Analytical Method Flashcards
4 BASIC DISCIPLINES: ANALYTICAL
CHEMISTRY
Spectrometry = spectrophotometry, atomic absorption, and mass spectrometry
Luminescence = fluorescence, chemiluminescence, and nephelometry
Electroanalytic methods = electrophoresis, potentiometry, and amperometry
Chromatography = gas, liquid, and thin- layer
MEASUREMENTS OF RADIANT ENERGY
+ Emitted
+ Transmitted
+ Absorbed
+ Scattered
+ Reflected
There are two primary considerations in
every colorimetric analysis:
- Quality of the color
- Intensity of the color
COLORIMETRY 2 types
a. Visual Colorimetry
b. Photoelectric Colorimetry -
The primary analytical utility of spectrophotometry or filter
photometry is the isolation of discreet portions
of the spectrum for purposes of measurement.
Photoelectric Colorimetry
2 types: photoelectric measurement
Spectrophotometric measurement
Photometric measurement
light intensity in a narrower wavelength
Spectrophotometric measurement
light intensity at multiple wavelengths.
Photometric measurement
transmitted via electromagnetic waves that
are characterized by their frequency and Wavelength
Energy
distance between two successive
peaks and it is expressed in terms of nanometer (n)
Wavelength
Wavelength of visible spectrum
400-700m
Wavelength of ultraviolet (UV)
<400nm
Wavelength of infrared region (IR)
> 700nm
What is the Planck’s formula:
E = hv
E means
energy of a photon in Joules or constant (6.626
x 10^27 erg sec)
V means
frequency
number of vibrations of
wave motion per second
Frequency
Wave frequency: lower
Wavelength:
Longer
Wave frequency:
Wavelength: shorter
Higher
TYPES OF RADIANT ENERGY
+ Cosmic rays
+ Gamma rays
+ X-rays
+ Visible
+ Ultra-violet (UV)
+ Infrared (IR)
+ Radio, TV, microwave, etc.
measurement of the light transmitted ; determine the concentration
Spectrophotometer
concentration of a substance is directly
proportional to the amount of the light absorbed or inversely proportional
BEER’S LAW/ BEER-LAMBERT’S-LAW
ratio of the radiant energy transmitted
Transmittance
amount of light absorbed
Absorbance
Absorbance Mathematically derived from ________
%T
A means
Absorbance
a means
Molar absorptivity
b means
Length of light (solution)
c means
concentration of absorbing (solution)
2 types of Spectrophotometer
Single beam spectrophotometer
Double-beam spectrophotometer
• simplest type of absorption spectrometer
• one measurement at a time at one specified wavelength.
• single-beam instrument is used.
Single beam spectrophotometer
• splits the monochromatic light into two components
• additional beam
• recorded directly as the electrical output
Double beam spectrophotometer
2 Types of Double-beam
Spectrophotometer:
Double beam in space
Double beam in time
2 photodetectors; sample beam and reference beam
Double beam in space
one photodetector; sample of cuvet and sample of reference
Double beam in time
7 basic components of single or double-
beam configuration spectrophotometer:
- Stable source of radiant energy
- Filter that isolates a specific region of the electromagnetic spectrum
- Cuvets
- Sample holder
- Radiation detector
- Signal processor and
- Readout device
Parts of the Spectrophotometer: provides polychromatic light; intense beam of light is directed; must be linear.
Light/Radiant source
2 types of light source
Continuum source
Line source
Type of light source: changes in
intensity; widely used in the laboratory.
Continuum source
Examples of continuum source
Tungsten, deuterium and xenon lamps
light source in the
visible and near infrared region
Tungsten light bulb
provide UV radiation in
analytic spectrometers.
Deuterium lamp
source of radiation covers both the UV and the visible range
Xenon discharges lamp/ xenon lamp
Type of light source: limited radiation and wavelength.
Line source
Examples of line source
Mercury and sodium vapor lamp and hollow cathode lamp (AAS)
Line source wide us in
Atomic absorption, molecular, and fluorescent spectroscopy
used as light sources for spectrophotometry.
Light Amplification by Stimulated Emission of Radiation (LASER)
Factors for choosing a light source:
- Range
- Spectral distribution within the range
- The source of radiant production
- Stability of the radiant energy and
- Temperature
Alternatives for tungsten bulb:
+ Mercury arc (visible and UV)
+ Deuterium lamp (165nm) - UV
+ Hydrogen lamp - UV
+ Xenon lamp - UV
+ Merst glower -IR
+ Globar (silicone carbide) - IR
• minimizes unwanted or stray light
• prevents the entrance of scattered light
Entrance slit
• minimizes unwanted or stray light
• prevents the entrance of scattered light
Entrance slit
• most common cause of loss of linearity
• limits the maximum absorbance
• causes absorbance error.
Stray light
isolates specific or individual
wavelength
Monochromator
isolates specific or individual
wavelength
Monochromator
• wedge-shaped pieces of glass, quartz or sodium chloride
• can be rotated
• narrow light focused
Prism
• the most commonly used kind monochromator
• made by cutting grooves (parallel grooves) or slits
• wavelengths are bent
• Produces linear spectrum
• light energy is absorbed by glass prism.
Diffraction gratings
• the most commonly used kind monochromator
• made by cutting grooves (parallel grooves) or slits
• wavelengths are bent
• Produces linear spectrum
• light energy is absorbed by glass prism.
Diffraction gratings