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Fourier Transform Infrared Spectroscopy

(FTIR)
Bruker Tensor 27

http://pubs.rsc.org/en/content/articlelanding/2016/re/c6re00127k/unauth#!divAbstract

January 6th, 2017

Instrument Center
Faculty of Science and Technology
Prince of Songkla University
Pattani campus
Contents

 Part 1 Principle and application of Infrared Spectroscopy 1-30

 Part 2 Using and Maintenance of FTIR 31-61

 Workshop 62

 Installation of OPUS program 63-67

@@@@@@@@@@@@@@@@@@
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
*******************************

January 6th, 2017


08.15 - 08.30 am Registration
08.30 - 08.45 am Inauguration
08.45 – 10.45 am Introduction of FTIR
Asst. Prof. Dr. Vanida Chairgulprasert
10.45 – 11.00 am Coffee Break
11.00 am – 12.00 pm Using and Maintenance of FTIR (Bruker Tensor 27)
Mr.Pisipong Meunprasertdee
12.00 – 01.00 pm Launch
01.00 – 02.30 pm Workshop #1 Preparation of sample (KBr powder, KBr pellet)
Workshop #2 Using FTIR (Bruker Tensor 27)
02.30 – 02.45 pm Coffee Break
02.45 – 04.15 pm Workshop #1 Preparation of sample (KBr powder, KBr pellet)
Workshop #2 Using FTIR (Bruker Tensor 27)
04.15 – 04.30 pm Test FTIR principle and using

***********************************
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

*******************************

No Name - Surname Year/Degree/Major Group Signature


st
1 Miss Jennifer Osamede 1 year, Master's degree, Food Science and 1
Nutrition
2 Mr.Alam Surya Wijaya 1st year, Master's degree, Sustainable Energy 2
Management
3 Miss Thaksaporn Banda 4th year, Bachelor's degree, Rubber Technology 1

4 Mr. Kamaruddin Waesateh 1st year, Master's degree, Polymer Technology 2

5 Mr. Mohamad Irfan 1st year, Doctor's degree, Polymer Technology 1


Fathurrohman
6 Miss Sitihaya Malibo 4th year, Bachelor's degree, Industrial Chemistry 2

7 Miss Thitima Supapan 4th year, Bachelor's degree, Industrial Chemistry 1

8 Miss Porntip Madlah 4th year, Bachelor's degree, Industrial Chemistry 2

9 Mr. Sampan Sengliang 4th year, Bachelor's degree, Industrial Chemistry 1

10 Miss Sakeeyah Masamae 4th year, Bachelor's degree, Industrial Chemistry 2

11 Mr. Damrong Adam 4th year, Bachelor's degree, Industrial Chemistry 1

12 Miss Solihah Binnuy 4th year, Bachelor's degree, Industrial Chemistry 2

13 Miss Umaporn Sangthong 4th year, Bachelor's degree, Industrial Chemistry 1

14 Mr. Anun salaeh 4th year, Bachelor's degree, Industrial Chemistry 2

15 Mr.Trin Khawsang 4th year, Bachelor's degree, Industrial Chemistry 1


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

*******************************

No Name - Surname Year/Degree/Major Group Signature


th
16 Mr.Nitipon Jeni 4 year, Bachelor's degree, Industrial Chemistry 2

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

21 Miss Pornpimol Powijit 4th year, Bachelor's degree, Chemistry (Education) 1

22 Miss Winanya Ngasaman 4th year, Bachelor's degree, Chemistry (Education) 2

23 Mr.Tanawat Wattanakul 4th year, Bachelor's degree, Chemistry (Education) 1

24 Miss Sininat Chansuk 4th year, Bachelor's degree, Chemistry (Education) 2


Part 1
Principle and Application of
Infrared Spectroscopy
Page 1

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 ?

Spectroscopy is the study of the interaction


between matter and electromagnetic radiation.

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

Courtesy NASA/JPL-Caltech, Linda Hermans-Killam

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 5

Source: NASA

Dicovery of Infrared Radiation

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)

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

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 7

What is Infrared Spectroscopy?


Infrared Spectroscopy is the analysis of infrared light
interacting with a molecule

The Mid IR range


= 2-50 m
 = 4000-500 cm-1

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 8

IR Spectroscopy Training 4
Page 5

A technique which reveals the bonds present in


a compound and therefore can be used to identify
functional groups in a molecule.

