Principle
Interferences
Instrumentation and
Applications
The principle of flame photometer
is based on the measurement of the emitted light intensity when a metal is introduced into the flame.
The wavelength of the colour gives information about the element and
the colour of the flame gives information about the amount of the element present in the sample.
Flame photometry is one of the branches of atomic absorption spectroscopy.
It is also known as flame emission spectroscopy.
Currently, it has become a necessary tool in the field of analytical chemistry. Used to
Determine the concentration of certain metal ions like
potassium,lithium, calcium, cesium etc. In flame photometer spectra the metal ions are used in the form of atoms.
(IUPAC) Committee on Spectroscopic Nomenclature has named this technique as flame atomic emission spectrometry (FAES). Principle of Flame photometer
The compounds of the alkali and alkaline earth metals (Group II) dissociate into atoms when introduced into the flame.
Some of these atoms further get excited to even higher levels. But these atoms are not stable at higher levels.
Hence, these atoms emit radiations when returning back to the ground state.
These radiations generally lie in the visible region of the spectrum.
Each of the alkali and alkaline earth metals has a specific wavelength. Instrumentation-Source of flame, Nebuliser, Monochromator(Prism monochromator, Grating monochromators)DETECTOR (
The radiation emitted by the elements is mostly in the visible region and measured by photo detector. Hence conventional detectors like photo voltaic cell or photo tubes or photomultiplier tube is used), READ OUT DEVICE
[The signal from the detector is shown as a response in the digital read out device. The readings are displayed in an arbitrary scale (% Flame Intensity).], working of flame photometer, Advantages and disadvantage of flame photometer, Errors /interference in Flame Photometry-Flame Temperature, chemical interference, Radiation interference
Application of flame photometry
In this slide contains Interference In Atomic Absorption Spectroscopy and applications.
Presented by: Shaik Gouse ul azam. ( department of pharmaceutical analysis.)
RIPER, anantpur.
This presentation include the detailed explanation of various parts of a UV-Visible spectrophotometer and two types of UV-Visible spectrophotometers-Single beam and Doube beam. It also include the comparison between single beam and double beam spectrophotometers.
In this slide contains Interference In Atomic Absorption Spectroscopy and applications.
Presented by: Shaik Gouse ul azam. ( department of pharmaceutical analysis.)
RIPER, anantpur.
This presentation include the detailed explanation of various parts of a UV-Visible spectrophotometer and two types of UV-Visible spectrophotometers-Single beam and Doube beam. It also include the comparison between single beam and double beam spectrophotometers.
Fluorimetry, principle, Concept of singlet,doublet,and triplet electronic sta...Vandana Devesh Sharma
Content-Principle
concept of singlet, doublet and triplet electronic stages,
Internal and external conversions,
Factors affecting fluorescence,
quenching,
Instrumentation and
applications
Types of luminescence including
bioluminescence,
chemiluminescence,
Fluorescence, and
phosphorescence
These various forms of luminescence differ in their method of emitting light.
Bioluminescence
Chemiluminescence
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds) Fluorimetry
An analytical technique for identifying and characterizing minute amounts of substance by excitation of the substance with a beam of ultraviolet/Visible light and detection and measurement of the characteristic wavelength of fluorescent light emitted.Excited – State Processes in molecules
in this slides contains principle and types of detectors used in Gas Chromatography.
Presented by: J.Vinay Krishna. (Department of industrial pharmacy),
RIPER, anantapur.
IR SPECTROSCOPY, INTRODUCTION, PRINCIPLE, THEORY, FATE OF ABSORBED RADIATION, FERMI RESONANCE, FINGERPRINT REGION, VIBRATIONS, FACTORS AFFECTING ABSORPTION OF IR RADIATION, SAMPLING TECHNIQUES, APPLICATIONS OF IR SPECTROSCOPY.
Fluorimetry, principle, Concept of singlet,doublet,and triplet electronic sta...Vandana Devesh Sharma
Content-Principle
concept of singlet, doublet and triplet electronic stages,
Internal and external conversions,
Factors affecting fluorescence,
quenching,
Instrumentation and
applications
Types of luminescence including
bioluminescence,
chemiluminescence,
Fluorescence, and
phosphorescence
These various forms of luminescence differ in their method of emitting light.
Bioluminescence
Chemiluminescence
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds)
Fluorescence starts immediately after the absorption of light and stops as soon as the incident light is cut off
Eg -The fluorescent clothes, shoes
Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation.
In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, than the absorbed radiation
In fluorescence, absorption and emission light takes place in very short time (10-12 or 10-9 seconds) Fluorimetry
An analytical technique for identifying and characterizing minute amounts of substance by excitation of the substance with a beam of ultraviolet/Visible light and detection and measurement of the characteristic wavelength of fluorescent light emitted.Excited – State Processes in molecules
in this slides contains principle and types of detectors used in Gas Chromatography.
