FTIR Review

Chem 228 WS/2012

The Electromagnetic Spectrum
‡ Radiation in the infrared region (IR) corresponds to stretching, bending, etc. of chemical bonds.

Modeling of IR Absorption
‡ Bonded atoms can be modeled as masses on springs.

‡ m is the atomic mass of the bonded atoms. .‡ k is proportional to the bond strength.

. ‡ IR absorption measurements are therefore useful for determination of organic functional groups.IR Spectra ‡ IR frequencies which cause resonance of the masses/springs are absorbed selectively. (~4000-400 cm-1) ‡ Symmetrical groups may NOT show up in IR due to requirement for a bond dipole moment.

combinations) occur in the ³fingerprint´ region of the IR spectrum (~1500-400 cm-1). absorptions corresponding to harmonics (overtones. ‡ Pattern matching in the IR ³fingerprint´ region is useful to identify the specific compound involved. .Fingerprint IR Absorptions ‡ In addition to the fundamental resonance frequencies.

Grating IR Spectrometer .

FTIR Spectrometer .

.Nicolet 750 Magna-IR ‡ This is the FTIR in the organic lab.

.FTIR of Liquid Samples ‡ NaCl plates are used for liquids since glass would absorb in the IR. ‡ A thin layer of liquid is sandwiched between two NaCl plates and placed in the beam path.

since the sample thickness can be controlled. .Liquid Samples-Sealed Cells ‡ Sealed cells allow IR of volatile liquids and quantitative measurements.

.Liquid or Solid Samples-ATR ‡ ATR=Attenuated Total Reflectance ‡ IR beam is reflected off surface of sample via a high RI prism (ZnSe).

‡ KBr disk is prepared by grinding the sample with KBr and pressing in a die to form a transparent disk. ‡ Nujol mull is prepared by grinding the sample in mineral oil.FTIR of Solid Samples ‡ Solids are usually run as KBr disks or Nujol (mineral oil) mulls. .

‡ Spectral artifacts (extra peaks) may occur if the disk is poorly made. . ‡ Nujol mulls show hydrocarbon IR spectrum superimposed on sample peaks.FTIR of Solid Samples ‡ KBr disks can be hard to make well.

.FTIR of Solid Samples ‡ KBr disk holder.

‡ (We do not currently have one of these.FTIR Microscope ‡ Microscope uses mirrors to avoid the need for NaCl lenses.) .

FTIR Microscopy .

Fiber Optic FTIR Dip Probe ‡ Useful for continuous process monitoring. .

. which make a convenient visual reference. ‡ Most organic compounds contain C-H single bond absorptions.FTIR Spectral Interpretation ‡ Most organic functional groups absorb somewhere between 4000-400 cm-1.

‡ Substituting D for H would shift peak location to right (lower energy) on plot.FTIR Spectral Interpretation ‡ Normal organic IR range is 4000-400 cm-1 ‡ Energy is directly related to cm-1 ‡ E=(k/m)0.5. . so going from C-C to C=C to triple bonds should shift peak location to left (higher energy) on plot.

FTIR Spectral Interpretation ‡ Table (visual) .

hexane .

3-dimethylbutane .2.

since C skeleton is the main difference.n-hexane vs 2. .3-dimethylbutane ‡ IR¶s are very similar-not the best method to identify.

NMR would be best for n-hexane vs 2.3-dimethylbutane ‡ n-hexane 13C ‡ 1H ‡ 13C .3-dimethylbutane ‡ 2.

toluene .

1-hexene .

1-heptyne .

Heptyl cyanide .

3-heptanone .

heptaldehyde .

1-hexanol .

‡ Pattern matching in the fingerprint region or NMR could determine which alcohol. .1-propanol vs 2-propanol ‡ IR shows ±OH group.

1-hexylamine .

Heptanoic acid .

Ethyl acetate .

Butyric anhydride .

(eg. ‡ KBr disk technique for solids may generate artifacts. making spectral interpretation difficult or misleading.IR-Problems ‡ Impurities also absorb. . moisture in sample) ‡ Film thickness for liquids may alter relative intensity of peaks.

Sample Thickness Effect on FTIR Too thick Thickness OK .

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