This document provides an overview of atomic absorption spectroscopy and mass spectrometry. It describes how atomic absorption spectroscopy can detect over 62 elements in samples by vaporizing the analyte and measuring light absorption. Mass spectrometry works by ionizing molecule fragments and separating them based on their mass-to-charge ratio to determine molecular structure. Both techniques are used in applications like pharmaceutical analysis, environmental testing, and forensics.
The presentation is about Inductively coupled plasma mass spectrometry (ICP-MS) which is a type of mass spectrometry that is capable of detecting metals and several non-metals at concentrations as low as parts per billion.
mass spectrometry, also called mass spectroscopy, analytic technique by which chemical substances are identified by the sorting of gaseous ions in electric and magnetic fields according to their mass-to-charge ratios.
The presentation is about Inductively coupled plasma mass spectrometry (ICP-MS) which is a type of mass spectrometry that is capable of detecting metals and several non-metals at concentrations as low as parts per billion.
mass spectrometry, also called mass spectroscopy, analytic technique by which chemical substances are identified by the sorting of gaseous ions in electric and magnetic fields according to their mass-to-charge ratios.
A scanning electron microscope is a type of electron microscope that produces images of a sample by scanning the surface with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that contain information about the sample's surface topography and composition.
SEMs can magnify an object from about 10 times up to 300,000 times. A scale bar is often provided on an SEM image. From this the actual size of structures in the image can be calculated.
Introduction and understanding of emission and absorption spectrum, discussion on flame and its characteristics and the types of flame sources used in AAS, a brief discussion of flame emission spectroscopy ,possibly deep discussion of AAS, Interferences involved in AAS and their reasons.
The ppt is divided into five topics within itself trying to understand each topics individually before jumping into AAS
Mass spectrometer converts molecules to ions under vacuum so that they can be moved about and manipulated by external electric and magnetic fields.
These ions are then separated and determined. Separation is achieved on different trajectories of moving ions in electrical and/or magnetic fields.
*Electrospray Ionization (ESI)
*Matrix-Assisted Laser Desorption/Ionization (MALDI)
*Time-of-Flight (TOF) Mass Analyzer
Recent advances in the application of mass spectrometry in food-related analysis
*LC-MS coupling techniques
*HPLC-MS coupling techniques
*MALDI-TOF-MS
*ESI-MS
Introduction to Activation analysis using Neutron
Baisc Principle of NAA
Instrumental NAA
Characteristics of INAA
Advantages, Limitation and Applications of INNA
A short lecture about Atomic Spectroscopy: Flame Photometry, Atomic Absorption, and Atomic Emission with Coupled Plasma (FP, AA and ICP-AES). Presented at 28.03.2011, Faculty of Agriculture, Hebrew University of Jerusalem, by Vasiliy Rosen, M.Sc.
A scanning electron microscope is a type of electron microscope that produces images of a sample by scanning the surface with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that contain information about the sample's surface topography and composition.
SEMs can magnify an object from about 10 times up to 300,000 times. A scale bar is often provided on an SEM image. From this the actual size of structures in the image can be calculated.
Introduction and understanding of emission and absorption spectrum, discussion on flame and its characteristics and the types of flame sources used in AAS, a brief discussion of flame emission spectroscopy ,possibly deep discussion of AAS, Interferences involved in AAS and their reasons.
The ppt is divided into five topics within itself trying to understand each topics individually before jumping into AAS
Mass spectrometer converts molecules to ions under vacuum so that they can be moved about and manipulated by external electric and magnetic fields.
These ions are then separated and determined. Separation is achieved on different trajectories of moving ions in electrical and/or magnetic fields.
*Electrospray Ionization (ESI)
*Matrix-Assisted Laser Desorption/Ionization (MALDI)
*Time-of-Flight (TOF) Mass Analyzer
Recent advances in the application of mass spectrometry in food-related analysis
*LC-MS coupling techniques
*HPLC-MS coupling techniques
*MALDI-TOF-MS
*ESI-MS
Introduction to Activation analysis using Neutron
Baisc Principle of NAA
Instrumental NAA
Characteristics of INAA
Advantages, Limitation and Applications of INNA
A short lecture about Atomic Spectroscopy: Flame Photometry, Atomic Absorption, and Atomic Emission with Coupled Plasma (FP, AA and ICP-AES). Presented at 28.03.2011, Faculty of Agriculture, Hebrew University of Jerusalem, by Vasiliy Rosen, M.Sc.
