Flame photometery DMLT 2ND

288 views 48 slides Jun 06, 2021
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About This Presentation

DMLT STUDENT MATERIAL


Slide Content

Compiled and Edited By
Prof. S. Salunke Sir
Msc, CMLT, DMLT, MLT, DLT.
2021 -2022
DMLT 2
nd
Year
1Pro S.Salunke Sir

I. Instrumental method of bio –chemical analysis
2
FlamePhotometer
Pro S.Salunke Sir

II. The flame photometers from A.Krüssare used to determine the
concentration of alkali and alkaline earth elements in aqueous solutions and
are a simple and particularly cost-effective alternative to analysis techniques
such as ICP or AAS
3
Flame photometer -Automatic unit with dilution
FP8700
Pro S.Salunke Sir

III. Lcd Display Microprocessor Flame Photometer, For Industrial
Use , Laboratory Use,
4
Flame photometer -Model: SSE-671
Pro S.Salunke Sir

5Pro S.Salunke Sir
In This Slides
Principle
Mechanism
•Nebulisation
•Brief overview of process in the flame
Applications
Advantages
Disadvantages
Introduction
Atomic spectroscopy
Types of Atomic Spectroscopy
Flame Photometry
Instrumentation
Parts of flame photometer

6
INTRODUCTION
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 color gives information about the element
and the color of the flame gives information about the amount of the
element present in the sample.
1980 च्यादशकातबॉल िंगबार्न्स, डेव्हिडरिचडससन, जॉनबेिीआलििॉबर्सहूडयािंनीसोल्यूशनमध्येसोलडयमआलि
पोर्ॅलशयमचीकमीप्रमािमोजण्यासाठीएकसाधनतयािके े.
त्ािंनीयावाद्या ाफ्लेमफोर्ोमीर्िअसेनावलद े. फ्लेमफोर्ोमीर्िचेलसद्ािंतमोजमापाविआधारितआहेजेिाज्योतीत
धातूचापरिचयहोतोतेिाउत्सलजसतप्रकाशाचीतीव्रता. ििंगाचीतििंगदैध्यसनमुनाउपव्हथितघर्कत्ाघर्कालवषयीमालहतीदेते
आलिज्योतचाििंगत्ाती प्रमािािंलवषयीमालहतीदेतो.
Pro S.Salunke Sir

Pro S.Salunke Sir 7
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.
Flame photometer can be used to determine the concentration of certain metal
ions like sodium,potassium,lithium, calcium and cesiumetc.
In flame photometer spectra the metal ions are used in the form of atoms.
The International Union of Pure and Applied Chemistry (IUPAC) Committee on
Spectroscopic Nomenclature has named this technique as flame atomic emission
spectrometry (FAES).
फ्लेमफोर्ोमेर्रीअिुशोषिस्पेक्ट्रोस्कोपीच्याशाखािंपैकीएकआहे.
या ाज्योतउत्सजसनस्पेक्ट्रोस्कोपीअसेहीम्हितात.
सध्याहेलवश्लेषिात्मकिसायनशास्त्रक्षेत्रातआवश्यकसाधनबन ेआहे. सोलडयम, पोर्ॅलशयम, ल लियम, कॅ व्हशशयमआलिसीलियम
इत्ादीलवलशष्टधातूिंच्याआयनचीएकाग्रतालनलितकिण्यासाठीज्योतफोर्ोमीर्िवापि ाजाऊशकतो. ज्योतप्रकाशमापकस्पेक्ट्रामध्ये
धातूचेआयनअिूच्यारूपातवापि ेजातात. इिंर्िनॅशन युलनयनऑफप्यूि.ण्डअप्लाइडके लमस्ट्री(आयईयूपीएसी) च्या
स्पॅक्ट्रोस्कोलपकनॉमनेक्लचियासलमतीनेयातिंत्रा ाज्योतअिुउत्सजसनस्पेक्ट्रोमेर्री(एफएईएस) असेनावलद ेआहे.

