MKK 6501 Analisis spektrometri (3 sks)

 Silabus: Membahas teori, instrumentasi dan aplikasi beberapa metode

spektrometri utama antara lain: Spektrometri UV-Visibel; Spektrometri
atom; Spektrofotometri inframerah; Spektroskopi Resonansi Magnetik Inti
dan Spektrometri Massa.
 Pustaka:
 Thomas, M., 2008, Ultraviolet and Visible Spectroscopy, 2nd Ed;
Publisher Wiley India Pvt. Limited, New Delhi.
 Broekaert, J. A. C, 2006, Analytical Atomic Spectrometry with Flames and
Plasmas; John Wiley & Sons, New York.
 Smith, B. C., 2009, Fundamentals of Fourier Transform Infrared
Spectroscopy; Edition 2, iCRC Press, Boca Raton.
 Günther, H., 2012, NMR Spectroscopy: Basic Principles, Concepts and
Applications in Chemistry; Edition 3; Wiley VCH Verlag GmbH,
Weinheim.
 Kraj, A., Desiderio, D. M., and Nibbering, N.M., 2008, Mass Spectrometry:
Instrumentation, Interpretation, and Applications, John Wiley & Sons,
New York.
Infrared (IR) Spectroscopy
????????????
Spectroscopy
“seeing the unseeable”
Using electromagnetic radiation as a probe
to obtain information about atoms and
molecules that are too small to see.
Electromagnetic radiation is propagated at
the speed of light through a vacuum as an
oscillating wave.
electromagnetic relationships:
λυ = c λ 1/υ
E = hυ E υ
E = hc/λ E 1/λ

λ = wave length
υ = frequency
c = speed of light
λ
E = kinetic energy
h = Planck’s constant c
Two oscillators will strongly interact when their
energies are equal.

E1 = E2
λ1 = λ2
υ1 = υ2

If the energies are different, they will not strongly

interact!
We can use electromagnetic radiation to probe atoms
and molecules to find what energies they contain.
some electromagnetic radiation ranges
Approx. freq. range Approx. wavelengths
Hz (cycle/sec) meters

Radio waves 104 - 1012 3x104 - 3x10-4

Infrared (heat) 1011 - 3.8x1014 3x10-3 - 8x10-7
Visible light 3.8x1014 - 7.5x1014 8x10-7 - 4x10-7
Ultraviolet 7.5x1014 - 3x1017 4x10-7 - 10-9
X rays 3x1017 - 3x1019 10-9 - 10-11
Gamma rays > 3x1019 < 10-11
Infrared radiation
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.

IR is used to tell:
1. what type of bonds are present
2. some structural information
Instrumentation
Perkin ElmerTM
Spectrum One

BRUKE TENSORTM
Series
• Dispersive instruments: with a monochromator to be
used in the mid-IR region for spectral scanning and
quantitative analysis.
• Fourier transform IR (FTIR) systems: widely applied
and quite popular in the far-IR and mid-IR spectrometry.
• Nondispersive instruments: use filters for wavelength
selection or an infrared-absorbing gas in the detection
system for the analysis of gas at specific wavelength.
 Dispersive IR spectrophotometers
Modern dispersive IR spectrophotometers are invariably double-beam
instruments, but many allow single-beam operation via a front-panel switch.

Simplified diagram of a double beam infrared spectrometer

Double-beam operation allows a stable 100% T baseline in the spectra.

Double-beam operation compensates for atmospheric absorption, for the

wavelength dependence of the source spectra radiance, the optical efficiency of
the mirrors and grating, and the detector instability, which are serious in the IR
region.single-beam instruments not practical.
 Dispersive spectrophotometers Designs

Null type instrument

 Components of dispersive spectrophotometers

1. IR source

Nernst Glower heated rare earth oxide rod 1-50 µm

(~1500 K) (mid- to far-IR)
Globar heated SiC rod (~1500 K) 1-50 µm
(mid- to far-IR)
W filament lamp 1100 K 0.78-2.5 µm
(Near-IR)
Hg arc lamp plasma 50 - 300 µm
(far-IR)
CO2 laser stimulated emission lines 9-11 µm
2. Detector / transducer
Thermocouple thermoelectric effect - cheap, slow,
dissimilar metal junction insensitive

Bolometer Ni, Pt resistance Highly sensitive

thermometer (thermistor) <400 cm-1

Pyroelectric Tri glycine sulfate fast and sensitive

piezoelectric material (mid IR)

