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SMT BNB SWAMINARYAN PHARMACY COLLEGE ,SALVAV
NMR
SPECTROSCOPY
PRESENTED BY :- OZA VRUSHNAT PRANAY
CLASS :- M.PHARM (PHARMACEUTICS) SEM 1
05-01-2023 smtbnbspc/vrushantoza/ 2
CONTENT
CONTENT
RELAXATION PROCESS AND
CHEMICAL SHIFT
SOLVENT REQUERED
INSTRUMENTATION
INTODUCTION
QUANTUM NUMBER
AND THEIR ROLE
THEORY & PRINCIPLE
INTRODUCTION
N
M
R
MEGNETIC
NUCLEAR RESONANCE
• Proton in nucleus shows spin movement because of that proton acts as small magnet
• Due to this the resonance in this small magnet takes place and processes NMR
• Range : 4-600 MHz
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QUANTUM NUMBER
AND THEIR ROLE
• Describe shape of
orbit .
• Value of I depends
on N.
• Have + or – value .
• Specify the orientation
• This number divides
the subshell into
individual orbital
which hold the
electron.
• Describes angular
momentum of
electron.
• Because angular
momentum is
vector spin
quantum number
has both
magnitude and
direction .
 Definition:- occurs in the theoretical expression for the value of some quantized property of a subatomic
particle , atom or molecules and can only have certain integer or half integer value.
 In simple term :- Quantum number is set of number use to describe position and energy of electron in atom.
 It has 4 types
1. Principal(N) 2.Angular
momentum(I)
3.Magnetic(M) 4. Spin (S)
• The main energy
level occupied by
the electrons
• Energy level are
fixed distance from
nucleus of given
atom
• Described in whole
number
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QUANTUM NUMBER
AND THEIR ROLE
05-01-2023 smtbnbspc/vrushantoza/ 5
• The theory behind NMR comes from the spin of a nucleus and it generates magnetic field.
• Without external applied magnetic field the nuclear spin are random in direction.
• When external magnetic field (B0) is present the nuclei aligned themselves either with or against the field of
external magnet.
Theory & Principle
 THEORY
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Theory & Principle
05-01-2023 smtbnbspc/vrushantoza/ 7
The spinning nucleus
The effect of external magnetic field
Precessional motion
Precessional frequency
Energy transition
Theory & Principle
 PRINCIPLE
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1) THE SPINNING NUCLEUS:-
 The nucleus of the hydrogen (proton)
behaves as a tiny spinning bar
magnet,
 and it does so because it possesses
both electric charge and mechanical
spin
 any spinning charged body will
generate a magnetic field, and the
nucleus of hydrogen is no exception
Theory & Principle
 PRINCIPLE
05-01-2023 smtbnbspc/vrushantoza/ 9
2) The effect of external magnetic field
 The proton can only adopt two orientations
with respect to an external magnetic
 field-either aligned with the field (the
lower energy state)
Or
 opposed to the field (the higher energy
state).
Theory & Principle
 PRINCIPLE
05-01-2023 smtbnbspc/vrushantoza/ 10
3) Precessional motion
 Proton will be showing precessional motion
due to interaction of spin & gravitational
force of earth [gyroscopic motion ]
 Energy of reorientation of magnetic dipole
∆E=hv
Where ,
H= plank’s constant
V= frequency of radiation
Theory & Principle
 PRINCIPLE
05-01-2023 smtbnbspc/vrushantoza/ 11
4) Precessional frequency
 Spinning frequency of proton will be same
 Precessional frequency ∝ external magnetic
force
v ∝ Bo
Theory & Principle
 PRINCIPLE
05-01-2023 smtbnbspc/vrushantoza/ 12
5) Energy transition
 If proton’s precessional frequency will be exactly same then only it will absorb the radiation and
resonance takes place which is know as NMR
 Proton goes to low energy level to high energy level.
 The emitted radiofrequency signal gives the NMR spectrum of the concerned nucleus.