ATOMIC ABSORPTION SPECTROSCOPY (AAS) a.k.a SPEKTROSKOPI SERAPAN ATOM (SSA))Anna Funniisa'
AAS (spektroskopi serapan atom/ Atomic absorption spectroscopy) pertama kali dimanfaatkan Alan Walsh (1955). metode ini sangat tepat untuk analisis zat berkonsentrasi rendah. metode AAS berprinsip padaabsorpsi cahaya oleh atom-atom. Atom menyerap cahaya tersebut pada panjang gelombang tertentu, tergantung sifat unsurnya. Unsur-unsur yang dapat dideteksi oleh AAS/SSA adalah unsur-unsur logam, dan beberapa unsur non-logam (3 unsur).
a brief discussion of AAS, an analytical technique use for heavy metal analysis. Atomic absorption spectroscopy is a quantitative method of analysis of any kind of sample; that is applicable to many metals
AAS can be used to determine over 70 different elements in solution, or directly in solid samples via electro thermal vaporization.
Atomic Absorption Spectroscopy is a very common technique for detecting metals and metalloids in samples.
It is very reliable and simple to use.
It also measures the concentration of metals in the sample.
Atomic Absorption Spectroscopy is an analytical technique that measures the concentration of an element by measuring the amount of light that is absorbed at a characteristic wavelength when it passes through cloud of atoms
As the number of atoms in the light path increases, the amount of light absorbed increases.
Applications: Presence of metals as an impurity or in alloys can be perform.
Level of metals could be detected in tissue samples like Aluminum in blood and Copper in brain tissues.
Due to wear and tear there are different sorts of metals which are given in the lubrication oils which could be determined for the analysis of conditions of machines.
Determination of elements in the agricultural samples.
Water sample analysis (e.g. Ca, Mg, Fe, Si, Al, Ba content).
Food sample analysis.
Analysis of animal feedstuffs (e.g. Mn, Fe, Cu, Cr, Se, Zn).
Analysis of additives in lubricating oils and greases (Ba, Ca, Na, Li, Zn, Mg). analysis of soils.
Clinical sample analysis (blood samples: whole blood, plasma, serum; Ca, Mg, Li, Na, K, Fe).
Analysis of Environmental samples such as- drinking water, ocean water, soil.
Pharmaceutical sample Analysis: Estimation of zinc in insulin preparation, calcium in calcium salt is done by using AAS. Principle: The sample, in solution, is aspirated as a spray into a chamber, where it is mixed with air and fuel.
This mixture passes through baffles, here large drops fall and are drained off. Only fine droplets reach the flame.
Light from the hollow-cathode lamp passes through the sample of ground-state atoms in the flame.
The amount of light absorbed is proportional to the concentration.
The element being determined must be reduced to the elemental state, vaporized, and imposed in the beam of the radiation in the source.
When a ground-state atom absorbs light energy, an excited atom is produced.
The excited atom then returns to the ground state, emitting light of the same energy as it absorbed.
The flame sample thus contains a dynamic population of ground-state and excited atoms, both absorbing and emitting radiant energy. The emitted energy from the flame will go in all directions, and it will be a steady emission.
Because the purpose of the instrument is to measure the amount of light absorbed, the light detector must be able to distinguish between the light beam emitted by the hollow cathode lamp and that emitted by excited atoms in the flame.
A presentation containing the Principle, shematic diagram, omponents of the instrument, working of the instrument, application, advantages and disadvantages of the instrument.
This presentation contains a simple discussion about the basic principles, Instrumentation, Various ionization techniques, mass analyzers, Mass detectors, Fragmentation, and various peak observed in Mass spectra(Molecular ion peak, Metastable peak, Base peak etc)
And application of Mass spectroscopy on various field.
Spectroscopy using spectrophotometers of different types like: U.V, Mass Spectrophotometer, absorption , Emission, Nuclear magnetic resonance and X-rays Spectrophotometer
Introduction, Basic Principles, Terminology, Instrumentation, Ionization techniques (EI, CI, FAB, MALDI, and ESI), Mass Analyzer (Magnetic sector instruments, Quadrupole, TOF, and ICR ), and Applications of Mass Spectrometry.
Pharmaceuticals: In some pharmaceutical manufacturing processes, minute quantities of a catalyst used in the process (usually a metal) are sometimes present in the final product. By using AAS the amount of catalyst present can be determined.
Atomic absorption spectroscopy (AAS) and atomic emission spectroscopy (AES) is a spectro analytical procedure for the quantitative determination of chemical elements by free atoms in the gaseous state.
Atomic absorption spectroscopy is based on absorption of light by free metallic ions.
In analytical chemistry the technique is used for determining the concentration of a particular element (the analyte) in a sample to be analyzed. AAS can be used to determine over 70 different elements in solution, or directly in solid samples via electrothermal vaporization
Atomic absorption spectrometry (AAS) is an analytical technique that measures the concentrations of elements.
Atomic absorption is so sensitive that it can measure down to parts per billion of a gram (µg dm–3 ) in a sample.
The technique makes use of the wavelengths of light specifically absorbed by an element. They correspond to the energies needed to promote electrons from one energy level to another, higher, energy level.