Pro S.Salunke Sir 8
In 1860 Robert Bunsen and
Gustav Kirchhoff discovered
two alkali metals, cesium and
rubidium, with the aid of the
spectroscope they had invented
the year before.
These discoveries inaugurated
a new era in the means used
to find new elements.
The potential of atomic spectroscopy in both the qualitative as well as
quantitative analysis were then well established.

Pro S.Salunke Sir 9
Atomic spectroscopy is an unavoidable tool
in the field of analytical chemistry.
It is divided into Threetypes which are
1 Absorption Spectroscopy
2 Emission Spectroscopy
3 Luminescence Spectroscopy
Another branch of atomic absorption spectroscopy is
❖Flame photometry or Flame Atomic Emission spectrometry
(in which the species is examined in the form of atoms)
❖Atomic Absorption Spectrophotometer (AAS)
❖Inductively coupled plasma –Atomic emission spectrometry (ICP-AES)

Pro S.Salunke Sir 10
Principle of Flame photometer
The basic principleupon which Atomic
Spectroscopy works is based on the fact that
"Matter absorbs light at the same
wavelength at which it emits light.”
When a metal salt solution is burned, the
metal provides a colored flame and each
metal ion gives a different colored flame.
Flame tests, therefore, can be used to test
for the absence or presence of a metal ion.
Atoms of
elements
Subjected to
hot flame
Specific quantum of
thermal energy
absorbed by orbital
electrons
Become
at high energy
level
Release energy as
photons of
particular
wavelength
Change back to
ground state

Pro S.Salunke Sir 11
The potential of atomic spectroscopy in both
the qualitative as well as quantitative analysis were then well established.
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

Pro S.Salunke Sir 12
instrumentation
Parts of a Flame Photometer
❖Source of Flame
A burnerthat provides flame and can be maintained in a constant form
and at a constant temperature.
❖Nebulizer and Mixing Chamber
Helps to transport the homogeneous solution of the substance into the flame at a steady
rate.
❖Optical System (Optical Filter)
The optical system comprises three parts: convex mirror,lensand filter. The convex mirror
helps to transmit light emitted from the atoms and focus the emissions to the lens. The convex lens help to focus
the light on a point called slit. The reflections from the mirror pass through the slit and reach the filters. This will
isolate the wavelength to be measured from that of any other extraneous emissions. Hence it acts as interference
type color filters.
❖Photo Detector
Detect the emitted light and measure the intensity of radiation emitted by the flame. That is, the emitted
radiation is converted to an electrical signal with the help of photo detector. The produced electrical signals are
directly proportional to the intensity of light.

Pro S.Salunke Sir 13
instrumentation
Parts of a Flame Photometer
❖Source of Flame
A burnerthat provides flame and can be maintained in a constant form
and at a constant temperature.
❖Nebulizer and Mixing Chamber
Helps to transport the homogeneous solution of the substance into the flame at a
steady rate.
❖Optical System (Optical Filter)
The optical system comprises three parts: convex mirror,lensand filter. The convex
mirror helps to transmit light emitted from the atoms and focus the emissions to the lens. The convex
lens help to focus the light on a point called slit. The reflections from the mirror pass through the slit and
reach the filters. This will isolate the wavelength to be measured from that of any other extraneous
emissions. Hence it acts as interference type color filters.
❖Photo Detector
Detect the emitted light and measure the intensity of radiation emitted by the flame. That is, the emitted
radiation is converted to an electrical signal with the help of photo detector. The produced electrical
signals are directly proportional to the intensity of light.
13

Pro S.SalunkeSir 14
Schematic diagram showing flame photometer
instrumentation

Pro S.Salunke Sir 15
Schematic diagram showing flame photometer
instrumentation

Pro S.Salunke Sir 16
Schematic diagram showing flame photometer
instrumentation

17Pro. S. Salunke Sir
Schematic diagram showing flame photometer
instrumentation

18Pro. S. Salunke Sir
Nebulization
“A dispenser that turns a liquid into a fine mist called nebulizer (such as
perfume).” The solution of the substance to be analyzed is first aspirated into
the burner, which is then dispersed into the flame as fine spray particles.
A brief overview of the process
The solvent is first evaporated leaving fine divided solid particles.
This solid particles move towards the flame, where the gaseous atoms and
ions are produced.
The ions absorb the energy from the flame and excited to high energy levels.
When the atoms return to the ground state radiation of the characteristic
element is emitted.
The intensity of emitted light is related to the concentration of the element.
Mechanism

