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7/21/2019 Atomic Absorption Spectroscopy and Atomic Emission Spectroscopy
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Atomic Spectroscopy
Ashraf M. Mahmoud, Associa
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,
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Atomic SpectroscopyTo understand the relationship of these techniques to each other, It is
important to understand the atom itself and the atomic process
involved in each technique.
Excited
states
Groundstate
λ3
λ3
λ3
Light energy
Excited state atom
Ground state atom (stable or
normal orbital coni!uration)
Excited
states
Groundstate
Spectral resonance line
(The strongest line
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Atomic Spectroscopy!ractically, the ratio of the excited to ground state atoms is extremely small.
Therefore, The a"sorption spectrum is usually only associated #ith transitions
from the ground state to higher energy states
E n e r g y
~100% population
Emission Absorption
~0% population
Ground state atoms
Excited state atoms
$olt%mann equation explain the relatioship "et#een the ground and excited state atoms
&'&) * (g'g)e+E-T
&' &o. of excited atoms &) &o. of ground state atoms E excitation energy
- $olt%mann constant T Temperature in /elvin
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Atomic Spectroscopy
The process of excitation and decay to groundstate is involved in the two techniques of atomic
spectroscopy.
We measure the energy absorbed or emitted anduse it for quantification process
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Atomic Emission Spectroscopy (AES)
(Flame Photometry)
!rinciple 0lame photometry is "ased upon those particlesthat are electronically excited in the medium.
0lame is the source of excitation energy. (lo# energy source.
1ses0lame photometry is used mainly for the determination of al/ali
metals and easily excited elements (&a, -, Li, 2a, etc. particularly
in "iological fluids and tissues
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0lame !hotometry
Ground state atoms
&a)
Solution of metal
salt (&a2l
Solvent evaporation
Solid aerosol of
metal salt (&a2l
3olatili%ation or decomposition
Gaseous metal
salt (&a2l
4tomi%ation 0ree atoms
&a)
Excitation
Excited atoms
&a5
Emission and
return to G)
Events occur in 0ES
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Flame Photometry
Inter%onal region
0uel+ oxidant mixture
!rimary
com"ustion %one
Secondary
com"ustion %one
Flame Structure
0lame 6etector
7onochromator
"nstrument
components
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Functions o Flame
'. To convert the constituents of liquid sample into the vapor state.
8. To decompose the constituents into atoms or simple molecules
79 9 e+ (from flame 7 9 hν
:. To electronically excite a fraction of the resulting atomic or
molecular species
7 75
Flame Photometry
;xidant + 0uel 7ax. temp. (o2
Air- propane 1!"
Air- acetylene !#$$%xygen- acetylene 31$$
&itrous oxide-acetylene 3$$$
Air-hydrogen !$$$
%xygen-hydrogen !$$
Air ' argon -hydrogen 1"
The flame is composed of
a fuel gas and oxidant gas
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Flame Photometry0actors affecting intensity of flame emission
'+ The concentration of the analyte in solution
8+ The rate at #hich excited atoms are formed in the flame.:+ The rate at #hich the sample is introduced into the flame.
<+ Temperature of the flame.
=+ 2omposition of the flame.
>+ The ratio of fuel to oxidant in the flame.?+ Solvent used to dissolve the sample.
The flame temperature is the most important factor. Increase in
flame temperature causes an increase in emission intensity. This is
controlled "y composition of the flame.
@igh temperature flames should not "e used for elements that
ioni%ed easily e.g. &a, -, Li or 2e. @o#ever, high temperature
flames are generally favored for transition elements and al/aline
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Effect of the solvent used to dissolve the sampleA if the solvent is
#ater the process is slo# and if it is organic solvent the processis fast and emission intensity is increased.
It is therefore very important that cali"ration curves "e
prepared using the same solvent.
The stochiometric ratio of fuel to oxidant in the flame must "e
used, in #hich "oth fuel to oxidant are totally consumed.