Photoconducting PbS, CdS, Pb Se light fast and sensitive

sensitive cells (near IR)
3. Optical system
• Reflection gratings ( made from various plastics): the
groove spacing is greater (e.g. 120 grooves mm-1). To reduce
the effect of overlapping orders and stray radiation, filters or
a preceding prism are usually employed. Two or more
gratings are often used with several filters to scan a wide
region.
• Mirrors but not lenses are used to focus and collimate the
IR radiation. Generally made from Pyrex or another material
with low coefficient of thermal expansion. Front surfaces
coated with a vacuum-deposited thin metal film of Al, Ag, or
Au.
•Windows are used for sample cells and to permit various compartment to be
isolated from the environment.
 transparent to IR over the wavelength region
 inert to the various chemicals analyzed
 capable of being shaped, ground, and polished to the desired
optical quality
Fourier Transform Infrared Spectrometer (FTIR)
The Fourier transform method provides an alternatives to
the use of monochromators based on dispersion.
In conversional dispersive spectroscopy, frequencies are
separated and only a small portion is detected at any
particular instant, while the remainder is discarded. The
immediate result is a frequency-domain spectrum.
Fourier transform infrared spectroscopy generates time-
domain spectra as the immediately available data, in which
the intensity is obtained as a function of time.
Direct observation of a time-domain spectrum is not
immediately useful because it is not possible to deduce, by
inspection, frequency-domain spectra from the
corresponding time-domain waveform (Fourier transform is
thus introduced).
 Single-beam FTIR Spectrometer

In one arm of the interferometer, the IR source radiation travels through the
beam splitter to the fixed mirror back to the beam splitter through the sample
and to the detector. In the other arm, the IR source radiation travels to the beam
splitter to the movable mirror, back through the beam splitter to the sample and
to the detector. The difference in pathlengths of the two beams is the retardation
. An He-NE laser is used as a monochromatic reference source. The laser
beam is sent through the interferometer in the opposite direction to that of the IR
beam.
Double-beam FTIR
Spectrometer
 Interferometer

Michelson interferometer

If moving mirror moves 1/4 l(1/2 lround-trip) waves are out of phase at beam-
splitting mirror - no signal
If moving mirror moves 1/2 l(1 lround-trip) waves are in phase at beam-
splitting mirror – signal
...
Interferograms
Difference in pathlength called retardation 
Plot vs. signal - cosine wave with frequency proportional to light frequency but
signal varies at much lower frequency
One full cycle when mirror moves distance l/2 (round-trip = l)
VMM 2VMM
Frequency of signal: f  
l/2 l
Substituting l=c/n 2VMM
f  n VMM velocity of moving mirror
c
If mirror velocity is 1.5 cm/s

Bolometer, pyroelectric, photoconducting IR detectors can "see“ changes on 10-4

s time scale!

3cm / s
f  n  10 10
n
3 10 cm / s
10
Computer needed to turn complex interferograms into
spectra.
Measuring processes
 Advantages of FTIR
• very high resolution (< 0.1 cm –1 )
Two closely spaced lines only separated if one complete "beat" is
recorded. As lines get closer together, must increase.
Dn(cm1) 1/
Mirror motion is 1/2 
Resolution governed by distance movable mirror travels

• very high sensitivity (nanogram quantity)

can be coupled with GC analysis (–> measure IR spectra in gas-phase)

• High S/N ratios - high throughput

Few optics, no slits mean high intensity of light

• Rapid (<10 s)

• Reproducible and • Inexpensive

 To improve S/N ratio

Usually to improve resolution decrease

slit width but less light makes spectrum
"noisier" - signal to noise ratio (S/N)
S S S
 n  n
N  ( S  Si ) N
2

n # scans
S/N improves with more scans (noise is
random, signal is not!)
 Spectrum calibration
For routine instrument calibration, run the spectrum of
polystyrene film (or indene) at resolution 2 cm-1. Band
positions are available in the literature.
Higher resolution calibrations may be made from gas-
phase spectra (e.g. HCl gas).
 Sample preparation techniques
Infrared spectra may be obtained for gases, liquids or
solids (neat or in solution)