Presented by: J.Vinay Krishna. (Department of industrial pharmacy),
RIPER, anantapur.
IR SPECTROSCOPY, INTRODUCTION, PRINCIPLE, THEORY, FATE OF ABSORBED RADIATION, FERMI RESONANCE, FINGERPRINT REGION, VIBRATIONS, FACTORS AFFECTING ABSORPTION OF IR RADIATION, SAMPLING TECHNIQUES, APPLICATIONS OF IR SPECTROSCOPY.
INSTRUMENTAL METHODS OF ANALYSIS, B.PHARM 7TH SEM. AND FOR BSC,MSC CHEMISTRY. This is Geeta prasad kashyap (Asst. Professor), SVITS, Bilaspur (C.G) 495001
Instrumental Method of AnalysisUnit 2 (3) Atomic absorption spectroscopy/AAS/
Atomic flame Photometry
(Part -1)
Introduction- Briefing
Atomic spectroscopy involved three major techniques- Atomic emission spectroscopy,
Atomic absorption spectroscopy, and Atomic fluorescence spectroscopy
Principle, Theory of atomic Absorption spectroscopy
Interferences
Instrumentation-
Type AAS
1. Single beam atomic absorption spectrophotometer
2. Double beam atomic absorption spectrophotometer
the light source/radiation source- that emits the spectrum of the element of inetrest
the atomization system/ absorption cell- in which atoms the sample are produced (flame, graphites furnance etc
the monochromator- for light dispersion
the detection system- which measures the light intensity and amplified the signal
A read out device- that show the reading after it has been processed
Working AAS instrument (B. chopper, C. Flame atomizer - There is two types of burners in common used
1. Total consumption burner
2. Premixed burner
D. Fuel/ oxidant
E. Monochromator- Prism, gratting
F. Detectors-Photomultiplier tube
G. Recorder
Difference between Atomic Absorption Spectroscopy and Atomic Emission Spectroscopy
Advantange and limitation
Applications
HPLC- Introduction, Theory, Instrumentation, Advantage, Applications
High-performance liquid chromatography or commonly known as HPLC, is an analytical technique used to separate, identify or quantify each component in a mixture.
The mixture is separated using the basic principle of column chromatography and then identified and quantified by spectroscopy.
In the 1960s, the column chromatography LC with its low-pressure suitable glass columns was further developed to the HPLC with its high-pressure adapted metal columns.
HPLC is thus basically a highly improved form of column liquid chromatography. Instead of a solvent being allowed to drip through a column under gravity, Solvent is forced through under high pressures of up to 400 atmospheres.
Principle
The separation principle of HPLC is based on the distribution of the analyte (sample) between a mobile phase (eluent) and a stationary phase (packing material of the column). Depending on the chemical structure of the analyte, the molecules are retarded while passing the stationary phase.
Instrumentation
1.Solvent reservoir and degassing system
2. Pumping System (Screw- driven syringe pump, Reciprocating pump, Pneumatic or constant- pressure pump)
3. Sample injection system(Septum injectors, Stop flow septum- less injection, Micro- volume sampling valves)
4. Columns- (1. Guard columns 2.separating column)
5. Detectors( The commonly used detectors in HPLC are
Bulk property detectors- examples
1. Refractive-index detectors
2. Conductivity detectors
Solute property detectors- Examples
1. UV detectors
2. Fluorescence detectors
Multipurpose detectors- Example-
1. Perkin-Elmer 3D system (UV absorption+ fluorescence + conductometric detection altogethers)
Electrochemical Detectors- Examples
1.Amperometric, 2. Coulometric detectors)
6. Recorder( There are various types of data processors; from a simple system consisting of the in-built printer and word processor while those with software that are specifically designed for an LC system which not only data acquisition but features, like peak-fitting baseline correction, automatic concentration calculation, molecular weight determination, etc.) Type of HPLC- Normal phase, Reverse Phase, ion exchange, size exclusion, Applications-Stability study- eg Atropin
Bioassays- HPLC is commonly used for the bioassay and analysis of peptide harmones and some antibiotics- cotrimoxazole, penicillins, sulphates and chloramphenicol
In cosmetic industries- used for analyzing the quality of various cosmetic products such as lipsticks, gels, creams etc
Isolation of Natural pharmaceutically Active Compounds– use in the isolation of different type of Alkaloids and Glycosides ( analysis of cinchona, liquorice, ergot extracts and digitalis.)
Control of microbiological processes- HPLC is used in analyse antibiotics (eg. Tetracyclines, chloramphenicol, strptomycin and penicillins )
Assay of cephalosporins
Advantage, Limitation
Gel chromatography, Introduction, Theory, Instrumentation, Applications .pptxVandana Devesh Sharma
Affinity chromatography- Content-Introduction
Theory
Instrumentation
Applications
Gel chromatography is a type of partition chromatography used for separating different sized molecules.