Flame Photometry
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Flame Photometry
#he nebuli$er%burner system
&e"uli%er produce an aerosol of the test solution
$urner in #hich the mixing "et#een fuel and oxidant
To convert the test sample into gaseous atoms
#ypes o burner system
1. Pre%mix or laminar lo& burner
4dvantages
6isadvantages
'. @omogenous flame
8. Suita"le for 44S and 4ES as
the path#ay could "e increased
(uel in
%xidant in
)urner
(lame
Aspiratorair
*ixing baffles
+rain
,ample
Suffers from explosion ha%ards
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Flame Photometry2. #otal consumption burner
0uel
; x
i d a n t
S a m p l e
;xidant
0uel
: concentric tu"es, the sample, fuel and
oxidant only mix at the tip of "urner
1sed mainly for 0ES (short "ath
4dvantages'. Simple to manufacture
8. 4llo#s a total representative sample
to reach the flame
:. 0ree from explosion ha%ards
6isadvantages
'. 4spiration rate varies #ith different solvents
8. Suita"le only for 4ES
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Flame Photometry
'on Flame Atomi$ers0or example @eated Gravite 0urnace
Sample evaporationB time and temp. controlled drying and ashing
4dvantages'. small samples are analysed
8. 'CCC+fold more sensitive than flame
:. ;ven is adapta"le to determination of solid samples
6isadvantages
'. Lo# accuracy 8. Lo# precision
8. 7ore ionic interferences due to very high temp.
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Flame Photometry
Monochromators
etectors
4s in 13
0ilms or photomultipliers
Analytical techniue
'. 2hoice of the #avelength of max. sensitivity and min. spectral interferences8. Sample preparation
a. t is very important to obtain the sample in a form of solution where the spectral
and chemical interferences are absent
b. +eminerali/ed dist. Water and very pure reagents are to be used because of thehigh sensitivity of the technique
c. )ecause of the instability of the very dil. ,olution it is advisable to dilute the
soln 0ust before use.
d. ,everal elements can be determined in blood urine cerebrospinal fluid and other
biological fluids by direct aspiration of the sample after dilution with water.
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Flame Photometry
2hemical interferences can often "e overcome "y simple
dilution #ith a suita"le reagent solution e.g. serum is diluted "yE6T4 solution for the determination of calcium in order to
prevent interference from phosphate.
:. Standard curves
A b s o r b
a n c e ,
A
Concentration, c
" n t e n
s i t y
6eviations from
linearity may occur
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Flame Photometry
:. Dualitative analysis
(lame photometry are useful mostly for the detection of elements in
group I and II of the periodic ta"le. The presence of certain
elements can be detected by the use of a filter or monochromator.
4dvantages and disadvantages
The method is not as relia"le as other atomic emission spectroscopic
methods but it is fast and simple.
<. Duantitative analysis
To perform quantitative analysis the sample is introduced into theflame and the intensity of radiation is measured. The concentration
of the emitting substance is then calculated from a calibration curve
or using standard addition method.
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Flame Photometry4pplication of flame photometry in pharmaceutical analysis
'. 7etals are maor constituents of several pharmaceuticals such as dialysissolutions, lithium car"onate ta"lets, antacids and multivitamin + mineral
ta"lets.
8. The elements &a, -, Li, 7g, 2a, 4l and Fn are among the most common
elements su"ected to pharmaceutical analysis using flame emission
technique.
:. Sodium and potassium levels in "iological fluids are difficult to analy%e "y
titrimetric or colorimetric techniques. Their analysis is very important for
control of infusion and dialysis solutions #hich must "e carefully monitored
to maintain proper electrolyte "alance.
4dvantages and disadvantages
'. 0lame emission is the simplest and least expensive technique.
8. The analysis may "e carried out #ithout prior separation as othercomponents such as dextrose, do not interfere.
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Atomic Absorption Spectroscopy
6etector
Monochromator
"nstrument components
Source *ampslow-pressure inert gas
nert carrier gas
&e or Ar @ollo# 2athod
lamp
4tomic 4"sorption spectroscopy involves the study of the a"sorption
of radiant energy "y neutral (ground state atoms in the gaseous state.
P P 0
Sample
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Atomic Absorption Spectroscopy
Electrodless 6ischarge Lamps, E6L
0or easily evapori%ed elements as @g or 4s
1sed for 44S and 4ES
Give much greater radiation intensities than hollo# cathod
There is no electrode, "ut instead , the inert carrier gas is
energi%ed "y an intense field of radiofrequency or micro#ave
radiation B plasma formation #hich cause excitation of the
metal inside
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Atomic Absorption Spectroscopy
6egree of a"sorption
Total amount of light a"sor"ed * (e8mc8&f Hhere
e * electronic charge, m * mass of electron
c * speed of light, & * total &o. of atoms that can a"sor" light
f * 4"ility of each atom to a"sor" light
, e, m, and c are constants, therefore
Total amount of light a"sor"ed * constant x &f
Since f is also constant for the same su"stance
4 2
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4tomic 4"sorption Spectroscopy
At i Ab ti S t
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Atomic Absorption Spectroscopy
Spectral Interferences'. They arise #hen the a"sorption line of an interfering species
either overlaps or lies so close to the analyte a"sorption line that
resolution "y the monochromator "ecomes impossi"le. Ex. 7g in
presence of 2a.8. They occur from "and or continuous spectra #hich are due to
a"sorption of molecules or complex ions remaining in the flame
:. They arise from flame "ac/ground spectrum.
