1.IR Spectroscopy EDITED

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Introduction & Applications of

IR Spectroscopy

IR Spectroscopy : Principle, Instrumentation,


Application
Prof. Harminder Kaur
hkaur@pec.edu.in 9876062207

1
Electromagnetic radiation
The spectrum covers EMA wave energy having wavelengths from
thousands of meters down to fractions of the size of an atom.
Frequencies of 30 Hz and below can be produced by and are
important in the study of certain stellar nebulae and frequencies as
high as 2.9×1027 Hz have been detected from astrophysical sources.
Electromagnetic energy at a particular wavelength λ (in vacuum) has
an associated frequency (ʋ) and photon energy E. Thus, the
electromagnetic spectrum may be expressed equally well in terms of
any of these three quantities. They are related by the equations:
E= hʋ = hc/λ
Energy of electromagnetic waves
1
c   

c
E  h  h  hc

c
E  N A h  N A h  N A hc


 (nu-bar) represents wavenumber, the
number of wavelengths in 1 cm
Electromagnetic
Electromagnetic Spectrum
Spectrum

Atkins & de Paula 2002


Types of Spectroscopy
O Emission spectroscopy
O Absorption spectroscopy
Absorption Spectroscopy
O Absorption spectroscopy is a technique in which the power
of a beam of light measured before and after interaction
with a sample is compared.
O In absorption spectroscopy, the intensity of a beam of light
measured before and after interaction with a sample is
compared. When combined with the word spectroscopy, the
words transmission and remission refer to the direction of
travel of the beam measured after absorption to that before.
The descriptions of the experimental arrangement usually
assume that there is a unique direction of light incident
upon the sample, and that a plane perpendicular to this
direction passes through the sample
Types of Absorption Spectroscopy

1. Ultra violet spectroscopy


2. Infra red spectroscopy
3. Microwave spectroscopy
4. Nuclear magnetic resonance (NMR)
spectroscopy
5. Electro spin resonance (ESR) spectroscopy
INFRA-RED
SPECTROSCOP
Y
IR Spectroscopy
Electromagnetic radiation in the infrared (IR) region of the spectrum
has the correct energy to cause bonds in a molecule to stretch and
bend. Individual functional groups have a characteristic absorption
in the IR region. The absence of an absorption in the IR spectrum of
a compound can be important. For example, if an oxygen-containing
compound shows no absorption in the C=O region (1680-1750 cm-1)
or in the O-H region (2500 - 3650 cm-1) of the IR spectrum, the
compound is likely to be an ether.
λ = 2.5 to 17 μm
υ = 4000 to 600 cm-1
These frequencies match the frequencies of covalent bond
stretching and bending vibrations. Infrared spectroscopy can be
used to find out about covalent bonds in molecules.
1.The quantum mechanical energy levels observed in IR
spectroscopy are those of molecular vibration

2.We perceive this vibration as heat

3.When we say a covalent bond between two atoms is of a


certain length, we are citing an average because the bond
behaves as if it were a vibrating spring connecting the two
atoms

4.For a simple diatomic molecule, this model is easy to


visualize:
Difference from UV
•Study the nature of functional groups
•IR gives a large number of absorption bands compared to
relatively few peaks in UV
•Absorption of IR radiations expressed in wavelength or wave
number
•Wave number=1/wavelength
Principle of IR Spectroscopy
➢ Atoms constituting a covalent molecule are not stationary.
They continuously rotate and vibrate in number of ways
➢ The absorption of IR produces either
i. Bond change in bond distance between
stretching: bonds with no displacement from
inter-nuclear axes
ii. Bond angle vibration: atoms are displaced from inter-
nuclear axes
•More energy is required for stretching. Stretching absorption
appears at higher frequency than bending frequency
Instrumentation of Infrared (IR)
Spectroscopy
1.Radiation source
2.Sample cells and sampling of substances
3.Monochromators
4.Detectors
5.Recorder

13
IR radiation sources
1.Nernst glower
2.Incandescent lamp
3.Mercury arc
4.Tungsten lamp
5.Globar source
6.Nichrome wire

15
Sample cells and sampling of substances

 Solid – Various techniques are used for preparing


solid samples such as pressed pellet technique, solid
run in solution, solid films, mull technique etc.

 Liquid – Samples can be held using a liquid sample


cell made of alkali halides. Aqueous solvents cannot
be used as they will dissolve alkali halides. Only
organic solvents like chloroform can be used.