Gel chromatography is also called Gel permeation chromatography or gel filtration or gel exclusion, size exclusion, molecular- sieve chromatography.
The separation is based on the analyte molecular sizes since the gel behaves like a molecular sieve.
In size exclusion chromatography, the stationary phase is a porous matrix made up of compounds like
cross-linked polystyrene, cross-like dextrans, polyacrylamide gels, agarose gels, etc.
The gel structure being used contains pores of different diameters upto maximum size.
1.The test molecules are washed through a gel column and molecules larger than the largest pores in the gel are excluded from the gel structure.
2. Smaller molecules penetrate the gel and the extent of penetration depends on the molecular size----- This delay their movement through the column
This technique is used for the separation of proteins, polysaccharides, enzymes, and synthetic polymers. Instrumentation- A. Stationary phase- It is composed of semi-permeable, porous polymer gel beads with a well-defined range of pore sizes. eg. Dextran, Agarose, Acrylamide. 2. sample size and concentration- sample is applied in small volume (1-5% of the total bed volume).3. Column parameters- use long column, ratio of column diameter to column length (1:20 to :100). The method or steps used for gel preparation. 4. Choice of eluent/mobile phase- Buffers Ex- Phosphate buffer pH 7, NaCl solution, Ammonium acetate (CH3COO-NH4+ ), Ammonium bicarbonate (NH₄HCO₃) ethylenediamine acetate. 5. Effect of Flow rate- maintain with the help of pump. Elution carried out with buffer at optimal flow rate (Eg- 0.25-5ml/min) to give maximum resolution with optimal separation time.6. Separation of components from the sample-
Separation of component from mixture is achieved with the help of column. The retention volume (VR).7. Detection- Using UV absorption detectors. A graph of Elution Volume (ml) Vs Molecular weight. 7. Detection- Using UV absorption detectors. A graph of Elution Volume (ml) Vs Molecular weight. For calibration of the gel in column – Calibrators - (Proteins of known molecular weight. Procedure for gel filtration technique-1. Preparation of column- 2. Washing of the column- 3. Loading of the sample-4. Elution using mobile phase (buffers)5. Detection of compounds . Applications
Fluorimetry part 2, Instrumentation, single beam and double beam, light sourc...Vandana Devesh Sharma
Flourimetry- instrumentation (single beam and double beam flourimeter),Light source
Monochromators / filters
Sample cells/cuvettes
Detectors and
Polarisers
1.Light sources- The radiant energy required for exciting the fluorescent molecule or fluorophore is supplied by the light source.
The fluorescent molecules become excited only at certain wavelength range of the source, therefore, the source should supply energy only at these wavelengths.
2.Monochromators/Filters
A. Filters- made up of
The glass or dye containing wratten filters
Filters- Primary filter and secondary filter
The primary filter- Selects the UV radiation while
The secondary filter transmits visible fluorescent radiation
B.Monochromators- Prisms, gratings
Now a days prism are more used
Monochromator adjusts the angle which the (of) incident radiation makes with the grating surface after striking.
2 gratings are used 1. for incident light and 2. for emitted light
Sample cells/Cuvettes (Glass Cuvettes,Quartz cuvettes,Matched quartz cuvettes)4. Detectors-
(Photomultiplier tube) Working
Potentiometry, Electrochemical cell, construction and working of indicator an...Vandana Devesh Sharma
Potentiometry - Electrochemical cell -Construction and working of reference (Standard hydrogen, silver chloride electrode and calomel electrode)
Indicator electrodes (metal electrodes and glass electrode)
Methods to determine end point of potentiometric titration
and applications
Potentiometry is the method to find the concentration of solute in
A given solution by measuring the potential between two Electrodes
(reference and Indicator electrode) . Potentiometric titration involves
the measurement of the potential of the indicator electrode and
reference electrode.
In potentiometric titration reference and indicator electrodes are
immersed in the solution of particular analyte (titrand) and
potential of indicator electrode is measured with relation to
reference electrode.
Titrant is added in analyte (Titrand) and change in potential is noted
down.
At the end point there is sharp change in potential on indicator
electrode.
Graph is plotted between the indicator electrode potential and
volume of titrant added.
This method is used for determination of sharp end point.
Types of Potentiometric Titration
1. Acid-base titration 2. Redox Titration 3.Complexometric titration 4. Precipitation Titration
content- Principle
Ilkovic equation
Construction and working of dropping mercury electrode and rotating platinum electrode
Applications
Polarography is a voltammetric technique in which chemical species (ions or molecules) undergo oxidation (lose electrons) or reduction (gain electrons) at the surface of a dropping mercury electrode (DME) at an applied potential. Polarography only applies to the DME.
Objective of polarography
Polarography is an electroanalytical technique that measures the current flowing between two electrodes in the solution (in the presence of gradually increasing applied voltage) to determine the concentration of solute and its nature respectively
Polarography is based upon the principle that gradually increasing voltage is applied between two electrodes, one of which is polarisable (dropping mercury electrode) and other is non-polarisable and current flowing between the two electrodes is recorded.