19Pro. S. Salunke Sir
In the flame
photometry employs a variety of fuels mainly air,
oxygen or nitrous oxide (N2O) as oxidant.
The temperature of the flame depends on
fuel-oxidant ratio.
The intensity of the light emitted could be described by the
Scheibe-LomakinEquation
??????= ??????×????????????
Where,
??????= Intensity of emitted light
??????= The concentration of the element
??????= Constant of proportionality
??????~1 (At the linear part of the calibration curve)
Then,
??????= ??????×??????
That is the intensity of emitted light is directly related
to the concentration of the sample.
Mechanism

20Pro. S. Salunke Sir
Mechanism

21Pro. S. Salunke Sir
As seen in the figure,
the flame may be divided into following regions or zones
1.Preheating zones
2.Primary reaction zone (inner zone)
3.Internal zone-max temp, used for flame
photometry
4.Secondary reaction zone
Structure of Flame
1
2
3
4

22Pro. S. Salunke Sir
❖a means of transporting a homogeneous solution (converting into a fine
mist) into the flame at a steady rate
❖can be done by passing a gas of high velocity over the upper outlet of
capillary tube, the lower end of which is inserted into the sample
❖Liquid is then drawn up into the chamber and dispersed into small droplets
The fine mist is then burnt in either laminar flow burner or total consumption
burner
❖The aerosol is desolated , vaporized and atomized in the flame of the
burner
Nebulizers or Atomizer

23Pro. S. Salunke Sir
A number of nebulisation methods are available like;
Pneumatic nebulisation
Ultrasonic nebulisation
Electro thermal vaporization
Hydride generation(used for certain elements only).
Pneumatic Nebulizer is the most commonly used nebulizer

24Pro. S. Salunke Sir
Burner (source):
a flame that can be maintained in a constant form and at a constant
temperature
should have ability to evaporate the liquid droplets from the sample solutions
must have capacity to excite the atoms formed and cause them to emit radiant
energy
a cylinder of compressed gas and two stage pressure regulator are required
High pressure tubing must be used to lead the gases to the flame

25Pro. S. Salunke Sir
Pre-mixed Burner:
widely used because uniformity in flame intensity
In this energy type of burner , aspirated sample , fuel and oxidant are
thoroughly mixed before reaching the burner opening.
The fine mist or aerosol of sample solution is produced in a vaporization
chamber
Larger droplets go to waste while the fine mist enters the flame, thus
producing a less noisy single
In addition, the path length through the flame of the burner is longer than
that of the total consumption burner producing greater absorption and
increases the sensitivity of the measurement

26Pro. S. Salunke Sir
Total consumption burner:
Made of 3 concentric tubes:
The central tube is a fine capillary tube
The sample solution is carried up by this tube directly into flame
The fuel gas, the oxidant gas and sample solution is aspirated through a
capillary by high pressure of fuel and Oxidant and burnt at the tip of burner
In this fuel and oxidant are hydrogen and oxygen gases
Entire sample is consumed.

Pro. S. Salunke Sir 27
Made of 3 concentric tubes:
The central tube is a fine capillary tube
The sample solution is carried up by this tube directly into flame
The fuel gas, the oxidant gas and sample solution is aspirated through a
capillary by high pressure of fuel and Oxidant and burnt at the tip of
burner
In this fuel and oxidant are hydrogen and oxygen gases
Entire sample is consumed.
Total consumption burner:

28Pro. S. Salunke Sir

Pro. S. Salunke Sir 29

Pro. S. Salunke Sir 30
Slits: -
Entrance and exit slits
Entrance slit : -Cuts out most of the radiation from the surrounding –
Allows only the radiation from the flame to enter into the
monochromator
Exit slit: -Placed after the monochromator –
Allows only the selected wavelength to pass through the photo
detector