 Gas– Sampling of gas is similar to the sampling of


liquids.
16
Spectrum two spectrophotometer

17
Infrared Spectroscopy of
Organic Molecules
• IR region lower energy than visible light (below red –
produces heating as with a heat lamp)

• 2.5  106 m to 2.5  105 m region used by organic


chemists for structural analysis

• IR energy in a spectrum is usually measured as


wavenumber (cm-1), the inverse of wavelength and
proportional to frequency
IR Spectroscopy

Introduction
The IR Spectroscopic Process
There are two types of bond vibration:
• Stretch – Vibration or oscillation along the line of the bond

H H
C
C
H
H

symmetric asymmetric

• Bend – Vibration or oscillation not along the line of the bond


H H H
H
C C
C C
H H
H H
rock twist wag
scissor in plane
out of plane
• Bend – Vibration or oscillation not along
the line of the bond

H H
C H H
C
C C
H H
H H

scissor rock twist wag


Number of Fundamental Vibrations
Number of bands formed are less
than expected value. Why?
Some fundamental vibrations are:-

1.Weak: not possible to record


2.So close: They may overlap
3.Involve energy which may fall outside the IR range
(2.5µm to 15µm )
Selection Rules
The compound to be studied using IR spectroscopy must meet
following requirements:

➢Polar
➢No center of symmetry of vibration causing absorption
➢Change in dipole moment on undergoing vibration

•The vibrations lead to fluctuation of dipole moment.


•The interaction between infra red vibration and oscillating dipole
moment leads to absorption of energy.
•Thus, only those vibrations are effective in causing absorptions
which are not centro-symmetric.
Important points:
• An IR active band will be observed if a vibration results in a change of
the dipole moment.
• The number of molecular vibrational modes equals 3n-6 (3n-5 for linear
molecules), where n is the number of atoms.
• The symmetric stretch does not result in a change (of the initially zero
dipole moment), so it is IR-inactive.
• The asymmetric stretch does result in a change in dipole moment so it is
IR-active. The bend also results in a change in dipole moment so it too
is IR-active.
• The symmetric molecules, like N2 or O2, the only vibrational modes
that can exist are stretching of the only bond, which doesn't lead to a
dipole change. Thus, those species are not IR active.
Calculation of Vibrational Frequency
Position of Absorption Bands
 Linked with nature of bond and functional group. Thus a
particular group can be characterized from position of band
E.g. Absorption band at 3µm (3333 cm-1) indicates presence of
hydroxyl group.
 Absorption bands in the region of 2.5 to 8 µm are associated
with changes in vibrational states of different bonds. Thus this
regions is characteristic of types of bonds.
 Absorption bands in the region of 8 µm are associated with
complex vibrational and rotational energy changes. This is
known as finger print region. No two molecules, however
closely related, can never have identical IR spectra.
Intensity of Absorption Bands

• Linked to magnitude of dipole moment (Polarity)


• Greater the polarity, more is the intensity of
absorption spectrum.
• E.g. bond between carbon and oxygen in carbonyl is
highly polar thus gives high intensity
Factors influencing Fundamental
Frequency

H H3C H3C
H3C ClH2C ClH2C

C O C O C O C O C O C O

H H H3C H3C H3C ClH2C

1715cm-1 1725cm-1 1740cm-1


1750cm-1 1740cm-1 1715cm-1
Resonance Effect:
Conjugation tends to decrease the force constant. Their
absorption always shifts to lower wave number.
O

H3C C C CH2 Shif t: 1715cm-1 to 1690 cm-1


H

O C H

Shif t: 1715 cm-1 to 1700cm-1

Hydrogen Bonding:
In organic compounds like phenols, acids or amines which show hydrogen
bonding, the value of force constant generally decreases because of attraction
and this shifts absorption towards lower wave number.
•Intermolecular H-bonding gives broader bands while intramolecular H-
bonding gives sharp and well defined bands.
•The absorption bands in intermolecular H-bonding are concentration
dependent but not in case of intramolecular H-bonding. Why?
The IR Spectroscopic Process
As a covalent bond oscillates – due to the oscillation of the dipole of
the molecule – a varying electromagnetic field is produced

The greater the dipole moment change through the vibration, the
more intense the EM field that is generated
The IR Spectroscopic Process
When a wave of infrared light encounters this oscillating EM field generated
by the oscillating dipole of the same frequency, the two waves couple, and
IR light is absorbed