A sigmoid shape current-voltage curve is obtained from which half wave potential as well as diffusion current is calculated.
Diffusion current is used for determination of concentration of substance.
Half wave potential is characteristic of every element.
Ilkovic equation is a relation used in polarography relating the diffusion current (id) and the concentration of the non-polarisable electrode, i.e., the substance reduced or oxidised at the dropping mercury electrode (polarisable electrode).
Definitions of types of currents
1. Residual current (ir), 2. Migration current (im): , 3. Diffusion current (id) 4.Half wave potential 5. Limiting current (il)
Dropping mercury electrode- Dropping mercury electrode (DME) is a polarisable electrode and can act as both anode and cathode.
The pool of mercury acts as counter electrode,
i.e., anode if DME is cathode or
cathode if DME is anode.
The counter electrode is a non-polarisable electrode.
To the analyte solution, electrolyte like KCl is added i.e., 50-100 times of sample concentration.
Pure nitrogen or hydrogen gas is bubbled through the solution, to expel (remove) out oxygen.
Eg: If the analyte solution contains cadmium ions, then cadmium ions are discharged at cathode (-)
Cd2+ + 2e- → Cd
Then, gradually increasing voltage is applied to the polarographic cell and current is recorded.
Graph is plotted between voltage applied and current. This graph is called Polarograph and the apparatus is known as Polarogram.
The diffusion current produced is directly proportional to concentration of analyte and this is used in quantitative analysis.
The half wave potential is characteristic of every compound and this is used in qualitative analysis.
Graph is plotted between voltage applied and current. This graph is called Polarograph and the apparatus is known as Polarogram.
The diffusion current produced is directly proportional to concentration of analyte and this is used in quantitative analysis.
The half wave potential is characteristic of every compound
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
The French Revolution, which began in 1789, was a period of radical social and political upheaval in France. It marked the decline of absolute monarchies, the rise of secular and democratic republics, and the eventual rise of Napoleon Bonaparte. This revolutionary period is crucial in understanding the transition from feudalism to modernity in Europe.
For more information, visit-www.vavaclasses.com
Unit 8 - Information and Communication Technology (Paper I).pdfThiyagu K
This slides describes the basic concepts of ICT, basics of Email, Emerging Technology and Digital Initiatives in Education. This presentations aligns with the UGC Paper I syllabus.
Synthetic Fiber Construction in lab .pptxPavel ( NSTU)
Synthetic fiber production is a fascinating and complex field that blends chemistry, engineering, and environmental science. By understanding these aspects, students can gain a comprehensive view of synthetic fiber production, its impact on society and the environment, and the potential for future innovations. Synthetic fibers play a crucial role in modern society, impacting various aspects of daily life, industry, and the environment. ynthetic fibers are integral to modern life, offering a range of benefits from cost-effectiveness and versatility to innovative applications and performance characteristics. While they pose environmental challenges, ongoing research and development aim to create more sustainable and eco-friendly alternatives. Understanding the importance of synthetic fibers helps in appreciating their role in the economy, industry, and daily life, while also emphasizing the need for sustainable practices and innovation.
Macroeconomics- Movie Location
This will be used as part of your Personal Professional Portfolio once graded.
Objective:
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.
How to Make a Field invisible in Odoo 17Celine George
It is possible to hide or invisible some fields in odoo. Commonly using “invisible” attribute in the field definition to invisible the fields. This slide will show how to make a field invisible in odoo 17.
3. Principle of flame photometry-2
Give principle, interferences and applications of flame
photometry.-5
Different type of burners used in flame photometry.- 8
Write a short note on instrumentation of flame photometry. 8
Explain the instrumentation of flame photometer and describe
the methods of analysis of a sample.-8
What is the principle of flame photometry? Discuss
instrumentation of flame photometer.-8
Write a short note on instrumentation of flame photometry. 8
4. During 1980s Bowling Barnes, David Richardson, John Berry and
Robert Hood developed an instrument to measure the low
concentrations of sodium and potassium in a solution. They
named this instrument as Flame photometer.
The principle of flame photometer
is based on the measurement of the emitted light intensity when
a metal is introduced into the flame.
The wavelength of the colour gives information about the
element and
the colour of the flame gives information about the amount of
the element present in the sample.
Flame photometry is one of the branches of atomic absorption
spectroscopy.
It is also known as flame emission spectroscopy.
Currently, it has become a necessary tool in the field of
analytical chemistry.
5. Used to
Determine the concentration of certain metal ions like
potassium,
lithium,
calcium
cesium etc.
In flame photometer spectra the metal ions are used in the
form of atoms.
(IUPAC) Committee on Spectroscopic Nomenclature has
named this technique as flame atomic emission spectrometry
(FAES).
