Spectroscopy: Cristian Ryan A. Argamino, RCH., M.SC

SPECTROSCOPY
Cristian Ryan A. Argamino, RCh., M.Sc

Spectroscopy
The study of the interaction of matter and radiated energy
Electromagnetic Spectrum
Jablonski Diagram
Instrumentation
Light Wavelength
Selector
Sample Detector
Source
Comparison of Techniques
Instrument Light Source Wavelength Sample Introduction Detector Application Remarks
Selector
UV-Vis Spectro Deuterium(D2) / Tungsten Czerny-Turner Sample Cell/Cuvette Silicon Metals and Organic
Iodide (WI); (quartz, silicate glass, photodiode; compounds(liquid
Xenon Arc (Xe) plastic) Photomultiplier solution)
tube (PMT)
AAS Hollow Cathode Lamp Czerny -Turner Nebulizer-Flame PMT Metals (liquid Requires gas
(HCL) Atomization or Graphite solution) for flame
Furnace Atomization (acetylene and
air/N2O);
argon for
furnace
Instrument Light Source Wavelength Selector Sample Introduction Detector Application
Spectrofluoro Xenon Arc 2x Concave blazed, Sample Cell/Cuvette (quartz) PMT Organic compounds(liquid
meter holographic grating solution)
(excitation + emission)
FTIR Heat source Michaelson Film, Attenuated Total Reflectance, Pyroelectric, Organic compounds/
(i.e. ceramic) Interferometer Diffuse Reflectance, Liquid Cell, KBr Mercury functional groups (liquid,
pellet Cadmium powder, film, solid)
Telluride (MCT)
Instrument Light Source Monochromator/ Sample Introduction Detector Application Remarks
Interferometer
ICP-AES Plasma Echelle, Paschen Runge Nebulizer -> Plasma PMT, Charged Metals (liquid solution) Requires Ar for
Ionization Couple Device plasma and sample
carrier flow; requires
vacuum pump or
inert gas purge for
spectrometer (i.e. N2)
Ultraviolet-Visible (UV-Vis)
Spectrophotometry
Used to determine the absorption or transmission of UV or Visible light by a
sample
 Can also be used to measure concentrations of absorbing materials based on
calibration curves of the material.
Spectrofluorometry
Measures fluorescent samples
Fluorescence occurs when a fluorescent capable material (fluorophore) is excited
into a higher electronic state by absorbing an incident photon and cannot return
to the ground state except by emitting a photon.
Atomic Absorption Spectrophotometry (AAS)
Determination of elemental metal concentration in a sample through its
electromagnetic spectrum based on atomic absorption
Burner
Monochromator detector
Light
source Reference
Beam Splitter/ Chopper lens slit
Fourier Transform Infrared Spectroscopy
(FTIR)
The study of the interaction of infrared light (heat) with matter
Can identify functional groups in a molecule through the vibration of bonds when
matter reacts with IR radiation
Inductively Coupled Plasma-Atomic Emission
Spectrometry (ICP-AES)
Also called ICP-OES (Optical Emission Spectrometer)
One of the most powerful analytical tools for quantifying or identifying trace
elements
Uses plasma to ionize samples
Can handle sequential or simultaneous elemental analysis
Light Source
Deuterium Lamp
used as light source for the UV Region (190-400 nm)
Tungsten Lamp
used as light source for visible region (400-800 nm)
Xenon Arc Lamp
continuous light source for the UV-Vis region
(can also be applied to spectrofluorometer)
Light Source
Hollow Cathode Lamp
provides analytical line for a specific metal in AAS analysis
Ceramic (heat source)
Provides infrared signal for FTIR
Monochromator
Used to isolate a narrow band of wavelengths
The idea is to have high light intensity at the selected wavelength and
minimum light outside the range.
Forms an image of the entrance slit in the exit plane at the wavelengths
present in the light source
Monochromator
Czerny Turner Monochromator
Polychromator
Rowland Circle (Paschen Runge mounting)
The grating, entrance slit, and focused images of the
diffracted wavelengths are all positioned on the
perimeter of the circle.
Polychromator
Echelle Spectrometer
Provides high efficiency at many wavelengths rather than a
single blaze wavelength
Sample Introduction
Cuvette (UV-Vis and Spectrofluoro)
Flow cell (UV-Vis)
Integrating Sphere (UV-VIs)
Sample Introduction
Atomization Chamber (AAS)
o Flame
o Furnace
Inductively Coupled Plasma (ICP-AES)
Sample Introduction
Transmission Techniques (FTIR)
o KBr Pellets
o Film
o Liquid Cell
o Microscope
Sample Introduction
Reflectance Techniques (FTIR)
o Diffuse Reflectance Spectroscopy
o Attenuated Total Reflectance
o Infrared Microscope
Detector
Silicon photodiode
o These detectors are capable of measuring all elements
of a beam of dispersed radiation simultaneously
Photomultiplier Tube
o Have fast response times.
o Intense light damages photomultipliers
o Limited to measuring low power radiation
o Easily damaged by shock and vibration.
Detector
Pyroelectric
• Deuterated, L-Alanine doped Triglycine Sulfate)
• Excellent S/N Ratio
• Stable
• Short response time
• Wide Range
MCT
• Mercury Cadmium Tellurium
• High sensitivity
• Faster response
• Must be cooled by liquid nitrogen
• Narrow band
Detector
CCD (Charge-Coupled Device) Detector
• Collects both the analyte and background spectra for
simultaneous background correction and improved precision
and analytical speed
• Cooled directly using a single -stage integrated Peltier cooler
operated at approximately -15 °C.

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SPECTROSCOPY

Cristian Ryan A. Argamino, RCh., M.Sc

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