The preparation of samples for infrared spectrometry is often the most

challenging task in obtaining an IR spectrum. Since almost all substances
absorb IR radiation at some wave length, and solvents must be carefully
chosen for the wavelength region and the sample of interest.
 Gas samples
• A gas sample cell consists of a cylinder of glass or sometimes a metal.
The cell is closed at both ends with an appropriate window materials
(NaCl/KBr) and equipped with valves or stopcocks for introduction of the
sample.
• Long pathlength (10 cm) cells – used to study dilute (few molecules)
or weakly absorbing samples.
• Multipass cells – more compact and efficient instead of long-pathlength
cells. Mirrors are used so that the beam makes several passes through
the sample before exiting the cell. (Effective pathlength  10 m).
• To resolve the rotational structure of the sample, the cells must be
capable of being evacuated to measure the spectrum at reduced
pressure.
• For quantitative determinations with light molecules, the cell is
sometimes pressurized in order to broaden the rotational structure and
all simpler measurement.
 Liquid samples
• Pure or soluted in transparent solvent – not water (attacks windows)
•The sample is most often in the form of liquid films (“sandwiched”
between two NaCl plates)
• Adjustable pathlength (0.015 to 1 mm) – by Teflon spacer
 Regions of transparency for common infrared
solvents.

The horizontal lines indicate regions where solvent transmits at least 25% of
the incident radiation in a 1-mm cell.
 Solid samples
• Spectra of solids are obtained as alkali halide discs (KBr), mulls
(e.g. Nujol, a highly refined mixture of saturated hydrocarbons) and
films (solvent or melt casting)

Alkali halide discs:

1. A milligram or less of the fine ground sample mixed with about
100 mg of dry KBr powder in a mortar or ball mill.
2. The mixture compressed in a die to form transparent disc.
Mulls
1. Grinding a few milligrams of the powdered sample with a mortar
or with pulverizing equipment. A few drops of the mineral oil
added (grinding continued to form a smooth paste).
2. The IR of the paste can be obtained as the liquid sample.
 Main uses of IR spectroscopy:
1. Fundamental chemistry
Determination of molecular structure/geometry.
e.g. Determination of bond lengths, bond angles of
gaseous molecules

2. Quantitative analysis – simple, fast,

nondestructive
Monitoring trace gases: NDIR.Rapid, simultaneous
analysis of GC, moisture, N in soil. Analysis of fragments
left at the scene of a crime
Quantitative determination of hydrocarbons on filters, in
air, or in water
 Near-infrared and Far-infrared absorption

The techniques and applications of near-infrared (NIR) and

far-infrared (FIR) spectrometry are quite different from those
discussed above for conventional, mid-IR spectrometry.

Near-infrared: 0.8 -2.5 m, 12500 - 4000 cm-1

Mid-infrared: 2.5 - 50 m, 4000 - 200 cm-1
Far-infrared: 50 - 1000 m, 200 - 10 cm-1
 Near-infrared spectrometry

NIR shows some similarities to UV-visible spectrophotometry and some to mid-

IR spectrometry. Indeed the spectrophotometers used in this region are often
combined UV-visible-NIR ones.
The majority of the absorption bands observed are due to overtones (or
combination) of fundamental bands that occur in the region 3 to 6 m, usually
hydrogen-stretching vibrations.
NIR is most widely used for quantitative organic functional-group analysis. The
NIR region has also been used for qualitative analyses and studies of hydrogen
bonding, solute-solvent interactions, organometallic compounds, and inorganic
compounds.
 Far-infrared spectrometry

Almost all FIR studies are now carried out with FTIR spectrometers.
The far-IR region can provide unique information.
i) The fundamental vibrations of many organometallic and inorganic
molecules fall in this region due to the heavy atoms and weak bonds in
these molecules.
ii) Lattice vibrations of crystalline materials occur in this region,
iii) Electron valence/conduction band transition in semiconductors often
correspond to far-IR wavelengths.
IR source  sample  prism  detector

graph of % transmission vs. frequency

=> IR spectrum

100

%T

0
4000 3000 2000 1500 1000 500

v (cm-1)
IR region and vicinity
 Infrared Energy Modes

 IR energy absorption corresponds to specific

modes, corresponding to combinations of atomic
movements, such as bending and stretching of
bonds between groups of atoms called “normal
modes”
 Energy is characteristic of the atoms in the group
and their bonding
 Corresponds to vibration and rotations
Hukum Hooke :
Hukum Hooke :

 3700 - 2500 cm-1: X-H stretching (X = C,N,O,S)