Note- IUPAC
The International Union of Pure and Applied Chemistry
sodium,
6. Principle of Flame photometer
The compounds of the alkali and alkaline earth metals (Group II)
dissociate into atoms when introduced into the flame.
Some of these atoms further get excited to even higher levels.
But these atoms are not stable at higher levels.
Hence, these atoms emit radiations when returning back to the
ground state.
These radiations generally lie in the visible region of the
spectrum.
Each of the alkali and alkaline earth metals has a specific
wavelength.
Element Emitted wavelength Flame color
Sodium 589 nm Yellow
Potassium 766 nm Violet
Barium 554 nm Lime green
Calcium 622 nm Orange
Lithium 670 nm Red
7. For certain concentration ranges,
The intensity of the emission or the light emitted ά the number
of atoms returning to the ground state or the concentration of the
sample.
Liquid sample
Formation of droplets
Fine residue
Formation of neutral atoms
Excitation of atoms by thermal energy
Emission of radiation of specific wavelength
λ& Intensity of emitted radiation measured
8. NOTE-
The wavelength of the radiation emitted is characteristic of the
elements and is used to identify the elements (Qualitative
Analysis).
The intensity of the radiation emitted depends upon the
concentration of the element analysed (Quantiative Analysis).
9.
10.
11.
12. The wavelength of the radiation emitted is given by the
following equation :-
λ = hc/ E2-E1
Where,
h = Planks constant
c= Velocity of light
E2 = energy levels of exited and
E1 =ground state respectively
BOLTZMAN LAW
The fraction of free atom that are thermally exited is governed
by a Boltzman Distribution
N* / N = Ae–∆E/kT
N* =is the number of exited atom
N = is the number of atom remainin in the ground state
ΔE = is the difference in energies levels
k = The Boltzman constant
T = the tempeature
13.
14. Additional information
Each element will emit radiation at wavelength specific for that
element.
The whole process can be categorised as below
1. Desolvation-The particles in the flame are dehydrated by the
flame and process of desolvation takes place. Water and other
solvent is vaporized leaving minute particles of dry salt
CaCl2 (solution) ----- CaCl2 (solid)
2. Vaporization- Evaporation of the solvent occurs as the second
step at the high temp of the flame
CaCl2 (Solid) ------- CaCl2 (Gas)
Atomization- Flame heat converts a part of all the gaseous
molecules/ metal particles to give neutral ions
Ionization and Excitation- The vapours of neutral atoms or
molecules containing the metal atoms are excited by the thermal
energy of flame resulting into ionization and excitation of neutral
atoms.
The electrostatic force of attraction between the electrons and
nucleus of the atom helps them to absorb a particular amount of
energy. The atoms then shifted to the excited energy state.
15. Emission process-
The excited energy state is unstable and atom return to the
initial stable lower energy state with the emission of energy in
the form of radiation of characteristic wavelength, which is
measured by the photo detector.
To obtain emission spectra, suitable flames are required.
Example-
CaCl2 (solution) CaCl2 (solid) CaCl2 (gas)
CaCl2 (g) Cl2 (g) + Ca (g)
Δ
Aspiration vaporization
Dissociation by
Δ
Flame
16. All the species example
Ionized atom and neutral atom of Ca, molecule of CaO and CaOH
Are excited by thermal energy of flame
these Ionized atom and neutral atom of Ca, molecule of CaO and
CaOH fall to the ground state
Emission spectra are produced
Type 1 spectra- those containing lines originated from excited atoms or
ions
Type 2 spectra- the band of spectra resulting from molecules
From this excited state when
18. Gases eg. Acetylene, Hydrogen,
Propane, butane
Oxidant-
oxygen or
(Condensing)
Slit
Prism
Photomultiplier
Total consumption burner
Premixed burner-
Filter
19.
20. A simple flame photometer consists of the following basic
components:
Source of flame: A Burner in the flame photometer is the source of
flame.
It can be maintained in at a constant temperature.
The temperature of the flame is one of the critical factors in
flame photometry.
Fuel-Oxidant mixture Temperature (°C)
Natural gas-Air 1700
Propane-Air 1800
Hydrogen-Air 2000
Hydrogen-Oxygen 2650
Acetylene-Air 2300
Acetylene-Oxyen 3200
Acetylene-Nitrous oxide 2700
Cyanogen-Oxygen 4800
21. Nebuliser: Nebuliser is used to send homogeneous solution into
the flame at a balanced rate.
Monochromator:
Filters are generally made from materials which are transparent in
a small selective wavelength region.
The filter chosen -has a wavelength range in which it is
transparent to emission from the element of interest.
A condenser lens system is employed to collect the emitted light
and sends the rays through the filter as an approximately
collimated (parallel) beam to reach the detector.
Filters have been designed for use in the determination of
lithium, sodium, potassium, calcium and other elements.
The radiation source-- emits the polychromatic light which--
contains the wide range of frequencies.
Monochromators are used for converting the polychromatic light
into monochromatic light.
Eg. of monochromators are prism and grating monochromators.