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 *

detects the transmitted frequencies,


reveals the values of the absorbed frequencies.

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 10

IR Spectroscopy Training 5
Page 6

Absorption of infrared radiation brings about changes


in molecular vibrations within molecules and
measurements of the ways in which bonds vibrate
gives rise to infrared spectroscopy.

IR spectroscopy
• Absorption technique
• A kind of vibrational spectroscopy

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 11

Infrared radiation stimulates molecular vibrations.


Fundamental vibration 2 Different Types

Stretching vibration : change of bond length

Bending vibration : change of bond length

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

In big molecules, there are many bonds and so a


large number of possible stretches and bends are
possible. The IR spectrum can be quite complicated.

Infra-red spectrum?

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 15

The most common IR spectrum

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

Specific bonds respond to (absorb)


specific frequencies

Polar bonds

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 18

IR Spectroscopy Training 9
Page 10

Polar bonds display bands in the IR spectrum


* IR actives *

  bondmass
strength

C-H O-H N-H 3600 – 2700 cm-1


CC CN 2300 - 2000 cm-1
C=O C=N N=O 1900 - 1500 cm-1
C-C C-O C-N 1300 - 800 cm-1

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

The intensity of the bands depends on the magnitude


of the dipole moment

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

Table of Characteristic IR Absorptions

frequency, cm–1 bond functional group

3640–3610 (s, sh) O–H stretch, free hydroxyl alcohols, phenols

3500–3200 (s,b) O–H stretch, H–bonded alcohols, phenols


primary, secondary amines,
3400–3250 (m) N–H stretch
amides
3300–2500 (m) O–H stretch carboxylic acids

3330–3270 (n, s) –CC–H: C–H stretch alkynes (terminal)

3100–3000 (s) C–H stretch aromatics


3100–3000 (m) =C–H stretch alkenes
3000–2850 (m) C–H stretch alkanes
2830–2695 (m) H–C=O: C–H stretch aldehydes
2260–2210 (v) CN stretch nitriles
2260–2100 (w) –CC– stretch alkynes

m=medium, w=weak, s=strong, n=narrow, b=broad, sh=sharp


Source: University of Colorado at Boulder, Department of Chemistry and Biochemistry.
http://orgchem.colorado.edu/Spectroscopy/specttutor/irchart.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 23

1760–1665 (s C=O stretch carbonyls (general)


1760–1690 (s) C=O stretch carboxylic acids

1750–1735 (s) C=O stretch esters, saturated aliphatic

1740–1720 (s) C=O stretch aldehydes, saturated aliphatic

1730–1715 (s) C=O stretch alpha,beta–unsaturated esters

1715 (s) C=O stretch ketones, saturated aliphatic

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

1335–1250 (s) C–N stretch aromatic amines


alcohols, carboxylic acids, esters,
1320–1000 (s) C–O stretch
ethers
1300–1150 (m) C–H wag (–CH2X) alkyl halides
1300–1150 (m) C–H wag (–CH2X) alkyl halides
1250–1020 (m) C–N stretch aliphatic amines
1000–650 (s) =C–H bend alkenes
950–910 (m) O–H bend carboxylic acids

910–665 (s, b) N–H wag primary, secondary amines

900–675 (s) C–H "oop" aromatics


850–550 (m) C–Cl stretch alkyl halides
725–720 (m) C–H rock alkanes

700–610 (b, s) –CC–H: C–H bend Alkynes

690–515 (m) C–Br stretch alkyl halides


Source: University of Colorado at Boulder, Department of Chemistry and Biochemistry.
http://orgchem.colorado.edu/Spectroscopy/specttutor/irchart.html
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 25

Each molecule has a unique IR spectrum.

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

Examples of FTIR spectrum : Known compounds


O
CH 3-C H2C H2 -C-H

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

Identification of an organic compound


1. Examine the group frequency region
What functional groups are most likely present ?

2. The fingerprint region (1200 to 600 cm -1)


- impossible to complete interpretation because of the
complexity of the spectra (seldom possible)
- particularly useful for comparing with a spectrum of an
authentic sample.

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 33

An IR spectrum is used to identify functional


groups that are present (or absent).

Cannot conclusively identify a structure by


IR alone unless an IR spectrum of an
authentic (known) sample of the compound
is available.