Atomic absorption spectrometry has many uses in different areas of chemistry.
Clinical analysis : Analysing metals in biological fluids such as blood and urine.
Environmental analysis: Monitoring our environment – eg finding out the levels of various elements in rivers, seawater, drinking water, air, petrol and drinks such as wine, beer and fruit drinks.
The technique makes use of the atomic absorption spectrum of a sample in order to assess the concentration of specific analytes within it. It requires standards with known analyte content to establish the relation between the measured absorbance and the analyte concentration and relies therefore on the [Beer–Lambert law].
The electrons within an atom exist at various energy levels. When the atom is exposed to its own unique wavelength, it can absorb the energy (photons) and electrons move from a ground state to excited states.
The radiant energy absorbed by the electrons is directly related to the transition that occurs during this process.
Furthermore, since the electronic structure of every element is unique, the radiation absorbed represents a unique property of each individual element and it can be measured.
An atomic absorption spectrometer uses these basic principles and applies them in practical quantitative analysis
A typical atomic absorption spectrometer consists of four main components:
Atomization
Light source,
Atomization system,
Monochromator &
Detection system
Atomization can be carried out either by a flame or furnace.
Heat energy is utilized in atomic absorption spectroscopy to convert metallic elements to atomic dissociated vapor.
The temperature should be controlled very carefully for the conversion of atomic vapor.
At too high temperatures, atoms
Mass spectrometry is an extremely valuable
analytical technique in which the molecules
in a test sample are converted into gaseous
ions that are subsequently separated in a mass
spectrometer according to their mass-to-charge
ratio (m/z) and detected .
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3. INTRODUTION
Atomic Absorption Spectroscopy is a very
common technique for detecting metals and
metalloids in samples.
It is very reliable and simple to use.
It can analyze over 62 elements.
It also measures the concentration of metals in
the sample.
4. HISTORY
The first atomic absorption spectroscopy was built
by CSIRO scientist Alan Walsh in 1954.
The first commercial atomic absorption
spectroscopy was introduced in 1959.
6. PRINCIPLE
The technique uses basically the principle that free atoms
(gas) generated in an atomizer can absorb radiation at
specific frequency.
Atomic Absorption spectroscopy quantifies the absorption
of ground state atoms in the gaseous state.
The atoms absorb ultraviolet or visible light and make
transitions to higher electronic energy levels. The analyte
concentration is determined from the amount of absorption.
Concentration measurements are usually determined from a
working curve after calibrating the instrument with
standards of known concentration.
9. LIGHT SOURCE
Hollow Cathode Lamp are the most common radiation
source in AAS.
It contains a tungsten anode and a hollow cylindrical
cathode.
These are sealed in a glass tube filled with an inert gas
(neon or argon ) .
Each element has its
own unique lamp which
must be used for that
analysis .
11. NEBULIZER
Suck up liquid samples at controlled rate.
Create a fine aerosol spray for introduction into
flame.
Mix the aerosol and fuel and oxidant thoroughly
for introduction into flame.
12. ATOMIZER
Elements to be analysed needs to in atomic state.
Atomization is separation of particles into
individual molecules and breaking molecules into
atoms. This is done by exposing the analyte to high
temperature in a flame or graphite furnace.
Sample Atomization Technique
Flame
Atomization
Electro thermal
Atomization
Hydride
Atomization
Cold-Vapor
Atomization
13. Flame Atomization
Nebulizer suck up liquid samples at controlled
rate.
Create a fine aerosol spray for introduction into
flame.
Mix the aerosol and oxidant thoroughly
for introduction into flame.
An aerosol is a colloid of fine solid particles or
liquid droplets, in air or another gas.
14. Flame Atomization
sample mist
Solid/gas
aerosol
Gaseous
molecules
Atom
s
nebulization desolvation volatilization
dissociation
15. Disadvantages of Flame
Atomization
Only 5-15% of the nebulized sample reaches the
flame.
A minimum sample volume of 0.5-1.0 ml is
needed to give a reliable reading.
Samples which are viscous require dilution with
a solvent.
16. Electro Thermal Atomization
Uses a graphite coated furnace to vaporize the
sample.
samples are deposited in a small graphite coated
tube which can then heated to vaporize and
atomize the analyte.
The graphite tubes are heated using a high
current power supply.
17. Advantages
Small sample size
Very little or no sample preparation is needed
Sensitivity is enhanced
Direct analysis of solid samples
Disadvantages
Analyte may be lost at the ashing stage
The sample may not be completely atomized
Analytical range is relatively low
18. MONOCHROMATOR
This is very important part in an AAS.
It is used to separate out all of the thousands of
lines.
A monochromator is used to select the specific
wavelength of light which is absorbed by the
sample, and to exclude other wavelengths.
The selection of the specific light allows the
determination of the selected element in the
presence of others.