 2300 - 2000 cm-1: C  X stretching (X = C or N)
 1900 - 1500 cm-1: C=X stretching (X = C, N, O)
 1300 - 800 cm-1: C-X stretching (X = C, N, O)
Molecular Vibrations
1. Absorption of infrared radiation corresponds to energy
changes on the order of 8-40 KJ/mole (2-10 Kcal/mole)
2. The frequencies in this energy range correspond to the
stretching and bending frequencies of the covalent
bonds with dipole moments.
3. Stretching (requires more energy than bending)
a. Symmetrical
b. Asymmetrical
4. Bending
a. Scissoring (in-plane bending)
b. Rocking (in-plane bending)
c. Wagging (out-of-plane bending)
d. Twisting (out of plane bending)
Infrared Energy Modes
Stretching – A rhythmical movement along the bond axis
such that the interatomic distance is
increasing or decreasing.
In any group of three or more atoms – at least two of which
are identical - there are two modes of stretching or
bending: Symmetric and Asymmetric

For the Methylene Group (CH2):

H H
C—H C C
H H
Symmetric Asymmetric
Stretch Stretch
(2853 cm-1) (2926 cm-1)
Bending – A movement of a group of atoms with respect
to the remainder of the molecule

Scissoring H Wagging
H H
~1450 cm-1 C ~1250 cm-1
(In Plane) (Out of Plane)
C
H

Rocking H Twisting H H
~750 cm-1 C ~1250 cm-1 C
(In Plane) H (Out of Plane)
 Thus, no two molecules of different structure will have
exactly the same natural frequency of vibration, each will
have a unique infrared absorption pattern or spectrum.

 Two Uses:
1. IR can be used to distinguish one compound from
another.
2. Absorption of IR energy by organic compounds will occur
in a manner characteristic of the types of bonds and atoms
in the functional groups present in the compound; thus,
infrared spectrum gives structural information about a
molecule.
 The absorptions of each type of bond (N–H, C–H, OH,

C–X, C=O,C–O, C–C, C=C, CC, CN, etc.) are regularly

found only in certain small portions of the vibrational

infrared region, greatly enhancing analysis possibilities.

 Common Structural Units
Stretching Vibrations
Stretching Vibrations (Double Bonds)
Stretching Vibrations (Double Bonds)
O HC C(alcohols) 3200-3600
1620-1680
C C
O HC O(carboxylic 2500-3600
acids)
Aldehydes and ketones 1710-1750
1620-1680
Carboxylic acids 1700-1725
N H
Acid anhydrides
3350-3500
1800-1850 and 1740-1790
Acyl halides 1770-1815
C O
Esters 1730-1750

sp C H
Amides 3310-3320
1680-1700

Aldehydes and ketones 1710-1750

sp2 C H 3000-3100 Carboxylic acids 1700-1725
Acid anhydrides 1800-1850 and 1740-1790
sp3 C H 2850-2950 Acyl halides 1770-1815
Esters 1730-1750
sp2 C O 1200
Amides 1680-1700

sp3 C O 1025-1200
Bending Vibrations (Diagnostic)
Alkenes:

cis-disubstituted 665-730

trans-disubstituted 960-980

trisubstituted 790-840
Stretching Vibrations Triple Bonds)
C C 2100-2200

C N 2240-2280

Substituted derivatives of benzene

monosubstituted 730-770 and 690-710
ortho-disusbstituted 735-770
meta-disubstituted 750-810 and 680-730
para-substituted 790-840
Serapan gugus fungsional pada Infra merah
Regions of the Infrared Spectrum
 Spectra Infrared
IR Spectrum Peak Characteristics
1.Primary Examination Regions of the Spectrum
 High Frequency Region - 4000 to 1300 cm-1
 Intermediate (Fingerprint Region) - 1300 to 900 cm-1
2.High Frequency Region (Functional Group Region)
 Characteristic Stretching frequencies of such groups
as:
=CH, OH, NH, C=O, CO, CN, CC, C=C
3.The Fingerprint Region
 Absorption patterns frequently complex
 Bands originate from interacting vibrational modes
 Valuable when used in reference to other regions
 Absorption unique for every molecular species
 Effective use comes from experience
 Infrared Spectroscopy (IR)
IR Spectrum Peak Characteristics (con’t)
Shape
 Sharp (narrow)
 Broad
Intensity
 Weak (w)
 Medium (m)
 Strong (s)
Note: Peak intensity is dependent on amount of sample
and sensitivity of instrument; therefore, the actual
intensity can vary from spectrum to spectrum
 Infrared Spectra of Hydrocarbons
 C-H, C-C, C=C, C  C have characteristic peaks
Hexane
Alkenes
1-Hexene
Alkynes
 IR: Aromatic Compounds
 Weak C–H stretch at 3030 cm1
 Weak absorptions 1660 - 2000 cm1 range
 Medium-intensity absorptions 1450 to 1600 cm1
Phenylacetylene
Cyclohexane or Cyclohexene?
The infra-red spectrum for a
simple carboxylic acid