Prism monochromators: When polychromatic light passes
through the prism, it is refracted.
22. Grating monochromators: Grating is nothing but the lines made
on the glass which is previously coated with aluminium.
Rotation of these gratings converts the polychromatic light to
monochromatic light more efficiently when compared to prism
monochromators.
DETECTOR :-
The radiation emitted by the elements is mostly in the visible
region and measured by photo detector.
Hence conventional detectors like photo voltaic cell or photo
tubes or photomultiplier tube is used as detector In a flame
spectrophotometer Here the emitted radiation is converted to an
electrical signal with the help of photo detector.
These electrical signals are directly proportional to the intensity
of light emitted.
READ OUT DEVICE :-
The signal from the detector is shown as a response in the digital read
out device. The readings are displayed in an arbitrary scale (% Flame
Intensity).
23.
24. Working procedure
Both the standard stock solution and sample solution are
prepared in fresh distilled water.
The flame of the photometer is calibrated by adjusting the air
and gas. Then the flame is allowed to stabilize for about 5 min.
Now the instrument is switched on and the lids of the filter
chamber are opened to insert appropriate colour filters.
The readings of the galvanometer are adjusted to zero --by
spraying distilled water into the flame.
The sensitivity is adjusted --by spraying the most concentrated
standard working solution into the flame. Now the full scale
deflection of the galvanometer is recorded.
Again distilled water is sprayed into the flame -- to attain
constant readings of galvanometer. Then the galvanometer is
readjusted to zero.
Now each of the standard working solutions is sprayed into the
flame for three times and the readings of galvanometer are
recorded. After each spray, the apparatus must be thoroughly
washed.
25. Finally sample solution is sprayed into the flame for three times
and the readings of galvanometer are recorded. After each
spray, the apparatus must be thoroughly washed.
Calculate the mean of the galvanometer reading.
Plot the graph of
concentration against the galvanometer reading
to find out the concentration of the element in the sample.
26. Flame photometer as measures the emitted radiation, the optical
and electronic system is used in spectrophotometer is similar.
Any model of flame photometer consists of the following parts:
1. Fuel gas, Pressure regulator or flow meter
2. The atomizer
3. The optical system
4. Photosensitive detectors
5. Recording or reading meter
Note-
1. Fuel gas- Propane, Butane, Hydrogen, Acetylene
2. The atomizer- Flame Atomiser: I) Flames II) Burners
Non flame Atomizers- 1) Graphite Furnace 2) Electrical
discharges 3) Plasmas
3. Optical System- Filters (Na, K, Ca, Li etc )and monochromator
(diffraction grating or prism)
4. Photosensitivity detector- Photomultiplier
5. Recording - Galvanometer
27.
28. 1. Fuel gas, Pressure regulator or flow meter
fuel gas is burnt in the burner - In order to supply suitable
thermal energy through flame
Region A -The unburnt fuel gas emerging from this region. Eg of
fuel gas- Propane, Hydrogen, Acetylene
Pre-heating region B - Fuel gas mixes with oxidant (air/oxygen)
at outlet of burner comes into this region.
Gases emerging from this mainly consist of CO, H2, CO2, and
hydrocarbons.
On burning, a steady temperature is provided throughout the
outer mantle of flame.
29. To supply sufficient temperature between 1000-3000o
C fuel
gases are used. Eg of fuel gases-
1. Coal gases (Hydrogen 50% Methane 35% Carbon monoxide 10%)
2. Illuminating gas ( Propane, Acetylene)
3. Cooking gas (Propane and butane)
Mixture of fuel gas with (oxidant) air/oxygen = to obtain
sufficient high temperature
Fuel-Oxidant mixture Temperature (°C)
Natural gas-Air 1700
Propane-Air 1800
Hydrogen-Air 2000
Hydrogen-Oxygen 2650
Acetylene-Air 2300
Acetylene-Oxyen 3200
Acetylene-Nitrous oxide 2700
Cyanogen-Oxygen 4800
30. Fuel gas generally obtained from – Cylinders (Store under
pressure)
To obtain steady flame for giving emission (release)= gas
pressure and gas flow (by operating capillary flow rate meter or
rotameter) is maintained constant.
Fuel gas generally obtained from – Cylinders (Store under
pressure)
To obtain steady flame for giving emission (release)= gas
pressure and gas flow (by operating capillary flow rate meter or
rotameter) is maintained constant.
Rotameter
Cylinder
31. 2. Atomizer-
Atomization and Excitation:
Atomization --is the process of converting a solid, liquid, or
solution to be analyzed into a free gaseous atom– usually by a
thermal energy using various sources.
Excitation is the process - the outer most electrons of atoms
absorb energy and shifted to higher energy state. (means the
same source of thermal energy serves as the excitation source)
Atomization and excitation is the process involved in all atomic
spectroscopic techniques.
