in a simple diatomic molecule A-B is the periodic stretching along the A-B bond [21]. A stretching vibration resembles the to and fro movements of two bodies which are connected by a spring. The vibrational frequency υ (cm-1) required to stretch a bond A- B is given by the equation

ν= c π 2 1 (

µ

Where f is the force constant of the bond, µ is the reduced mass of the system, and c is the velocity of light. µ is defined by the equation below.

µ= B A B A m m m m + 3.17

Where mA and mB are the individual masses of A and B.

Bond vibrations modes are divided into two types:- the stretching and the deformation (bending) vibrations. As defined earlier, the stretching vibration is the periodic stretching of the bond A-B along the bond axis [21]. Bending vibrations are

displacements which occur at right angles to the bond axis of the bond A-B. Stretching and deformation vibration frequencies are differentiated by spectroscopists using the symbols ν and δ. τ is used to symbolize twisting vibration frequencies and π for out –of- plane deformation.

Each atom has three degrees of freedom. This corresponds to motions along any of the three Cartesian coordinate axes (x, y, z) [22]. A molecule containing n number of atoms which is non-linear will have 3n degrees of freedom. These degrees of freedom are distributed as 3 rotational, 3 translational, and 3n-6 vibrational motions. Each motion has a distinctive fundamental band frequency [21]. When a molecule is exposed to infrared radiation, and the dipolar character of the molecule changes, it is only then that absorption will occur. Total symmetry about a bond will eliminate certain absorption bands. It has been confirmed by spectrocopists that specific absorption bands for particular bonds or groups occur within a molecule at or around the expected frequencies [21].

Figure 3.19 Stretching and Bending vibration modes [21].

Wavenumbers (ν) or wavelengths (λ) are usually used to represent infra-red absorption. Wavenumbers define the number of waves per unit length, and they are directly proportional the energy of the infra-red absorption, and also the frequency [22]

When a specimen is exposed to infrared radiation, radiant power is transmitted by the sample [22]. The ratio of this radiant power transmitted by the sample to the radiant power incident (I0) on the sample is known as the transmittance T, If the value of the

transmittance is reciprocated, and its logarithm of base 10 is taken, we will get the absorbance(A) [68]. The transmittance spectrum ranges from 0 to 100% T, while the range of absorbance spectra is from infinity to zero. As a result, the transmittance spectrum provides a better contrast between the intensities of strong and weak bands [25].

3.5.1 Uses of Infra-red Spectroscopy

The primary aim of infra-red spectroscopy is the determination of functional groups in the sample [22]. Other uses of infra-red spectroscopy are;

i) Identifying all types of organic compounds. Compounds can be identified by matching the spectrum of the unknown compound with a reference spectrum.

ii) Identification of many inorganic compounds.

iii) It is used to determine the molecular composition of surfaces.

iv) Chromatographic effluents can be identified using infra-red spectroscopy.

v) The molecular orientation of polymers and solutions can be determined using infra-red spectroscopy [22].

vi) It is used for the determination of purity, production control, and quantitative analysis.

vii) Reaction kinetic studies.

Two types of instruments are generally used for recording infrared spectra. They are the Fourier Transform Infrared spectrometer (FT-IR), and the classical dispersive spectrometer. Most modern instruments are of the Fourier Transform Infrared Spectrometer type. This is because the FT-IR has several advantages over the classical dispersive spectrometer; some of which are having the ability to record complete spectra in a much shorter timescale [69]. FT-IR also has better signal-to-noise ratios. The figure 3.15 shows the basic construction of the FT-IR spectrometer

Figure 3.20 Schematic Diagram of the FT-IR spectrometer [70].

The infrared radiation is generated from a source; which is usually a globar or a Nernst filament. This generated infrared radiation passes into the Michelson interferometer. The interferometer consists of two mirrors which are at 90 degrees to each other. It also consists of a beam splitter which is at an angle of 45 degrees to both mirrors. One

Mirror drive Piston Mirror B (movable) Mirror A (fixed) Source Beam splitter Combined beam Sample cell Detector

Analog to digital convertor

The beam splitter partially transmits and partially reflects the beam. The transmitted and the reflected beams are incident normal to the two mirrors and after reflection, they recombine at the beam splitter, and there they produce interference effect. When the optical path difference is an integral number of wavelengths, the reflected beams are in phase and hence produce constructive interference. In contrast, when the optical path is an odd number of half wavelengths, then destructive interference will occur. This will result in an oscillalatory pattern or interferogram, which represents the spectral distribution of the absorption signal. Fourier transformation derives the true absorption spectrum from the interferogram [70].

A Thermo Nicolet 5700 FT-IR spectrometer with single bounce Diamond ATR crystal was used for this study. KBR discs were used for measuring the infrared spectra of the uncured Araldite DLS 772 / 4 4’DDS and Araldite LY 5052 / 4 4’ DDS epoxy systems in order to prevent the resin from sticking to the sampling plate. The microwave cured samples were broken into pieces and a few pieces were extracted and placed on the sampling plate for infrared measurements. Infrared spectroscopy was taken using the Attenuated Total Reflectance (ATR) method. DSC pans were used to conventionally cure the samples in an oven, and the single point diamond FT-IR was used to take the infrared spectra via the ATR method.