 The emitted radiofrequency is directly proportional to the strength of the applied magnetic field
Theory & Principle
 PRINCIPLE
05-01-2023 smtbnbspc/vrushantoza/ 13
SAMPLE TUBE / HOLDER
MAGNET
SWEEP GENERATOR
RADION FREQUANCY
GENRATOR
RF RECEIVER
READ OUT DEVICE /
DETECTORE
INSTRUMENTATION
 INSTRUMENTATION
05-01-2023 smtbnbspc/vrushantoza/ 14
INSTRUMENTATION
 INSTRUMENTATION
05-01-2023 smtbnbspc/vrushantoza/ 15
INSTRUMENTATION
 INSTRUMENTATION
1.SAMPLE HOLDER:
5mm GLASS TUBE IS USED,
WHICH CAN HOLD 0.4ml
LIQUID SAMPLE.
MICROTUBES ARE USED FOR
LOW VOLUMES.
2.MAGNET:
• ACCURACY & QUALITY OF THE INSTRUMENT IS DEPENDENT ON
ITS STRENGTH.
• RESOLUTION INCREASES WITH INCREASE IN THE FIELD
STRENGTH.
• THREE TYPES OF MAGNETS CAN BE USED
• CONVENTIONAL MAGNET (30 - 60MHz)
• PERMANENT MAGNET (60,90, 100MHz)
• SUPER CONDUCTING MAGNET (470MHz)
3.SWEEP GENERATOR:
A SET OF SWEEP COIL IS LOCATED PARALLEL TO THE
MAGNET, WHICH ALLOWS THE MAGNETIC FIELD TO SWEEP
05-01-2023 smtbnbspc/vrushantoza/ 16
INSTRUMENTATION
 INSTRUMENTATION
4. RF TRANSMITTER / GENERATOR :
• IT IS A PAIR OF COILS MOUNTED PERPENDICULAR
TO THE PATH OF FIELD & RECIEVER COIL.
5. RECIEVER COIL & AMPLIFIER:
• AMPLIFIES THE RECEIVED EMR BY 10 5
TIMES.
6. DETECTOR:
• DETECTS THE SIGNAL PRODUCED
BY RESONATING NUCLEI.
05-01-2023 smtbnbspc/vrushantoza/ 17
SOLVENT USED
IN NMR
 CRITERIAS
CHEMICALLY INERT
SOLVENTS SHOULD
BE MAGNETICALLY
ISOTROPIC IN
NATURE
FREE FROM ANY
HYDROGEN ATOM
SOLVENT SHOULD
BE ABLE TO
DISSOLVE THE
MOLECULARAMPLE
IN A RESONABLE
QUANTITY.
COMMONLY USED SOLVENTS:
CARBON TETRACHOLRIDE(CCL4)
CARBON DISULPHIDE(CS2)
DEUTEROCHLOROFORM(CDCI3)
HEXACHLOROACETONE((CDCI,),CO),
DEUTEROBENZENE(C;D.).
DEUTERODIMETHYLSULFOXIDE((CH;)250)
05-01-2023 smtbnbspc/vrushantoza/ 18
RELEXATION
PROCESS
 RELEXARION
PROCESS
 RELAXATION IS PROCESS BY WHICH THE
SPINS IN THE SAMPLE COME TO
EQUILLIBRIUM WITH THE SURROUNDINGS.
 RATE OF RELAXATION:
 DETERMINES HOW FAST AN EXPERIMENT
CAN BE REPEATED
 INFLUENCED BY THE PHYSICAL
PROPERTIES OF MOLECULE & THE SAMPLE
 AN UNDERSTANDING OF RELAXATION
PROCESSES IS IMPORTANT FOR THE PROPER
MEASUREMENT & INTERPRETATION OF NMR
SPECTRA.
1. SPIN LETICE /LONGITUDINAL RELAXATION :
 CHARACTERISED BY T1 NUCLEI IN UPPER
STATE STARTS TO LOSE ENERGY TO THE
SURROUNDING .
2.SPIN-SPIN/ TRANSVERSE RELAXATION:
 CHARACTERISED BY T2 DOESN’T LEAD TO A
CHANGE IN UPPER & LOWER ENERGY LEVEL
 NUCLEI IN THE UPPER STATE STARTS TO
TRANSFER ITS ENERGY TO A NUCLEI IN
LOWER ENERGY LEVEL.
05-01-2023 smtbnbspc/vrushantoza/ 19
CHEMICAL SHIFT
 CHEMICAL SHIFT
the chemical shift is the resonant frequency of an
atomic nucleus relative to a standard in a magnetic
field.
