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(FTIR)
Bruker Tensor 27
http://pubs.rsc.org/en/content/articlelanding/2016/re/c6re00127k/unauth#!divAbstract
Instrument Center
Faculty of Science and Technology
Prince of Songkla University
Pattani campus
Contents
Workshop 62
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Schedule of
“Using Fourier Transform Infrared Spectrometer (FTIR) Bruker Tensor 27” Training
January 6th, 2017
At Instrument Center, 2nd floor, Building 71 (Pre-Clinical Building)
Faculty of Science and Technology, Prince of Songkla University
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Training of
“Using Fourier Transform Infrared Spectrometer (FTIR) Bruker Tensor27” Training
January 6th, 2017
At Instrument Center, 2nd floor, Pre-Clinical Building
Faculty of Science and Technology, Prince of Songkla University
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17 Miss Mariam Salaemae 4th year, Bachelor's degree, Chemistry and biology 1
18 Miss Suhailanee Chesu 4th year, Bachelor's degree, Chemistry and biology 2
19 Miss Aseeyah Adae 4th year, Bachelor's degree, Chemistry and biology 1
20 Miss Rohana Epong 4th year, Bachelor's degree, Chemistry and biology 2
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 1
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 2
IR Spectroscopy Training 1
Page 2
What is spectroscopy ?
Electromagnetic Radiation
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 3
Electromagnetic Radiation
Graphics source: Wade, Jr., L.G. Organic Chemistry, 5th ed. Pearson Education Inc., 2003
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 4
IR Spectroscopy Training 2
Page 3
Infrared radiation
Infrared radiation = Thermal radiation
Infra = beyond
Infrared = beyond red region
Beyond the Visible
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 5
Source: NASA
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 6
IR Spectroscopy Training 3
Page 4
2.5-25 m
Infrared light
4000-500 cm-1
Wave number, = 1
Wave number(cm-1), = 10000
(m)
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 7
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 8
IR Spectroscopy Training 4
Page 5
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 9
IR Chemical Transmitted
light Detector
source sample
4000-500 cm-1
absorb specific frequencies
* Chemical Bonds *
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 10
IR Spectroscopy Training 5
Page 6
IR spectroscopy
• Absorption technique
• A kind of vibrational spectroscopy
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 11
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 12
IR Spectroscopy Training 6
Page 7
Sources :© http://namrataheda.blogspot.com/2014/01/spectrophotometry-ir-spectroscopy.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 13
Bending Vibrations
Sources :© http://namrataheda.blogspot.com/2014/01/spectrophotometry-ir-spectroscopy.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 14
IR Spectroscopy Training 7
Page 8
Infra-red spectrum?
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 15
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 16
IR Spectroscopy Training 8
Page 9
Absorbance IR
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 17
Polar bonds
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 18
IR Spectroscopy Training 9
Page 10
bondmass
strength
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 19
IR absorption range
Graphics source: Wade, Jr., L.G. Organic Chemistry, 5th ed. Pearson Education Inc., 2003
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 20
IR Spectroscopy Training 10
Page 11
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 21
broad
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 22
IR Spectroscopy Training 11
Page 12
alpha,beta–unsaturated aldehydes,
1710–1665 (s) C=O stretch
ketones
1680–1640 (m) –C=C– stretch alkenes
1650–1580 (m) N–H bend primary amines
1600–1585 (m) C–C stretch (in–ring) aromatics
1550–1475 (s) N–O asymmetric stretch nitro compounds
1500–1400 (m) C–C stretch (in–ring) aromatics
1470–1450 (m) C–H bend alkanes
1370–1350 (m) C–H rock alkanes
1360–1290 (m)
IR Spectroscopy N–O symmetric stretch
Training nitro compounds
Asst.Prof.Dr. Vanida Chairgulprasert 24
IR Spectroscopy Training 12
Page 13
IR spectra
• functional groups.
• a molecular fingerprint
• does not proof of molecular structure
• must be used in conjunction with other techniques to
provide a molecular structure.
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 26
IR Spectroscopy Training 13
Page 14
O
CH3C H 2C H2 CH 2 CH2-C -O-H
O
C -O-C H2C H3
CH3-CH2-O-H
CH 3
Cl-C H2 -CHC H3
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 27
Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/aldehydesir.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 28
IR Spectroscopy Training 14
Page 15
Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/carbacidsir.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 29
Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/estersir.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 30
IR Spectroscopy Training 15
Page 16
Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/alcoholsir.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 31
Source:http://orgchem.colorado.edu/Spectroscopy/irtutor/ketonesir.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 32
IR Spectroscopy Training 16
Page 17
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 33
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 34
IR Spectroscopy Training 17
Page 18
Alkane
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 35
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 36
IR Spectroscopy Training 18
Page 19
Alcohol
C4H9OH
OH OH
OH
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 38
IR Spectroscopy Training 19
Page 20
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 39
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 40
IR Spectroscopy Training 20
Page 21
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 41
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 42
IR Spectroscopy Training 21
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IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 43
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 44
IR Spectroscopy Training 22
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Quantitative Applications
Notes
• Quantitative data obtained with infrared instruments are generally
significantly inferior in quality to data obtained with ultraviolet/visible
spectrophotometers
• Because of the greater complexity of the spectra, the narrowness of
the absorption bands, and the instrumental limitations of infrared
instruments
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 45
Infrared Spectrometer
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 46
IR Spectroscopy Training 23
Page 24
Source: http://www.chemicool.com/definition/fourier_transform_infrared_spectrometer_ftir.htm
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 47
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 48
IR Spectroscopy Training 24
Page 25
Source: http://epic.ms.northwestern.edu/KeckII/ftir1.asp
© 2009 NUANCE. All rights reserved. Northwestern University, 2220 Campus Drive #2036, Evanston, IL 60208-3108
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 49
Preparation of sample
• Gas
• Liquid
• Solid
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 50
IR Spectroscopy Training 25
Page 26
Gas sample
- gas cell
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 51
Liquid samples
• Neat liquids
- thin film on salt plate
- making a sandwich
(made of NaCl or KBr)
Be careful : without moisture in the
samples
: not for aqueous samples
• Solution
using a liquid cell
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 52
IR Spectroscopy Training 26
Page 27
The solvent must not affect the material, (sodium chloride, the cell)
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 53
Cells: are transparent to the infrared light and do not introduce any
lines onto the spectra.