The coupled wave now vibrates with twice the amplitude

IR beam from spectrometer

“coupled” wave

EM oscillating wave
from bond vibration
D. The IR Spectrum
1. Each stretching and bending vibration occurs with a characteristic
frequency as the atoms and charges involved are different for different
bonds

The y-axis on an IR In regions where


spectrum is in units of % no osc. bond is
transmittance interacting with
IR light,
transmittance
In regions where the EM nears 100%
field of an osc. bond
interacts with IR light of
the same n –
transmittance is low
(light is absorbed)
IR Spectroscopy

D. The IR Spectrum
2. The x-axis of the IR spectrum is in units of wavenumbers, n, which is the
number of waves per centimeter in units of cm-1 (Remember E = hn or E =
hc/l)
D. The IR Spectrum
3. This unit is used rather than wavelength (microns) because
wavenumbers are directly proportional to the energy of transition
being observed – chemists like this, physicists hate it

High frequencies and high wavenumbers equate higher energy


is quicker to understand than
Short wavelengths equate higher energy

4. This unit is used rather than frequency as the numbers are more
“real” than the exponential units of frequency

5. IR spectra are observed in the range : 400-4000 cm-1

6. In general:
Lighter atoms will allow the oscillation to be faster – higher energy
This is especially true of bonds to hydrogen – C-H, N-H and O-H

Stronger bonds will have higher energy oscillations


Triple bonds > double bonds > single bonds in energy
E. The IR Spectrum – The detection of different bonds
7. As opposed to chromatography or other spectroscopic methods, the
area of a IR band (or peak) is not directly proportional to concentration
of the functional group producing the peak

8. The intensity of an IR band is affected by two primary factors:


Whether the vibration is one of stretching or bending

Electronegativity difference of the atoms involved in the bond

• For both effects, the greater the change in dipole moment in a


given vibration or bend, the larger the peak.

• The greater the difference in electronegativity between the atoms


involved in bonding, the larger the dipole moment

• Typically, stretching will change dipole moment more than bending


Infrared Spectroscopy

II. Functional Group Analysis


A. General
1. The primary use of the IR is to detect functional groups

2. Because the IR looks at the interaction of the EM spectrum with


actual bonds, it provides a unique qualitative probe into the
functionality of a molecule, as functional groups are merely different
configurations of different types of bonds

3. Since most “types” of bonds in covalent molecules have roughly the


same energy, i.e., C=C and C=O bonds, C-H and N-H bonds they
show up in similar regions of the IR spectrum

4. Remember all organic functional groups are made of multiple bonds


and therefore show up as multiple IR bands (peaks)
Infrared Spectroscopy

II. Infrared Group Analysis


A. General
5. The four primary regions of the IR spectrum

Bonds to H Triple bonds Double bonds Single Bonds

Fingerprint
Region

O-H C≡C C=O C-C


N-H C≡N C=N C-N
C-H C=C C-O

4000 cm-1 2700 cm-1 2000 cm-1 1600 cm-1 600 cm-1
Infrared Spectroscopy
Octane
1. Alkanes – combination of C-C and C-H bonds H
• C-C stretches and bends 1360-1470 cm-1
H C
H
• CH2-CH2 bending 1450-1470 cm-1 (m)

• CH2-CH3 bending 1360-1390 cm-1(m)

• sp3 C-H stretching between 2800-3000 cm-1 (s)

(w – s) (m)
Infrared Spectroscopy 1-Octene
2. Alkenes – addition of the C=C and vinyl C-H bonds
H
• C=C stretch at 1620-1680 cm-1 weaker as C
H C
substitution increases
H
• vinyl C-H stretch occurs at 3000-3100 cm-1

• The difference between alkane, alkene or alkyne C-H


is important! If the band is slightly above 3000 it is
vinyl sp2 C-H or alkynl sp C-H if it is below it is alkyl
sp3 C-H

(w – m)
(w – m)
Infrared Spectroscopy
1-Octyne
3. Alkynes – addition of the C=C and vinyl C-H bonds
• C≡C stretch 2100-2260 cm-1; strength depends on
asymmetry of bond, strongest for terminal alkynes, H C C
weakest for symmetrical internal alkynes

• C-H for terminal alkynes occurs at 3200-3300 cm-1

• Internal alkynes ( R-C≡C-R ) would not have this band!