The common sources used for atomization are
1. Flames
2. Burners
Purpose of atomizer- is to introduced liquid sample into flame at
stable and reproducible rate
Qualities of atomizer –
Should remain unaffected by solutions and solvents
Can be readily cleaned and shold be sturdy in nature
Flame Atomiser
32. Atomizer can be classified in to 2 types
Flame Atomiser: I) Flames II) Burners
Non flame Atomizers- 1) Graphite Furnace 2) Electrical
discharges 3) Plasmas
Flame Atomizer:
I) Flames-Most of molecules are dissociated into free atoms and
excited by heating energy produced by flames
Premixed flame- Premixed flames occur
in any homogeneous mixture where the
fuel and the oxidant are mixed before to
the reaction or combustion.
Ex. the Bunsen burner flame
Diffusion flame -When the
oxygen feeding the
combustion gets to the flame
from the air, the flame is
called diffusion flame.
Eg. a candle flame
33. Fuel and oxidants-
Fuel and oxidant required-- to produced flame
Combination of fuel and oxidants is important--- It should be
suitable for conversation of samples-- to neutral atoms --
followed by the excitation of atoms
Temperature of flame plays a major role-
High temprature of flame - the elements in sample may get
convert into ions instead of neutral atoms.
Similarly with low temperature of flame there may not be
excitation of atoms occurs
NOTE- so a combination of fuel and oxidants is used in such that
there is desired temperature to facilitate atomization and
excitation.
Structure of flame-
the flame may be divided into the following regions or zones:
1. Preheating zones.
2. Primary reaction zone or inner zone.
3. Internal zone.
4. Secondary reaction zone.
34. Primary combustion Zone/Primary reaction zone- Don't take part
in the flame emission process– Usually blue in color
Interconal regions-
take part in emission process- Most important region.
It is rich in free atoms and involve in the excitation process.
The outer zone- covert the products to stable oxide
Or inner
zone
35. 1.Burner :-
Main requirement of burner is that when fuel gas
is supplied along with air/oxygen at a constant
pressure, it should produce a steady flame.
For low temperature flame Meeker burner is used.
It carries a metal grid across the burner open tube
which prevent flame from striking back down.
There are two common types of atomizer burner
employed in flame photometers. These are-
Total consumption burner
Premixed burner- The sample is nebulized and
mixed with the fuel and oxidant prior to
introduction into the flame, with the used of a
series of buffles
Sample is drawn from the sample container via
vacuum created by rushing the fuel and oxidant
(Aspiration)
Advantage of is the uniformity of flame produced.
Open tube
metal grid
Across
the burner
Meeker Burner
38. Total consumption burner
It consist of inlets for fuel and
oxidants at the base of the apparatus
Sample is also kept at the base to be
aspirated.
Acetylene -commonly used as fuel
and air -used oxidant are forced,
under pressure, into the flame
The sample is drawn into the flame
by aspiration by vacuum created
because of movement of fuel and
oxidant.
The aspirated sample reaches-- the
burner head with a nebulizing effect.
This sample is mixed with fuels and
oxidant at the base of the flame.
Advantage over other is the entire
consumption of sample,
Limitation
The resulting flame is turbulent and
not homogeneous
Acetylene
air
39. 3.Optical system-
Function-
1. Is to collect the light from steady flame, render it
Monochromatic by means of lens, prism, --and focus on to the
phototube.
2. Concave mirror- placed behind flame to collect scattered
radiation and focus back into flame- By this mechanism intensity
of emitted light is nearly doubled
Filters and monochromator -are needed to isolate the light of
specific wavelength from the remaining light of the flame
Simple filter is sufficient in case of few elements Ca, Na, K and Li.
So a filter wheel with filter is for filter is taken with instrument
Type of filter- 1) absorption glass filter 2) interference filter
Interference filter is better
Glass absorption filters are used to pass a specific band of
wavelengths.
Interference Filters - These filters differ from absorption filters in
the fact that they reflect and destructively interfere with
unwanted wavelengths as opposed to absorbing them.
40.
41. Dispersion medium- Prism or Diffraction grating is employed in
flame spectrophotometer
4. Photo- Detector-
Phototube
Photo- multiplier
Barrier layer cell
Or diffraction grating
45. The method of analysis is very simple and
economical.
It is quick, convenient, selective and sensitive
analysis.
It is both and qualitative and quantitative in
nature.
Even very low concentrations (parts per
million/ppm to parts per billion/ppb range) of
metals in the sample can be determined.
This method compensates for any unexpected
interfering material present in the sample
solution.
This method can be used to estimate elements
which are rarely analyzed.
46. In spite of many advantages, this analysis technique has quite a
few disadvantages:
The accurate concentration of the metal ion in the solution
cannot be measured.
It cannot directly detect and determine the presence of inert
gases.
Though this technique measures the total metal content present
in the sample, it does not provide the information about the
molecular structure of the metal present in the sample.
Only liquid samples may be used. Also sample preparation
becomes lengthy in some cases.