ETHANOIC ACID

carbon-oxygen double, C=O

carbon-oxygen single, C-O
oxygen-hydrogen, O-H
carbon-hydrogen, C-H
carbon-carbon single, C-C
IR: Alcohols
Infrared Absorption Spectrum of Ethanol
dilute t-butanol in choloroform
t-butanol
 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
 C=O in Ketones
 1715 cm1 in six-membered ring and acyclic ketones
 1750 cm1 in 5-membered ring ketones
 1690 cm1 in ketones next to a double bond or an aromatic
ring
 C=O in Esters

 1735 cm1 in saturated esters

 1715 cm1 in esters next to aromatic ring or a
double bond
Practice problem:
Phenylacetaldehyde
The infra-red spectrum for a ketone
Propanone
Amines
The infra-red spectrum for a primary amine
1-aminobutane
 Analyzing the Spectrum – A Suggested Approach
Step 1. – Check for the presence of the Carbonyl group (C=O) at
1715 cm-1. If molecule is conjugated, the strong (C=O)
absorption will be shifted to the right by ~30 cm-1,
i.e. ~1685 cm-1
If the carbonyl absorption is present, check for:
 Carboxylic Acids - Check for OH group (broad absorption
near 3300-2500 cm-1)
 Amides - Check for NH group
(1 or 2 absorptions near 3500 cm-1)
 Esters - Check for C-O group (medium
absorptions near 1300-1000 cm-1)
 Anhydrides - Check for 2 C=O absorptions near
1810 and 1760 cm-1
 Aldehydes - Check for Aldehyde CH group (2 weak
absorptions near 2850 and 2750 cm-1)
 Ketones - Ketones (The above groups have been
eliminated)
 IR Spectrum Isobutyric Acid
Carboxylic Acids

C4H8O2
IR Spectrum Benzamide
Amides

C7H7NO
IR Spectrum Methyl Benzoate
Esters

C8H8O2
IR Spectrum Nonanal
Aldehydes

C9H18O
IR Spectrum Methyl Isopropyl Ketone
Ketones

C5H10O
Step 2. - If the Carbonyl Group is Absent Check for Alcohols,
Amines, or Ethers.
 Alcohols & Phenols - Check for OH group (Broad
absorption near 3600-3300 cm-1
Confirm present of CO near
1300-1000 cm-1
 Amines - Check for NH stretch (Medium
absorptions) near 3500 cm-1
Primary Amine - 2 Peaks
Secondary Amine - 1 Peak
Tertiary Amine - No peaks
N-H scissoring at 1560 - 1640 cm-1
 Ethers - Check for C-O group near 1300-
1000 cm-1 and absence of OH
 IR Spectrum Propargyl Alcohol
Alkynes (CC)

C3H4O HC CCH2OH
 IR Spectrum
Alcohols & Phenols 2-Naphthol

C10H9O
IR Spectrum
Amines n-butylamine

C4H11N
IR Spectrum Butyl Ether
Ethers

C8H18O CH3(CH2)3 – O – (CH2)3CH3

Step 3. – Refine the Structure Possibilities by Looking for
Double Bonds, Triple Bonds and Nitro Groups
 Double Bonds - C=C is weak absorption near 1650 cm-1
Aliphatics occur on right side of
3000 cm-1.
Unsaturated C=C or CC bonds show
an absorption on the left side of 3000
cm-1.
 Triple Bonds - CN (medium, sharp absorption near
2250 cm-1
CC (weak, sharp absorption near
2150 cm-1
 Nitro Groups - Two strong absorptions 1600-1500 cm-1
and 1390-1300 cm-1
Step 3 (Con’t)
Aromatic Ring Absorptions
 Aromatic unsaturated C=C bonds show an absorption
on the left side of 3000 cm-1, but the aromaticity must
be verified in the overtone region (1667 - 2000cm-1) and
the out-of-plane (OOP) region (900 - 690 cm-1)
 Medium to strong absorption in region 1650 - 1450 cm-1
 Many weak combination and overtone absorptions
appear between 2000 and 1667 cm-1
The relative shapes and numbers (1 - 4) of the overtone
absorptions can be used to tell whether the aromatic
ring is monosubstituted or di-, tri-, tetra-, penta-, or
hexasubstituted.
Positional (ortho-, meta-, para-) isomers can also be
distinguished.
Note: A strong carbonyl absorption can overlap these
overtone bands, making them unusable.
Step 3 (Con’t)
Aromatic Ring Absorptions (Con’t)
 The unsaturated =C-H “Out-of-Plane (OOP) bending
absorptions in the region 900 – 690 can also be used
to determine the type of ring substitution.
 The number of absorptions and their relative positions
are unique to each type of substitution.
 Although these absorptions are in the “fingerprint”
region they are particularly reliable for rings with alkyl
group substitutions.
 They are less reliable for polar substituents.
IR Spectrum
Nitriles
Benzonitrile