(w-m)

(m – s)
Infrared Spectroscopy
Ethyl benzene
4. Aromatics H
• Due to the delocalization of e- in the ring, C-C bond
order is 1.5, the stretching frequency for these
bonds is slightly lower in energy than normal C=C
• These show up as a pair of sharp bands, 1500 &
1600 cm-1, (lower frequency band , s)

• C-H bonds off the ring show up similar to vinyl C-H


at 3000-3100 cm-1

(w – m) (w – m)
Infrared Spectroscopy

4. Aromatics
• If the region between 1667-2000 cm-1 (w) is free of interference (C=O stretching
frequency is in this region) a weak grouping of peaks is observed for aromatic
systems
• Analysis of this region, called the overtone of bending region, can lead to a
determination of the substitution pattern on the aromatic ring

Monosubstituted
G
G
1,2 disubstituted (ortho or o-)

G
1,2 disubstituted (meta or m-)
G
G
1,4 disubstituted (para or p-)

G
IR spectra BENZENEs
=C—H bond, “unsaturated” “aryl”
(sp2) 3000-3100 cm-1
+ 690-840
mono-substituted + 690-710, 730-770
ortho-disubstituted + 735-770
meta-disubstituted + 690-710, 750-810(m)
para-disubstituted + 810-840(m)

C=C bond 1500, 1600 cm-1


Infrared Spectroscopy

5. Unsaturated Systems – substitution patterns


• The substitution of aromatics and alkenes can also be discerned through the out-
of-plane bending vibration region
• However, other peaks often are apparent in this region. These peaks should only
be used for reinforcement of what is known or for hypothesizing as to the functional
pattern.
cm-1 cm-1
R
985-997 730-770
C CH2 905-915 R
690-710
H

R H
C C 960-980 R 735-770
H R
R
R R
C C 665-730 860-900
H H R 750-810
680-725
R
R
C CH2 885-895
R
R R 800-860
R R
C C 790-840
R H
Infrared Spectroscopy
Diisopropyl ether
6. Ethers – addition of the C-O-C asymmetric band and
vinyl C-H bonds
• Show a strong band for the antisymmetric C-O-C
stretch at 1050-1150 cm-1 O
• Otherwise, dominated by the hydrocarbon
component of the rest of the molecule

(s)
Infrared Spectroscopy
1-butanol
7. Alcohols
• Strong, broad O-H stretch from 3200-3400 cm-1 H
O
• Like ethers, C-O stretch from 1050-1260 cm -1

• Band position changes depending on the alcohols


substitution: 1° 1075-1000; 2° 1075-1150; 3° 1100-1200;
phenol 1180-1260

• The shape is due to the presence of hydrogen bonding

(m– s)
br

(s)
IR spectra ALCOHOLS & ETHERS

C—O bond 1050-1275 (b) cm-1


1o ROH 1050
2o ROH 1100
3o ROH 1150
ethers 1060-1150

O—H bond 3200-3640 (b)


Infrared Spectroscopy
2-aminopentane
8. Amines - Primary H H
• Shows the –N-H stretch for NH2 as a doublet N
between 3200-3500 cm-1 (symmetric and anti-
symmetric modes)
• -NH2 has deformation band from 1590-1650 cm-1
• Additionally there is a “wag” band at 780-820 cm-1
that is not diagnostic

(w) (w)
Infrared Spectroscopy
pyrrolidine
9. Amines – Secondary
• N-H band for R2N-H occurs at 3200-3500 cm-1
as a single sharp peak weaker than –O-H N H
• Tertiary amines (R3N) have no N-H bond and
will not have a band in this region

(w – m)
Infrared Spectroscopy

Pause and Review


• Inspect the bonds to H region (2700 – 4000 cm-1)

• Peaks from 2850-3000 are simply sp3 C-H in most organic molecules

• Above 3000 cm-1 Learn shapes, not wavenumbers!:

V-shape peak
-N—H bond for 2o
Broad U-shape peak amine (R2N—H)
-O—H bond
W-shape peak
-N—H bond for 1o
amine (RNH2)
Sharp spike 3000 cm-1
-C≡C—H bond
Small peak shouldered
just above 3000 cm-1
C=C—H or Ph—H
Infrared Spectroscopy
Cyclohexyl carboxaldehyde
10. Aldehydes O
• C=O (carbonyl) stretch from 1720-1740 cm-1 C
H
• Band is sensitive to conjugation, as are all
carbonyls (upcoming slide)

• A highly unique sp2 C-H stretch appears as a


doublet, 2720 & 2820 cm-1 called a “Fermi doublet”

