Atomic spectroscopy plays a major role as the basis of a wide range of analytical techniques that contribute data on elemental concentrations and isotope ratios .These analytical data provide the raw material on which progress in geochemistry depends.
The main advantages of AAS & AES are that it is relatively inexpensive and easy to use, while still offering high throughput, quantitative analysis of the metal content of solids or liquids. This makes it suitable for use in a wide range of applications.
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 Spectrophotometer is for determining the concentration of a particular metal(element) in a sample. Atomic Absorption Spectrophotometer can be used to analyze the concentration of over 62 different metals. For More Information Please Logon http://goo.gl/1dTEGl
Atomic spectroscopy plays a major role as the basis of a wide range of analytical techniques that contribute data on elemental concentrations and isotope ratios .These analytical data provide the raw material on which progress in geochemistry depends.
The main advantages of AAS & AES are that it is relatively inexpensive and easy to use, while still offering high throughput, quantitative analysis of the metal content of solids or liquids. This makes it suitable for use in a wide range of applications.
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 Spectrophotometer is for determining the concentration of a particular metal(element) in a sample. Atomic Absorption Spectrophotometer can be used to analyze the concentration of over 62 different metals. For More Information Please Logon http://goo.gl/1dTEGl
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.
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
introduction
Interference is a phenomena
that leads to changes (either positive or negative) in intensity of the analyte signal in spectroscopy.
Interferences in atomic absorption spectroscopy fall into two basic categories, namely, non-spectral and spectral.
1. spectral 2. Non Spectral ( Matrix interference, chemical interference, ionization interference)
PRINCIPLE - atomic absorpion spectroscopy
Atoms of the analyte have a fixed number of electrons.
If the light of a specific wavelength is passed through a flame containing that atom, electrons present in different energy levels, known as orbitals, absorb a certain wavelength and excite to higher energy levels.
The extent of absorption ά the number of ground-state atoms in the flame.
Only for information- The ground state is more stable than the excited state. The electrons spontaneously return back to the ground state. It emits the same amount of radiant energy. This process is called fluorescence. Fluorescence is used in atomic emission spectroscopy.
Brief note on - Instrumentation
The basic components of atomic absorption are:
Light source
Chopper
Atomizer
Burners
flames
Monochromators
Detectors
Amplifier
Readout devices
WORKING PROCESS
Calibration
Quantitative analysis in AAS
Safety measures
Important questions and answer
Queueing theory is the mathematical study of waiting lines, or queues. A queueing model is constructed so that queue lengths and waiting time can be predicted
Ionizing radiations can play a significant role in the control of biotic factors responsible for the spoilage of fruits and vegetables. Radiation processing involves the controlled application of the energy of ionizing radiations such as gamma rays, X-rays, and accelerated electrons to fruits and vegetables for achieving safety of the produces.
The liquid food is generally preconcentrated by evaporation to economically reduce the water content. The concentrate is then introduced as a fine spray or mist into a tower or chamber with heated air. As the small droplets make intimate contact with the heated air, they flash off their moisture, become small particles, and drop to the bottom of the tower, and are removed. The advantages of spray drying include a low heat and short time combination which leads to a better quality product.
The oscillating magnetic field is one of the emerging nonthermal processing methods of food preservation. OMF has the potential to inactivate microorganisms, pasteurize food with an improvement in the quality and shelf life, and alters the growth and reproduction of microorganisms. It has its own limitations and drawbacks.
Pulsed electric field (PEF) processing is an emerging non-thermal food preservation technology. PEF technology is established on the utilization of electric fields to remove food-borne pathogens and to subjugate the spoilage microorganisms in foods. This technology is notably acknowledged for its capability to amplify the mean life of food products without the utilization of heat also preserving the quality aspects such as sensory and nutritional attributes, together with enabling the safety of food products
Non-thermal processes have become increasingly popular over the last decades. As one of the emerging non-thermal
technologies, pulsed light (PL) represents a fast, tailored and residue-free technology that—via high frequency,
high intensity pulses of broad-spectrum light rich in the UV fraction—is capable of inactivating microbial
cells and spores.