 FACTORS INFLUENCING CHEMICAL
SHIFT
1. ELECTRONEGATIVITY -SHIELDlNG AND
DESHIELDING
2. VAN DER WAALS DESHIELDING
3. ANISOTROPIC EFFECTS
05-01-2023 smtbnbspc/vrushantoza/ 20
Thank You

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NMR SPECTROSCOPY.pptx

  • 1. SMT BNB SWAMINARYAN PHARMACY COLLEGE ,SALVAV NMR SPECTROSCOPY PRESENTED BY :- OZA VRUSHNAT PRANAY CLASS :- M.PHARM (PHARMACEUTICS) SEM 1
  • 2. 05-01-2023 smtbnbspc/vrushantoza/ 2 CONTENT CONTENT RELAXATION PROCESS AND CHEMICAL SHIFT SOLVENT REQUERED INSTRUMENTATION INTODUCTION QUANTUM NUMBER AND THEIR ROLE THEORY & PRINCIPLE
  • 3. INTRODUCTION N M R MEGNETIC NUCLEAR RESONANCE • Proton in nucleus shows spin movement because of that proton acts as small magnet • Due to this the resonance in this small magnet takes place and processes NMR • Range : 4-600 MHz 05-01-2023 smtbnbspc/vrushantoza/ 3
  • 4. QUANTUM NUMBER AND THEIR ROLE • Describe shape of orbit . • Value of I depends on N. • Have + or – value . • Specify the orientation • This number divides the subshell into individual orbital which hold the electron. • Describes angular momentum of electron. • Because angular momentum is vector spin quantum number has both magnitude and direction .  Definition:- occurs in the theoretical expression for the value of some quantized property of a subatomic particle , atom or molecules and can only have certain integer or half integer value.  In simple term :- Quantum number is set of number use to describe position and energy of electron in atom.  It has 4 types 1. Principal(N) 2.Angular momentum(I) 3.Magnetic(M) 4. Spin (S) • The main energy level occupied by the electrons • Energy level are fixed distance from nucleus of given atom • Described in whole number 05-01-2023 smtbnbspc/vrushantoza/ 4
  • 5. QUANTUM NUMBER AND THEIR ROLE 05-01-2023 smtbnbspc/vrushantoza/ 5
  • 6. • The theory behind NMR comes from the spin of a nucleus and it generates magnetic field. • Without external applied magnetic field the nuclear spin are random in direction. • When external magnetic field (B0) is present the nuclei aligned themselves either with or against the field of external magnet. Theory & Principle  THEORY 05-01-2023 smtbnbspc/vrushantoza/ 6
  • 7. Theory & Principle 05-01-2023 smtbnbspc/vrushantoza/ 7
  • 8. The spinning nucleus The effect of external magnetic field Precessional motion Precessional frequency Energy transition Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 8
  • 9. 1) THE SPINNING NUCLEUS:-  The nucleus of the hydrogen (proton) behaves as a tiny spinning bar magnet,  and it does so because it possesses both electric charge and mechanical spin  any spinning charged body will generate a magnetic field, and the nucleus of hydrogen is no exception Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 9
  • 10. 2) The effect of external magnetic field  The proton can only adopt two orientations with respect to an external magnetic  field-either aligned with the field (the lower energy state) Or  opposed to the field (the higher energy state). Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 10
  • 11. 3) Precessional motion  Proton will be showing precessional motion due to interaction of spin & gravitational force of earth [gyroscopic motion ]  Energy of reorientation of magnetic dipole ∆E=hv Where , H= plank’s constant V= frequency of radiation Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 11