(w-m)

(s)
Infrared Spectroscopy
3-methyl-2-pentanone
11. Ketones O
• Simplest of the carbonyl compounds as far as IR
spectrum – carbonyl only

• C=O stretch occurs at 1705-1725 cm-1

(s)
IR: Carbonyl Compounds
• Strong, sharp C=O peak 1670 to 1780 cm1
• Exact absorption characteristic of type of carbonyl
compound
– 1730 cm1 in saturated aldehydes
– 1705 cm1 in aldehydes next to double bond or
aromatic ring
Infrared Spectroscopy
Ethyl pivalate
12. Esters O
• C=O stretch at 1735-1750 cm-1
O
• Strong band for C-O at a higher frequency than
ethers or alcohols at 1150-1250 cm-1

(s)
(s)
Infrared Spectroscopy
4-phenylbutyric acid
13. Carboxylic Acids:
• Gives the messiest of IR spectra O
C H
• C=O band occurs between 1700-1725 cm -1 O

• The highly dissociated O-H bond has a broad band from 2400-
3500 cm-1 covering up to half the IR spectrum in some cases

(w – m) (s) (s)
br
Infrared Spectroscopy
Propionic anhydride
14. Acid anhydrides O O

• Coupling of the anhydride though the ether oxygen


splits the carbonyl band into two with a separation O
of 70 cm-1

• Bands are at 1740-1770 cm-1 and 1810-1840 cm-1

• Mixed mode C-O stretch at 1000-1100 cm-1

(s) (s)
Infrared Spectroscopy
Propionyl chloride
O
15. Acid halides
• Clefted band at 1770-1820 cm-1 for C=O
Cl
• Bonds to halogens, due to their size (see Hooke’s
Law derivation) occur at low frequencies, only Cl is
light enough to have a band on IR, C-Cl is at 600-
800 cm-1

(s)

(s)
Infrared Spectroscopy
pivalamide
O
16. Amides
• Display features of amines and carbonyl compounds
• C=O stretch at 1640-1680 cm-1 NH2

• If the amide is primary (-NH2) the N-H stretch occurs


from 3200-3500 cm-1 as a doublet

• If the amide is secondary (-NHR) the N-H stretch


occurs at 3200-3500 cm-1 as a sharp singlet

(m – s) (s)
Infrared Spectroscopy
2-nitropropane
17. Nitro group (-NO2) O
O

• Proper Lewis structure gives a bond order of 1.5 N

from nitrogen to each oxygen

• Two bands are seen (symmetric and asymmetric) at


1300-1380 cm-1 and 1500-1570 cm-1

• This group is a strong resonance withdrawing group


and is itself vulnerable to resonance effects

(s) (s)
Infrared Spectroscopy
propionitrile
18. Nitriles (the cyano- or –C≡N group) N
• Principle group is the carbon nitrogen triple C
bond at 2100-2280 cm-1

• This peak is usually much more intense than


that of the alkyne due to the electronegativity
difference between carbon and nitrogen

(s)
Infrared Spectroscopy

Effects on IR bands
1. Conjugation – by resonance, conjugation lowers the
energy of a double or triple bond. The effect of this is
readily observed in the IR spectrum:O
O

1684 cm-1 1715 cm-1


C=O C=O

• Conjugation will lower the observed IR band for a


carbonyl from 20-40 cm-1 provided conjugation
gives a strong resonance contributor
O
C X X= NH 2 CH 3 Cl NO 2
H3 C
1677 1687 1692 1700 cm -1

O O
O
N C
H 2N C CH 3 vs.
CH3
O

Strong resonance contributor Poor resonance contributor


(cannot resonate with C=O)
Infrared Spectroscopy

Effects on IR bands
1. Steric effects – usually not important in IR spectroscopy, unless they reduce the
strength of a bond (usually p) by interfering with proper orbital overlap:
O O

CH 3
C=O: 1686 cm-1 C=O: 1693 cm-1

• Here the methyl group in the structure at the right causes the carbonyl
group to be slightly out of plane, interfering with resonance

2. Strain effects – changes in bond angle forced by the constraints of a ring will
cause a slight change in hybridization, and therefore, bond strength