Flame photometry cannot be used for the direct determination of
each and every metal atom. A number of metal atoms cannot be
analysed by this method.
The elements such as carbon, hydrogen and halides cannot be
detected due to their non-radiating nature.
47. 1. Flame Temperature-
It is very essential to have proper temperature of flame to bring
about excitation and release of energy
If flame temperature is very low – It would be insufficient to cause
vaporization, dissociation and excitation of atom.
No line or weak lines would be obtained
The temperature should not be too high to have deteriorating
effect
2. Chemical interference-
When another component is present in the sample as impurity,
error occurs.
The magnitude of error depends upon -
the ratio of concentration of contaminant with the element under
examination
48. In determination of certain metal ions (cations), anions present
in the solution have depressant effect on the intensities of
number of cation liones, eg. More than 5% oxalate, sulphate,
phosphate ions bring decrease in emission intensities of alkaline
earth cations
Thus the contaminants are present, they need to be eliminated
by precipitations/complexations or by other methods.
3. Radiation interference-
Sometimes, presence of certain element, causes radiation
interference-- by emitting light of wavelength, identical to that
of element under examination.
The detector is thus unable to distinguish the line and their
intensities.
This difficulty is generally eliminating by removing the
interfering element or by adding an identical amount of the
solution for constructing calibration curves
49.
50. Flame photometry is widely used in various chemicals and
pharmaceuticals, soils and agriculture, ceramics and glass, plant
materials and water, oceanography, and in biological and
microbiological laboratories
1. Determination of Na, K, Ca, and Mg in biological fluids like
serum, plasma, urine etc is routinely carried out by flame
photometer
2. Analysis of industrial water, natural water for determining
elements responsible for hard water (like Ca, Mg, Ba etc) is
standard procedure in many laboratories
3. Soil samples are routinely analyzed mainly for Na and K and also
for Ca and Mg (after removing other interfering elements) by
flame photometer
4. Some important elements which are commonly determined by
this method are Al, Ba, Ca, cesninum, chromium, Cu, Fe, lead,
Mg, Manganese, K, Na, strontium and zinc
51. 5. In glass industry- flame photometry is used in determination of
Na, K, boron, lithium etc
6. In cement industry, this method is used in estimation of Sodium
(Na2O), Potassium (K2O), Calcium (CaO), magnesium (MgO),
manganese (MnO2) and Lithium (Li2O).
7. Flame photometry used in estimation of alkali-alkaline earth
metals besides other metals present in metallurgical products,
catalysts, alloys etc.
8. Flame photometry has also been used in determination of certain
metals like lead, manganese, in petroleum products like gasoline,
lubricating oils and organic solvents.
9. Analysis of ash by flame photometer is routinely carried out in
various industries for estimating alkali and alkaline earth metals
as their oxides
52. 1. Which of the following is the principle of Flame emission
photometers?
a) Radiation is absorbed by non-excited atoms in vapour state and are
excited to higher states
b) Medium absorbs radiation and transmitted radiation is measured
c) Colour and wavelength of the flame is measured
d) Only wavelength of the flame is measured
2. Which of the following is not an advantage of Laminar flow burner
used in Flame photometry?
a) Noiseless
b) Stable flame for analysis
c) Efficient atomization of sample
d) Sample containing two or more solvents can be burned
efficiently
3.Which of the following is not a detector used in Flame emission
photometers?
a) Photronic cell
b) Photovoltaic cell
c) Photoemissive tube
d) Chromatogram
53. 4. If Propane and air are used in burner how many °C temp. is
produced ?
a)1900°C
b)2200°C
c)2300°C
d)2100°C
5. If Hydrogen and air are used in burner how many °C temp. is
produced ?
a)1900°C
b)2200°C
c)2300°C
d)2100°C
6. Which is not application of flame photometry ?
a)To estimate sodium, magnesium, calcium
b) Assay of metformin.
c)Used to determine magnesium and calcium in cement.
d) To detected metalic ions in sample.
54. 7. BOLTZMANN Equations is
a)N* / N =R Ae–∆E/kT
b)N* / N = e–∆E/kT
c)N* / N = Ae–∆E/kT
d)N* / N = Ae–∆E/kc
8. Choose correct sequence of flame photometry ?
a) Sample residue → excited state atoms → Return in ground
state → Emission of radiation
b)Sample residue → ground state → excited state → Emission of
radiation
c) Emission of radiation → excited state →ground state → Sample
residue
d) Sample residue → ground state → excited state → Emission of
radiation
9. Which equations are used to determine wavelength of radiation ?
a)λ = hc/ E2-E1
b)N* / N = e–∆E/kT
c) λ = h/E2-E1
d)N* / N = Ae–∆E/kT
55. 10. Which is application of flame photometry ?
a) To determine functional group
b) To study of chemical structure
c) To assay of drug
d) To estimate metalic ions like sodium, potassium, etc.