2orrection'. It may "e useful to shift to another spectral line
8. T#o line correction method (Instrumental correction
It employs a line from the source as a reference. The line should lie as close as
possi"le to the analyte line "ut must not "e a"sor"ed "y the analyte. If the
conditions are met, any decrease in the reference line from that o"serveddurin cali"ration arises from a"sor tion " the matrix of the sam le.
Interferences
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Atomic Absorption Spectroscopy
2hemical Interferences
occurrs during atomi%ation that prevent the gaseous atomsproduction of the analyte. They are more common than spectral
ones.
Types of chemical interferences
'. 0ormation of sta"le compounds B incomplete dissociation of the sample in flame
8. 0ormation of refractory oxides B #hich fail to dissociate into the constituent atoms
Examples '. 6etn. of 2a in presence of sulphate or phosphate
8. 0ormation of sta"le refractory oxides of Ti;8, 38;= or 4l8;:
reaction #ith ;8 and ;@ species in the flame
;vercome'. Increase in the flame temp. B 0ormation of free gaseous atoms
e.g. 4l8;: is readily dissociated in acetylene+nitrous oxide flame
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Atomic Absorption Spectroscopy
8. 1se of releasing agents 7+J 9 K B KJ 9 7 ex. 6etn of 2a
in presence of phosphate(2a + phosphate 9 Sr2l8 B Sr+phosphate 9 2a atoms or
(2a phosphate 9 E6T4 B 2a+E6T4 easily dissociated complex .
:. Solvent extraction of the sample or of the interferring elementsIoni%ation Interferences
Ioni%ation of atoms in the flame B decrease the a"sorption or emission
;vercome '. 1se of lo#est possi"le temp #hich is satisfactory forthe sample ex. 4cetylene air must not "e used for easily ionised
elements as &a, -, 2a, $a
8. 4ddition of an ionisation supressant ( soln of cation has a lo#er
ionisation potential than that of the sample, e.g. addition of -+solnto 2a or $a soln. 2a B 2a89 9 8e - B - 9 9 e
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Atomic Absorption Spectroscopy
!hysical Interferences
'. 3ariation in gas flo# rate
8. 3ariation in sample viscosity
:. 2hange in flame temp.
;vercome '. "y continuous cali"ration
8. 1se of internal standard
4dvantages of 44S 3ery sensitive. 0ast.
6isadvantages of 44S @ollo# cathode lamp for each element.
Expensive element.
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elationship )etween Atomic Absorption and (lame
2mission ,pectroscopy
4tomic 4"sorption 0lame Emission
'. 7easures the radiationa"sor"ed "y the unexcited
atoms
'. 7easures the radiationemitted "y the excited atoms
8. 6epends only on thenum"er of unexcited atoms
8. 6epends only on thenum"er of excited atoms
:. 4"sorption intensity is&;T affected "y thetemperature of the flame
:. Emission intensity is greatlyaffected "y the temperaturevariation of the flame
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Atomic Emission Spectroscopy
+sin! 'on%Flame excitation sources'. There is no single excitation source can excite all
elements
8. The emitted radiation usually consists of sharp #ell
defined lines, #hich fall in 13 or visi"le region
:. Identification of the λ of these lines permits qualitative
analysis of these elements, #hereas measurements of
their intensities permits quantitative analysis
4dvantages
'. Excellent method for trace element analysis at ppm level
8. 1sed nearly for all elements in periodic ta"le
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Atomic Emission Spectroscopy
@igh energy excitation sources
!lasma excitation sources
Laser
4rc and spar/ emission spectrometry (Spectrography
7icro#ave and x+ray
:. 1sed for very small samples, even less than ' mg
<. There is no need for prior separation=. Kelatively rapid technique
6isadvantages '. Expensive
8. Lo# precision and accuracy
:. 6estroying the sample
<. 1sed mainly for metals
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'. 4 plasma is a cloud of highly ioni%ed gas containing significant num"ers of
positive and negative ions, free electrons and neutral particles.