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 54
IR Spectroscopy Training 27
Page 28
Solid samples
• KBr Pellet Method
The concentration of the sample in KBr (anhydrous solid)
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 55
•Nujol mulls
a small drop of mineral oil (nujol), KBr plate
• solution
• thin film
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 56
IR Spectroscopy Training 28
Page 29
Polystyrene
Cl
Cl C Cl
Cl
no C-H!
C-Cl stretch
Carbon Tetrachloride
IR Spectroscopy Training 29
Page 30
59
IR Spectroscopy Training 30
Part 2
Using and Maintenance of FTIR
(Bruker Tensor 27)
Page 31
Using
Bruker Tensor27 FTIR
Pisipong Meunprasertdee
Scientist
Instrument Center
Faculty of Science and Technology 1
Sample Preparation
2
Page 32
g
- Organic Powder - Metal complex
p
- Ingredients in cosmetic - Pharmaceutical
- Food and Diary product - Polymer
- Azo dye - Catalyst
- Packaging - Gemstone
- Rubber
- Electronic
Gas sample
4
Page 33
Liquid Sample
Organic and Inorganic compounds
Transmission Technique
IR light sample
detector
4 volatile, scentless
4 quantitative application
8
Page 35
Transmission KBr-pellet :
Reflectance Technique
sample
IR light
detector
η1 • sinθ1 = η2 • sinθ2
Substance n2
Φ Φ
Θ
θ1 : incidence angle
Θ
(Medium 1)
Θ θ2 : refraction angle
Crystal n1 η1 : refraction index of medium 1 (crystal)
η2 : refraction index of medium 2 (sample)
a) b) c) d)
The angle of incidence beam is higher than the critical angle of crystal
11
Sample Sample
n2
Refraction index
n1 > n2
ATR crystal n1 Θ
η1 > η2
ATR crystal
12
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13
2) Diffuse Reflectance
Diffuse reflectance occurs when the scattered
(reflected randomly) light is collected and
measured. It is used to analyze a wide variety of
solid samples.
Specular Energy
Diffuse Energy
SAMPLE CUP
14
Page 38
Using
Bruker Tensor27 FTIR
16
Page 39
Turning on FTIR
1. Turn on UPS and computer
17
Turning on HPLC
2. Open “OPUS” software by clicking OPUS
icon, password is “OPUS” then click “Login”
18
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19
OPUS workplace
20
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44. Click
Cli k “L
“Load”
d” tto choose
h
technique
21
22
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23
7. Back to “Advanced”
24
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25
26
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27
28
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29
30
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31
33
34
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35
36
Page 49
- Add “Annotation”
37
- Add “Annotation”
38
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- Peak picking
39
- Peak picking
40
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41
42
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43
44
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45
- Click save
46
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Other function
47
Manipulation : AB ↔ TR conversion
90
80
70
mittance [%]
60
Transm
50 40
30
20
AB = - log (TR)
Wavenumber cm-1
0.7
0.6 0.5
Benefit of AB
AB--spectra
spectra::
Absorbance Units
to concentration
0.3 0.2
0.1
48
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber cm-1
Page 55
Before
Baseline Correction
49
50
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Manipulation: Cut
51
52
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Unknown
Library
Unknown Drug
Library
53
54
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Structure Information
Spectrum
55
Evaluation : Quantitative
56
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Quick Print
Prints current content of spectrum
window
d without
th t preview
Print Spectra
Print spectra via menue
60
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62
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Workshop
Operator name : ….…………………………….……..… Code ………….………
Workshop 1 Preparation of sample
- Prepare unknown A and B powder by press with KBr powder
What unknown?
Choices
1. Acetone
2. Ascorbic acid Answer
3. Ethylbenzoate A=
4. Eugenol
B=
5. Glycerol
6. Palmitic acid C=
7. Polyethylene D=
8. Polypropylene E=
9. Polystyrene
10. Polyvinylchloride
11. Salicylic acid
12. Steroid
13. TritonX
14. Toluene
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Installation of
OPUS Program
1
2
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4
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6
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8
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