19. DETECTOR
The light selected by the monochromator is
directed onto a detector that is typically a
photomultiplier tube, whose function is convert
the light signal into an electrical signal
proportional to the intensity.
The processing of electrical signal is fulfilled by
a signal amplifier.
The signal could be displayed for readout, or
further fed into a data station for printout by the
requested format
20. Calibration Curve
A calibration curve is used to determine the
unknown concentration of an element in a
solution.
The instrument is calibrated using several
solutions of known concentrations.
The absorbance of each known solution is
measured and then a calibration curve of
concentration vs absorbance is plotted.
The sample solution is fed into the instrument, and
the absorbance of the element in this solution is
measured.
The unknown concentration of the element is then
calculated from the calibration curve
21.
22. Applications
Determination of even small amounts of metals
(lead, mercury, calcium, magnesium, etc.)
Environmental studies: drinking water, ocean
water, soil.
Food industry.
Pharmaceutical industry.
Presence of metals as an impurity or in alloys
could be done easily
Level of metals could be detected in tissue
samples like Aluminum in blood and Copper in
brain tissues
24. Introduction
Mass Spectroscopic method is one of the most popular
molecular analysis methods today.
Mass Spectroscopy is an analytical spectroscopic tool
primarily concerned with the separation of molecular
(and atomic) species according to their mass.
It is a microanalytical technique requiring only a few
nanomoles of the sample to obtain characteristic
information pertaining to the structure and molecular
weight of analyte.
It is not concerned with non- destructive interaction
between molecules and electromagnetic radiation.
25. Principle
Mass spectroscopy is the most accurate method
for determining the molecular mass of the
compound and its elemental composition.
In this technique, molecules are bombarded with
a beam of energetic electrons.
The molecules are ionised and broken up into
many fragments, some of which are positive
ions.
26. Mass spectra is used in two general ways:
To prove the identity of two compounds.
To establish the structure of a new a compound.
The mass spectrum of a compound helps to
establish the structure of a new compound in
several different ways:
It can give the exact molecular mass.
It can give a molecular formula or it can reveal
the presence of certain structural units in a
molecule.
29. METHODOLOGY
Gaseous or liquid substances that vaporize under
vacuum are admitted to a mass spectroscopy.
The gas is diluted by being partially pumped down to
a low pressure (molecular flow range) in a vacuum
chamber and ionized through electron bombardment.
The ions thus generated are introduced to a mass
filter and separated on the basis of their charge to
mass ratio.
30. IONISATION
The atom is ionised by knocking one or more
electrons off to give a positive ion. (Mass
spectrometers always work with positive ions).
The particles in the sample (atoms or molecules) are
bombarded with a stream of electrons to knock one or
more electrons out of the sample particles to make
positive ions.
31. ACCELERATION
The ions are accelerated so that they all have the same
kinetic energy.
32. The positive ions are repelled away from the
positive ionization chamber and pass through three
slits with voltage in the decreasing order.
The middle slit carries some intermediate voltage
and the final at ‘0’ volts.
All the ions are accelerated into a finely focused
beam.
33. DEFLECTION
The ions are then deflected by a magnetic field
according to their masses. The lighter they are, the more
they are deflected.
The amount of deflection also depends on the number
of positive charges on the ion -The more the ion is
charged, the more it gets deflected.
34. Different ions are deflected by the magnetic
field by different amounts. The amount of
deflection depends on:
The mass of the ion: Lighter ions are deflected
more than heavier ones.
The charge on the ion: Ions with 2 (or more)
positive charges are deflected more than ones
with only 1 positive charge.
35. DETECTION
The beam of ions passing through the machine is
detected electrically.
When an ion hits the metal box, its charge is
neutralized by an electron jumping from the metal on
to the ion.
36. That leaves a space among the electrons in the
metal, and the electrons in the wire shuffle along
to fill it.
A flow of electrons in the wire is detected as an
electric current which can be amplified and
recorded. The more ions arriving, the greater the
current.
37.
38. APPLICATIONS
Pharmaceutical analysis
Bioavailability studies
Drug metabolism studies, pharmacokinetics
Characterization of potential drugs
Drug degradation product analysis
Screening of drug candidates
Identifying drug targets
Biomolecule characterization
Proteins and peptides
Oligonucleotides
40. Reference
Mass Spectroscopy Amruta S. Sambarekar
Mass Spectroscopy - An Overview Dr. M. Vairamani,
IPFT
http://www.uga.edu/~sisbl/aaspec.html
http://www.clu-in.org/char/technologies/graphite.cfm
B. Welz, M. Sperling, Atomic Absorption
Spectrometry, Wiley-VCH, Weinheim, Germany, ISBN
3-527-28571-7.
Skoog, Douglas (2007). Principles of Instrumental
Analysis (6th ed.). Canada: Thomson Brooks/Cole.
ISBN 0-495-01201-7.