O O O
O O

1815 cm-1 1775 cm-1 1750 cm-1 1715 cm-1 1705 cm-1

• As bond angle decreases, carbon becomes more electronegative, as well


as less sp2 hybridized (bond angle < 120°)
Infrared Spectroscopy

Effects on IR bands
1. Hydrogen bonding
• Hydrogen bonding causes a broadening in the
band due to the creation of a continuum of bond
energies associated with it
• In the solution phase these effects are readily
apparent; in the gas phase where these effects
disappear or in lieu of steric effects, the band
appears as sharp as all other IR bands:
OH
Gas phase spectrum of
1-butanol

H
O O
Steric hindrance to H-bonding
in a di-tert-butylphenol C=O; 1701 cm-1
NOW WE WILL
MOVE FORWARD
TO SOME
QUESTIONS
Which compound is this?
a) 2-pentanone 1-pentanol
b) 1-pentanol
c) 1-bromopentane
d) 2-methylpentane
What is the compound?
a) 1-bromopentane 2-pentanone
b) 1-pentanol
c) 2-pentanone
d) 2-methylpentane
C8H6

C-H 1500, 1600


unsat’d benzene

3300 C8H6 – C6H5 = C2H


C-H mono

phenylacetylene
C4H8

Unst’d

1640- 880-
1680
900
C=C
R2C=CH2

isobutylene CH3
CH3C=CH2
tert-butyl alcohol

O-H
C-O 3o
2-butanone

 C=O
~1700 (s)
APPLICATIONS OF IR SPECTROSCOPY TO BIOMOLECULES
APPLICATIONS OF IR SPECTROSCOPY TO NATURAL
PRODUCTS/EXTRACTS

Nicotine

3400cm-1 = water, 2970, 2780 cm-1 =CH stretching , 1677 cm-1 = aromatic C=N,
1691 cm-1 = C=Cstrecting , 717 cm-1 and 904 cm-1 out of plane bending of the
C-H bond of pyridine ring
In this spectrum, we can notice several peaks, which
characterize the different chemical functions of
Nicotine:
• Around 3400 cm-1 , we can see the large peak of
water (it deals with a liquid film).
• Between 2970 and 2780 cm-1: C-H stretching.
• The peak at 1677 cm-1 : aromatic C=N double
bond stretching.
• The peak at 1691 cm-1 : aromatic C=C double
bond stretching.
• The peaks at 717 cm-1 and 904 cm-1 correspond to
the out of plane bending of the C-H bond of the
monosubstituted pyridinic cycle.
Research Work
Re-Sn Schiff base complex
N
N

O
O

NH
NH
N
N toluene,
R 2SnO
6 h

O
HO
R=C6H5 DPTC (2a)
Sn O R=CH3 DMTC (2b)
R
HO
R=C8H17 DOTC (2c)
Schif f base (1) R

CO

toluene,
16 h, -2CO
OC CO
Re +
OC CO
Br

CO
OC O

Re
OC NH
N
Br

O
R=C6H5 ReDPTC (3)
Sn
R=CH3 ReDMTC (4)
R O
R=C8H17 ReDOTC (5)
R
H
O N
FTIR spectra of Schiff base (1) N

HO

OH
70 N

60

50
Transmittance

40

30

20 3360
2826
10
2968

3390 1618
0
1677
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)
H
O N
N
FTIR spectra of Sn Schiff base complex (2a)
O
60 Sn O
N

50

40

30

20

10 735
1558
3427 1366 676
1603
0 1447
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)
N

CO
FTIR spectra of Re-Sn Schiff base complex (3) OC O

Re
OC NH
N
Br
80

70

O
60
Sn O
Ph

50
742
Ph
1195 691
2923 1350
%T

40

30 1610 1454
3442
1566
20
1951 1506

10 2032
1929
0
4000 3500 3000 2500 2000 1500 1000 500
-1
Wavenumber (cm )
Schiff base coated Fe3O4 nanoparticles

D.I. refluxed for 8 hrs.


FeCl3. 3H2O+FeSO4. 6H2O Fe3O4 Nanoparticles
NH3, pH11 +
Schiff base

Refluxing for 16 hrs.

Schiff base coated


magnetite nanoparticles
Pure Fe3O4
80 Fe3O4@SB

70
Transmittance

60
1632
631
50 1506 580
1543
40 1588
1440
30
1647
20 3412
639 572
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)
3412, 1647 cm-1 for absorbed water on surface of Fe3O4 nanoparticles.
639, 572 cm-1 for Fe-O strecthing. Presence of additional peaks in the spectra
of Fe3O4@Schiff base, majorly corresponding to C=O, C=N and C-C in the region
1500-1632 cm-1
END

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