Operation “Blue Star” is the only event in the history of Independent India where the state went into war with its own people. Even after about 40 years it is not clear if it was culmination of states anger over people of the region, a political game of power or start of dictatorial chapter in the democratic setup.
The people of Punjab felt alienated from main stream due to denial of their just demands during a long democratic struggle since independence. As it happen all over the word, it led to militant struggle with great loss of lives of military, police and civilian personnel. Killing of Indira Gandhi and massacre of innocent Sikhs in Delhi and other India cities was also associated with this movement.
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Prepare a presentation or a paper using research, basic comparative analysis, data organization and application of economic information. You will make an informed assessment of an economic climate outside of the United States to accomplish an entertainment industry objective.
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3. AAS
3
AAS,
An analytical method based on the absorption of ultraviolet or visible radiation by free atoms in the
gaseous state.
Major role in the development of current database for mineral nutrients and toxicants
Accurate measuring of mineral elements in trace amounts
Advances : Food analysis, nutrition, biochemistry, and toxicology
Replaced traditional wet chemistry methods for mineral analysis of foods
■ Exceptions: Calcium, chloride, iron, and phosphorus
All of the elements in the periodic chart may be determined by AAS & AES (Mineral elements)
4. AAS quantifies the absorption of electromagnetic radiation by well-separated neutral
atoms in the gaseous state
AES measures emission of radiation from atoms excited by heat or other means
AAS suitability is due to,
Atomic spectra consist of discrete lines
Every element has a unique spectrum
Individual elements can be identified and quantified accurately and precisely
AAS
4
5. AAS
5
Production of atomic absorption spectra:
When Ground state atoms (or ions) absorb energy from a radiation source.
Absorption of a photon of radiation causes an outer shell electron to jump to a higher energy level,
an excited state
The excited atom may fall back to a lower energy state, releasing a photon in the process.
Atoms absorb or emit radiation of discrete wavelengths because the allowed energy levels of
electrons in atoms are fixed (not random).
6. AAS
6
The energy change associated with a transition between two energy levels is directly related to the frequency of the
absorbed radiation:
Ee−Eg = hν
■ Ee = energy in excited state
■ Eg = energy in ground state
■ h = Planck’s constant
■ ν = frequency of the radiation
Rearranging, we have:
ν = (Ee − Eg)/h
or, since ν = c/λ
λ = hc/(Ee − Eg)
where:
■ c = speed of light
■ λ = wavelength of the absorbed or emitted light
For absorption, transitions involve primarily the excitation of electrons in the ground state, so the number of
transitions is relatively small.
7. AAS requires atoms of the element of interest to be in atomic state.
In foods, all elements are compounds or complexes must be converted to neutral atoms
Atomization: Separation of particles into individual molecules (vaporization) & breaking molecules
into atoms
Exposing the analyte as fine mist to high temperatures , flame or plasma
Solvent evaporates, leaving solid particles of the analyte that vaporize and decompose to atoms
Atoms absorb radiation (atomic absorption) or become excited and subsequently emit radiation
(atomic emission).
AAS
7
8. AAS
8
Two types of atomization are commonly used in AAS: flame atomization and electrothermal
(graphite furnace) atomization.
Schematic representation of a double-beam atomic absorption spectrophotometer
9. 1. Radiation source, a hollow cathode lamp (HCL) or an electrode-less discharge lamp (EDL)
2. Atomizer, usually a nebulizer–burner system or an electrothermal furnace
3. Monochromator, usually an ultraviolet-visible (UV-Vis) grating monochromator
4. Detector, a photomultiplier tube (PMT) or a solid-state detector (SSD)
5. Computer
AAS
9
10. HOLLOW CATHODE LAMPS
A hollow tube filled with argon or neon, an anode ( tungsten), & a cathode (the metallic form of the
element being measured)
Voltage applied across the electrodes, the lamp emits radiation characteristic of the metal in the
cathode
If the cathode is made of iron, an iron spectrum is emitted.