C7H5N
 IR Spectrum Propargyl Alcohol
Alkynes (CC)

C3H4O HC CCH2OH
 IR Spectrum Nitro Benzene
Nitro Compounds

C6H5NO2
Step 4. If none of the above apply then the compound is
most likely a hydrocarbon.

Generally, very simple spectrum

Hydrocarbons - Check for main absorptions near

right side of 3000 cm-1
IR Spectrum
Alkane Decane

C10H22 CH3(CH2)8CH3
 IR Analysis Scheme
Carbonyl (C=O) @ 1715-1685
(Conjugation moves absorption to right ~30 cm-1

Yes No

Acid

Alcohol
Ester
Amine
Ether
Amide
Saturation Unsaturation
< 3000 cm-1 > 3000 cm-1
Anhydride

Aldehyde Alkanes -C-H Alkenes (Vinyl) -C=C

Methylene -CH2 Alkynes (Acetylenes) -CC
Methyl -CH3 Aromatic -C=C
Ketone

Nitriles Hydrocarbons Nitro

 IR Analysis Scheme

Carbonyl (C=O) is Present

Acid - Broad OH Absorp @ 3300-2500 cm-1

Ester - C-O Absorp @ 1300-1000 cm-1

Amide - NH absorp @ 3500 cm-1 (1 or 2 peaks)
Anhydride - 2 C=O absorptions 1810 & 1760 cm-1
Aldehyde - Aldehyde C-H absorp @ 2850 & 2750 cm-1
Ketone - None of the above except C=O

Carbonyl is Absent
Alcohol - Broad OH absorp @ 3300 - 3000 cm-1
Also C-O absorp @ 1300 - 1000 cm-1

Amine - 1 to 2 equal NH absorp @ 3500 cm-1

Ether - C-O absorp @ 1300 - 1000 cm-1
 IR Analysis Scheme
Saturation

Alkanes -C-H Stretch – several absorptions to “right” of 3000 cm-1

Methylene -CH2 1450 cm-1
Methyl -CH3 1375 cm-1

Unsaturation

Double Bonds =C-H Stretch – several absorptions to “left” of 3000 cm-1

OOP bending at 1000 – 650 cm-1
Alkenes (Vinyl) -C=C Stretch (weak) @ 1675 – 1600 cm-1
Conjugation moves absorption to the right
Alkynes -CH Terminal Alkyne Stretch at 3300 cm-1
Alkynes (Acetylenes) -CC Stretch @ 2150 cm-1
Conjugation moves absorption to the right
Aromatic =C-H Stretch absorptions also to left of 3000 cm-1
OOP bending at 900 – 690 cm-1
OOP absorption patterns allow determination of
ring substitution (p. 902 Pavia text)
-C=C 4 Sharp absorptions (2 pairs) @ 1600 & 1450 cm-1
Overtone absorptions @ 2000 – 1667 cm-1
Relative shapes and numbers of peaks permit
determination of ring substitution pattern (p. 902 Pavia text).
 Sample Preparation
1. IR spectra of liquids.
IR spectra of liquid compounds may be obtained either
from the neat liquid or from a solution of the liquid in an
appropriate solvent. It is generally desirable to obtain the
spectrum from the neat liquid, if possible, since
interference by solvent absorption is thereby avoided.
2. IR spectra of solids.
- The Mull Method. In this method, the solid sample is
thoroughly ground up, using an agate mortar and pestle,
with a weakly absorbing, non-volatile liquid to form a
thick paste, called a mull.
- The KBr pellet Method. In this method, the solid sample
is finely pulverized with pure, dry KBr, the mixture is
pressed in a hydraulic press to form a transparent pellet,
and the spectrum of the pellet is measured.
Latihan soal : Rumus Molekul : C5H10O
Rumus molekul C8H8O
Analysis: C7H8O
Analysis: C8H7N
Analysis: C7H6O
Analysis: C3H10NO
Analysis: C4H8O2
Analysis:
C7H5OCl
Analysis: C4H6