8. !lasma sources operate at high temperatures "et#een ?CCC and '=CCC -.
Thus, it produces a greater num"er of excited emitted atoms, especially in
the 13 region, than that produced "y flame.
:. 1sing this technique, excitation operates through a plasma produced
electrically in a carrier gas such as nitrogen or argon.
Atomic Emission Spectroscopy
!lasma excitation sources
:. The main types of argon plasma sources
a. Inductively coupled plasmaA I2!
". 6irect current plasmaA 62!
c. 4 micro#ave+induced plasmas is recently introduced to spectro+chemical
analysis methods.
At i E i i S t
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Induction coils
Sample flo#
Duart% tu"es
7agnetic field
!lasma
4rgon
tangential flo#
Atomic Emission Spectroscopy
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A i E i i S
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It consists of a high+voltage discharge "et#een t#o graphite
electrodes. The recent design employs a third electrode arranged
in an inverted M+shaped #hich improves the sta"ility of discharge.
The sample is ne"ulised at a flo# rate of ' mlmin. 4rgon is used
as carrier gas. The argon ioni%ed "y the high+voltage is a"le to
sustain a current.
62! generally has lo#er detection limits than I2!. @o#ever, 62!is less expensive than I2!.
6irect current, 62!
Atomic Emission Spectroscopy
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'+ The sample could "e introduced in solution form through a
ne"uli%er (easy for quantitative analysis.
8+ It is suita"le for quantitative multielement determinations
:+ The high temperature of plasma eleminates many chemical
interferences present in a flame
<+ It is #ell suited for refractory (oxide forming elements e.g.!, 1r and tungeston and for difficult+to+excite elements
such as Fn and 2d.
=+ The emission intensity+versus+cencentration range is linear
over a very #ide dynamic ranges of analytes.
4dvantages of plasma excitation source
Atomic Emission Spectroscopy
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Laser "eam is used to vapori%e the sample, #hich is then excited
electrically.
The sample is loaded ust "eneath the t#o electrodes that #ill "eused to generate the electrical discharge.
4 ru"y laser is then focused through a microscope onto the
surface. The energy from the laser causes an intense local hot spot #hich vapori%es a small quantity of sample.
The vapor circuits the electrodes and electrical discharge occurs
#hich excites the metals in vapor. The excited metals emit typical
emission spectra #hich are collected and measured as usual.
Laser excitation source
Atomic Emission Spectroscopy
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'. Laser excitation produces a high density plasma and is used
for the spectrochemical analysis of solid materials.
8. The locali%ation effect permits examination of areas as smallas =C Nm in diameter, providing the "iological researcher #ith
a tool capa"le of examining the insides of individual cells
#ithout destruction of organic materials.
:. In laser excitation, the sample needs not to "e electrically
conducting.
4dvantages of laser excitation source
Atomic Emission Spectroscopy
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If the composition of sample and matrix is un/no#n. The internal
standard is added to "oth un/no#n and cali"ration standards.
The internal standard should
'. resem"le the element to "e determined in rate of volatili%ationand chemical reactivity.
8. have a measura"le emission line in the same spectral vicinity as
the sample emission line.
:. It must not also present in the original sample.
1se of an inernal standard
Duantitative analysis
Then, "y plotting the ratio of intensities of the element to the
internal+standard element vs. concentration of the element, any
fluctuations should "e compensated for.
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Standard 4ddition 7ethod
in order to partially or #holly counteract the chemical and
spectral interferences introduced "y the sample matrix.
4 li ti f 4ES ( i fl it ti
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4ES is rapid method for qualitative and quantitative
determination of most metals.
It is superior than flame and atomic a"sorption methods. 0lameemission spectroscopy has the limitations of "eing only good for
fe# elements #hile atomic a"sorption techniques need a separate
source lamp for each element. 4ES methodsA "eing very sensitive,
have numerious applications in analysis of "iological samples.0or examples
'. evaluation of platinum in "ody fluids and tissues after
administration of platinum containing anticancer drugs
8. determination of organic and inorganic Se compounds in"iological fluids and environmental samples
:. determination of trace elements such as 2d, 2o, 2r, 2u, 0e,
@g, 7n, &i and !"
<. Silicon is recogoni%ed as an essential trace element
ti i ti i l " d t " li
4pplications of 4ES (using non+flame excitation sources