For a given electronic transition, either up or down in energy, the energy of an emitted photon is
exactly the same as the energy of an absorbed photon.
HCLs available for about 60 metallic elements.
AAS
10
11. CHOPPER
A chopper is a disk with segments removed.
The disk rotated at constant speed that the light beam reaching the flame is either on or off at
regular intervals.
The flame also produces radiation but flame radiation is continuous
The radiation reaching the detector consists of the sum of an alternating and a continuous
signal.
Instrument electronics subtract the continuous signal & sends only the alternating signal to
the readout.
AAS
11
12. AAS
12
ATOMIZERS
Types of atomizers are,
Flame atomizers
Electrothermal atomizers
Cold vapor technique for mercury
Hydride generation technique
FLAME ATOMIZER
Consist of a nebulizer and a burner.
Nebulizer converts sample solution into a fine mist or aerosol.
Sample mixed with fuel and an oxidant, and burned in a flame
Only 1% of the total sample is carried into the flame by the oxidant–fuel mixture
Flame atomizer
13. Flame characteristics may be manipulated by, Adjusting oxidant/fuel ratios and by choice of oxidant
and fuel.
Commonly used oxidant–fuel mixtures: Air-acetylene and nitrous oxide-acetylene
TYPES OF FLAMES
Stoichiometric: the fuel and oxidant is completely consumed. yellow fringes.
Oxidizing: Flame is produced from a fuel – lean mixture, hottest flame & clear blue
appearance.
Reducing: Flame is produced from a fuel-rich mixture, relatively cool flame & yellow color
AAS
13
Cont’d…
14. Cylindrical graphite tubes connected to an electrical power supply, referred as graphite
furnaces.
The sample is introduced through a microliter syringe (sample volumes normally range from
0.5 to 10 μl).
The system is flushed with an inert gas to,
Prevent the tube from burning
Exclude air from the sample compartment.
Tube is heated electrically.
Stepwise increase in temperature, first the sample solvent is evaporated
The sample is ashed & temperature is rapidly increased to 2,000–3,000⁰ C , quickly vaporize
and atomize the sample.
AAS
14
15. AAS
15
This technique works only for mercury,
Mercury, exist as free atoms in the gaseous state at room temperature.
Reduced to elemental mercury by the action of stannous chloride (a strong reducing agent ).
The elemental mercury is then carried in a stream of air or argon into an absorption cell
Atomic absorption is measured the same way as it is in flame ionization and Electrothermal
instruments.
This method has the advantage of very high sensitivity
16. Volatile hydrides of elements are formed by reacting samples with sodium borohydride .
Hydrides are carried into an absorption cell and heated to decompose into free atoms.
Then atomic absorption measurements are carried out in the same manner as with other atomization
techniques
Limited to a relatively few elements which are capable of forming volatile hydrides.
E.g: As, Pb, Sn, Bi, Sb, Te, Ge, and Se.
AAS
16
17. Positioned in the optical path between the flame or furnace and the detector
Its purpose is to isolate the resonance line of interest
Only the desired wavelength reaches the detector.
Monochromators of the grating type are used
Two types of detectors
Photomultiplier tubes
solid-state detectors.
Detectors convert the radiant energy into an electrical signal
The signal is processed to produce either an analog or a digital readout
AAS
17
Monochromator
18. A generalized procedure that will be similar but not identical to procedures found in instrument
operating manuals:
1. Turn the lamp current control knob to the off position.
2. Install the required lamp in the lamp compartment.
3. Turn on main power and power to lamp. Set lamp current to the current shown on the lamp label.
4. Select required slit width and wavelength and align light beam with the optical system.
5. Ignite flame and adjust oxidant and fuel flow rates.
6. Aspirate distilled water. Aspirate blank and zero instrument.
7. Aspirate standards and sample.
8. Aspirate distilled water.
9. Shut down instrument.
AAS
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