Pro. S. Salunke Sir 31
Monochromator :
❖a means of isolating light of the wavelength to be measured from that of
extraneous emissions
❖When kept between the flame and detector, the radiation of the desired
wavelength from the flame will be entering the detector and be measured
❖Remaining will be absorbed by the monochromator and not measured
❖Either prisms or diffraction gratings
❖ Prism: Quartz material is used for making prism, as quartz is
transparent over entire region
❖ Grating: it employs a grating which is essentially a series of
parallel straight lines cut into a plane surface

Pro. S. Salunke Sir 32
Detectors: -
a means of measuring the intensity of radiation emitted by the flame –
Should be sensitive to radiation of all the wavelengths that has to be analyzed -The flame
instability reduces their accuracy so multichannel polychromator is used in some procedures
Photomultiplier tubes
Photo emissive cell
Photo voltaic cell
Photo emissive cells or photomultiplier tubes are commonly employed for the purpose.
Photovoltaic cell:
It has a thin metallic layer coated with silver or gold which act as electrode, also has metal
base plate which act as another electrode
Two layers are separated by semiconductor layer of selenium, when light radiation falls on
selenium layer.
This creates potential diff. between the two electrode and cause flow of current.

Pro. S. Salunke Sir 33
Flame photometer has both quantitative and qualitative applications.
Flame photometer with monochromators emits radiations of characteristic
wavelengths which help to detect the presence of a particular metal in the
sample. This help to determine the availability of alkali and alkaline earth metals
which are critical for soil cultivation.
In agriculture, the fertilizer requirement of the soil is analyzed by flame test
analysis of the soil.
In clinical field, Na+ and K+ ions in body fluids, muscles and heart can be
determined by diluting the blood serum and aspiration into the flame.
Analysis of soft drinks, fruit juices and alcoholic beverages can also be
analyzed by using flame photometry.
Application

Pro. S. Salunke Sir 34
Simple quantitative analytical test based on the flame analysis.
Inexpensive.
The determination of elements such as alkali and alkaline earth metals is
performed easily with most reliable and convenient methods.
Quite, convenient, selective and sensitive to even parts per million (ppm)
to parts per billion (ppb) range.
Advantages

Pro. S. Salunke Sir 35
The concentration of the metal ion in the solution cannot be measured
accurately.
A standard solution with known molarities is required for determining the
concentration of the ions which will corresponds to the emission spectra.
It is difficult to obtain the accurate results of ions with higher
concentration.
The information about the molecular structure of the compound present in
the sample solution cannot be determined.
The elements such as carbon, hydrogen and halides cannot be detected due
to its non-radiating nature.
Disadvantages

Pro S.Salunke Sir 36
To be continue….

Pro S.Salunke Sir 37
1.Which of the following is the principle of Flame emission photometers?
a)Radiation is absorbed by non-excited atoms in vapor state and are excited to higher states
b) Medium absorbs radiation and transmitted radiation is measured
c) Color and wavelength of the flame is measured
d) Only wavelength of the flame is measured
MCQs

Pro S.Salunke Sir 38
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

Pro S.Salunke Sir 39
3.Which of the following is not a detector used in Flame
emission photometers?
a)Photroniccell
b)Photovoltaic cell
c)Photoemissivetube
d)Chromatogram

Pro S.Salunke Sir 40
4. IfPropane and air are used in burner how many°C temp.
is produced ?
a)1900°C
b)2200°C
c)2300°C
d)2100°C

Pro S.Salunke Sir 41
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

Pro S.Salunke Sir 42
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 metalicions in sample.

Pro S.Salunke Sir 43
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

Pro S.Salunke Sir 44
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

Pro S.Salunke Sir 45
9. Which equations are used to determine wavelength of radiation ?
a)λ= hc/ E
2-E
1
b)N* / N = e
–∆E/kT
c)λ= h/E2-E1
d)N* / N = Ae
–∆E/kT

Pro S.Salunke Sir 46
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 metallic ions like sodium, potassium, etc.

Pro S.Salunke Sir 47
ANSWER KEY :-
1. c
2.d
3.d
4.d
5.a
6.b
7.c
8.a
9.a
10.d

Pro S.Salunke Sir 48
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