  • 12. 4) Precessional frequency  Spinning frequency of proton will be same  Precessional frequency ∝ external magnetic force v ∝ Bo Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 12
  • 13. 5) Energy transition  If proton’s precessional frequency will be exactly same then only it will absorb the radiation and resonance takes place which is know as NMR  Proton goes to low energy level to high energy level.  The emitted radiofrequency signal gives the NMR spectrum of the concerned nucleus.  The emitted radiofrequency is directly proportional to the strength of the applied magnetic field Theory & Principle  PRINCIPLE 05-01-2023 smtbnbspc/vrushantoza/ 13
  • 14. SAMPLE TUBE / HOLDER MAGNET SWEEP GENERATOR RADION FREQUANCY GENRATOR RF RECEIVER READ OUT DEVICE / DETECTORE INSTRUMENTATION  INSTRUMENTATION 05-01-2023 smtbnbspc/vrushantoza/ 14
  • 16. INSTRUMENTATION  INSTRUMENTATION 1.SAMPLE HOLDER: 5mm GLASS TUBE IS USED, WHICH CAN HOLD 0.4ml LIQUID SAMPLE. MICROTUBES ARE USED FOR LOW VOLUMES. 2.MAGNET: • ACCURACY & QUALITY OF THE INSTRUMENT IS DEPENDENT ON ITS STRENGTH. • RESOLUTION INCREASES WITH INCREASE IN THE FIELD STRENGTH. • THREE TYPES OF MAGNETS CAN BE USED • CONVENTIONAL MAGNET (30 - 60MHz) • PERMANENT MAGNET (60,90, 100MHz) • SUPER CONDUCTING MAGNET (470MHz) 3.SWEEP GENERATOR: A SET OF SWEEP COIL IS LOCATED PARALLEL TO THE MAGNET, WHICH ALLOWS THE MAGNETIC FIELD TO SWEEP 05-01-2023 smtbnbspc/vrushantoza/ 16
  • 17. INSTRUMENTATION  INSTRUMENTATION 4. RF TRANSMITTER / GENERATOR : • IT IS A PAIR OF COILS MOUNTED PERPENDICULAR TO THE PATH OF FIELD & RECIEVER COIL. 5. RECIEVER COIL & AMPLIFIER: • AMPLIFIES THE RECEIVED EMR BY 10 5 TIMES. 6. DETECTOR: • DETECTS THE SIGNAL PRODUCED BY RESONATING NUCLEI. 05-01-2023 smtbnbspc/vrushantoza/ 17
  • 18. SOLVENT USED IN NMR  CRITERIAS CHEMICALLY INERT SOLVENTS SHOULD BE MAGNETICALLY ISOTROPIC IN NATURE FREE FROM ANY HYDROGEN ATOM SOLVENT SHOULD BE ABLE TO DISSOLVE THE MOLECULARAMPLE IN A RESONABLE QUANTITY. COMMONLY USED SOLVENTS: CARBON TETRACHOLRIDE(CCL4) CARBON DISULPHIDE(CS2) DEUTEROCHLOROFORM(CDCI3) HEXACHLOROACETONE((CDCI,),CO), DEUTEROBENZENE(C;D.). DEUTERODIMETHYLSULFOXIDE((CH;)250) 05-01-2023 smtbnbspc/vrushantoza/ 18
  • 19. RELEXATION PROCESS  RELEXARION PROCESS  RELAXATION IS PROCESS BY WHICH THE SPINS IN THE SAMPLE COME TO EQUILLIBRIUM WITH THE SURROUNDINGS.  RATE OF RELAXATION:  DETERMINES HOW FAST AN EXPERIMENT CAN BE REPEATED  INFLUENCED BY THE PHYSICAL PROPERTIES OF MOLECULE & THE SAMPLE  AN UNDERSTANDING OF RELAXATION PROCESSES IS IMPORTANT FOR THE PROPER MEASUREMENT & INTERPRETATION OF NMR SPECTRA. 1. SPIN LETICE /LONGITUDINAL RELAXATION :  CHARACTERISED BY T1 NUCLEI IN UPPER STATE STARTS TO LOSE ENERGY TO THE SURROUNDING . 2.SPIN-SPIN/ TRANSVERSE RELAXATION:  CHARACTERISED BY T2 DOESN’T LEAD TO A CHANGE IN UPPER & LOWER ENERGY LEVEL  NUCLEI IN THE UPPER STATE STARTS TO TRANSFER ITS ENERGY TO A NUCLEI IN LOWER ENERGY LEVEL. 05-01-2023 smtbnbspc/vrushantoza/ 19
  • 20. CHEMICAL SHIFT  CHEMICAL SHIFT the chemical shift is the resonant frequency of an atomic nucleus relative to a standard in a magnetic field.  FACTORS INFLUENCING CHEMICAL SHIFT 1. ELECTRONEGATIVITY -SHIELDlNG AND DESHIELDING 2. VAN DER WAALS DESHIELDING 3. ANISOTROPIC EFFECTS 05-01-2023 smtbnbspc/vrushantoza/ 20