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MASS,IR,NMR,UV-VISIBLE
SPECTROSCOPY
Presented by
Dr. A. Suneetha
Dept. of Pharm. Analysis
Hindu College of Pharmacy
APPLICATIONS OF MASS
SPECTROSCOPY
• Molecular mass determination :
-mass spectroscopy is one of the best
method to determine the molecular mass
accurately
-when a substance bombarded with
moving electrons and the mass spectrum
is recorded, the mass of the peak at
highest m/e is the molecular mass
accurately
• Characterization of polymers :
- initially the polymer is pyrolised (decomposed by
heating) and then the pyrolised products are fed in to the
inlet of mass spectrometer and identified
• Impurity detection :
-mass spectroscopy is one of the best method to detect
the impurities,
-if the molecular weight of the impurities are much larger
than major components their detection is more easy
because their masses peaks are free from contribution
by those of the major components.
on the other hand if the molecular weight of
impurities are much lower then the major components ,
their detection is not easy job because of the formation
of common fragment ion
Distinction between cis and trans isomers :
-mass spectroscopy is successful in making distinction between cis
and trans isomers
-both cis – trans isomers yield similar mass spectra but the
molecular ion peak for the trans isomer is more intense than cis
isomer
Latent heat of vaporization of liquids :
- clausius-clapeyron eqution useful for measure the latent heat of
liquid
Toxological :
Use ful for identification of toxic compounds like
organo phosphorus compounds
Also useful for estimation of narcotic substance
• It is useful for the study the environmental
gases present at planets (it is coupled with
satellites)
• Natural products :
It is useful to identify the compound
mass which is present in herbal extract
• Chemical criminology:
It is useful for identify the mass of at a
time 25 different ball pens
• Isotopic abandance
The isotopic abandace of easily
vapourisable elements can be determined
by using mass spectrometer when this
information coupled with precise isotopic
mass determination , values of atomic
weight of elements may be obtained
Eg: cl35 ,cl37 these two isotops
can add to the sample cl35 gives more
intense peak than cl37. it can give peaks in
1:3 ratio, based up on peak we can
identify the particular compound
APPLICATIONS OF NMR
• Structural elucidation of organic compounds
Organic compounds invariably have
hydrogen atoms in their structure and the
environment of each proton is not same
CH3CH2CH2OH CH3CH(OH)CH3
(propanol-1) (propanol-2)
4 signals 3 signals
• Based upon the δ values we can elucidate
the structure of compound
• H1 –NMR is useful for identification of
nature of the carbon
• C13NMR is useful for identification of
nature of carbon
• 2D NMR is useful for identification of exact
position of carbon and hydrogen
• DEPT it is useful for identification of no. of
CH3 and CH2
• Structure determination of polyethylene
-It shows two types of lines one of
these is narrow while the other is broad,
narrow component is denote the
amorphous phase where as broad
component to the crystalline phase
• Determination of optical purity
• Study of molecular interactions like micelle
formation and drug macromolecule or drug
receptor interactions
• Detection of electro negative atom or group
It is known that the presence of an
electronegative atom or group in the
neighbourhood of the proton cause
deshielding and signal is shifted to down
field
Fluorine cause more downward shift
as compared to oxygen
Oxygen cause more downward shift
compared to nitrogen
• Distinction between cis-trans isomers
-The cis and trans isomers of compound can be easily
distinguished as the concerned proton have different
values of chemical shifts as well as coupling constants
• Elemental analysis
-NMR spectroscopy can be used for
determination of total concentration of given kind
of magnetic nucleus in a sample
• Rates of reactions
-An interesting special use of PMR spectroscopy is study of certain
reaction that are too fast for measurement by ordinary techniques
• Detection of hydrogen bonding
-By NMR we can differentiate whether the compound having
intermolecular and intramolecular hydrogen bonding
• Anti-gauche confirmation of a compound
• Quantitative analysis
Assay of components:
Single or multi component with out separation of
components, can be quantitatively estimated
Specific peak for each component is identified and
peak area /height ratio given by integral value is found
using standard and sample and the quantity can be
estimated
Iodine value :
which is measure of double or triple bond can be
known form the proportion of olefinic protons
Moisture analysis :
-since water can give characteristic peak, the % can
be known from the peak ratio of water peak and
component peak
APPLICATION OF INFRA-RED
SPECTROSCOPY
• Identification of drug substance
IR spectrum of sample and standard can be compared to identify
a substance, if the spectra same then the identify of the sample can
be confirmed
• Structure determination
This technique helps to establish the structure of a unknown
compound. all major functional groups absorb at their characteristic
wave number
• Identification of functional groups
The presence or absence of absorption bands help in predicting
the presence of certain functional groups in the compounds.
Benzene 1 261nm
Napthalene 2 312nm
Anthracene 3 375nm
Napthacene 4 480nm
Pentacene 5 580nm
• Quantitative analysis
To determine the concentration and
amount of drug in sample solution and thus
%purity can be determine
Several quantitative methods are
A) using E1%1cm values
%purity = observed absorbance / E × 100/CONC
B) reference standard method
1)single standard or direct
comparision method
C2=C1 × A2/A1
2) multiple standard method or
caliberation curve
• Determination of molecular weight
• Chemical kinetic
kinetic of a reaction can also be
studied using UV spectroscopy. The UV
radiation is passed through reaction cell
And absorbance changes can be followed
• Keto-enol tautomerism
Keto-enol form of a substance have
different UV absorption pattern using this
principle the% of keto and enol form in
mixture can be calculated
• Examination of poly nuclear hydrocarbons
• Elucidation of the structure of vitamin A and
vitamin K
• Assay of medicinal substance
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