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 34

IR Spectroscopy Training 17
Page 18

Alkane

- Finger print region


- compare with authentic sample

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

- Finger print region


- compare with authentic sample
IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 37

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 38

IR Spectroscopy Training 19
Page 20

What functional groups are present ?

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 39

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 40

IR Spectroscopy Training 20
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IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 41

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 42

IR Spectroscopy Training 21
Page 22

Computer Search System

Virtually all infrared instrument manufactures now offer


computer search systems to assist chemist in identifying
compounds from stored infrared spectral data.

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 43

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 44

IR Spectroscopy Training 22
Page 23

Quantitative Applications

• the characteristic band (specific wave number)


• calibration curve

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

The dispersive Infrared Spectrometer : Dispersive IR


Monochromater = monochromatic IR light

Fourier transform infrared spectrometer : FTIR


Interferometer = multi-chromatic light

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 46

IR Spectroscopy Training 23
Page 24

The dispersive Infrared Spectrometer : Dispersive IR

Source: http://www.chemicool.com/definition/fourier_transform_infrared_spectrometer_ftir.htm

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 47

IR-spectrometer Continuous Wave

Source : K. Gable, Department of Chemistry, Oregon State University


http://chemistry.oregonstate.edu/courses/ch361-464/ch362/irinstrs.htm

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 48

IR Spectroscopy Training 24
Page 25

Fourier transform infrared spectrometer : FTIR

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

Polystyrene Reference Materials

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.

Sodium chloride window (NaCl) is most commonly employed

(Potassium bromide, Potassium chloride, Cesium iodide)

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)

should be in the range of 0.2% to 1%.

IR Spectroscopy Training
Asst.Prof.Dr. Vanida Chairgulprasert 55

•Nujol mulls
a small drop of mineral oil (nujol), KBr plate

Nujol by itself shows a characteristic spectrum!

• 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

IR solution Cell (Quantitative analysis)

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

Solid and Powder sample


Organic and Inorganic compounds

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

- Organic solvent - Metal complex


- Ingredients in cosmetic - Pharmaceutical
- Food and Diary product - Drinking water
- Azo dye - Catalyst
- Oil : Engine oil, Used oil, Insulating oil
- Edible Oil : Fat, Lipid
- Paint

Transmission Technique

Transmission is the basic and popular technique for


analyzing samples in FT-IR spectroscopy

IR light sample
detector

It can be used in many different form such as liquid,


solid & gas
6
Page 34

Transmission: Liquid Sample


Liquid film : - is the simplest method
- sample (1-2 drops) is pressed between two
IR-transparent windows (sandwich)
- great viscosity such as oil

4 volatile, scentless
4 quantitative application

Transmission: Solid sample

Magnetic film holder :


- is
i the
th simplest
i l t accessory ffor polymer
l fil
film
- a very thin film is placed over magnetic holder &
held in place with a magnetic rubber strip

8
Page 35

Transmission KBr-pellet :

-sample is ground into a find powder in a mortar and


p
pestle
-dry KBr (or other alkaline halide) powder, then added
and mixture ground further
- pressed it to from pellet

Reflectance Technique

sample

IR light
detector

There are especially samples that are difficultly


examined
by transmission technique

Used for most samples with the exception of gases 10


Page 36

1) Attenuated Total Reflectance (ATR)


If light impinges on a boundary separating two
media, the path of the light can be described by
Snell’s Law.
(Medium 2)

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)

sample is placed on crystal θ2 = 90°


θc (critical angle) = θ1

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

sample is placed on crystal

- some of IR beam is absorbed by sample

12
Page 37

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

2) Diffuse Reflectance Accessory

rough surface solid, soil, cloth, coal


15

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
Page 40

- Click “OK” to next page Æ Workplace

19

OPUS workplace

20
Page 41

3. Click “Advance measurement” icon

44. Click
Cli k “L
“Load”
d” tto choose
h
technique

21

5. Choose technique such as “MIR_ATR.XPM”


or “MIR_TR.XPM”, then click Open

22
Page 42

6. Click “Check Signal” and record Amplitude

Click “Save Peak Position

23

7. Back to “Advanced”

24
Page 43

8. Choose your folder to save IR data, click OK

25

9. Set parameter in “Advanced”

26
Page 44

27

10. Click “Basic” and type sample name (Sample


description) then click Background single channel

28
Page 45

11. Analyst blank or nothing (air)

29

- Wait to finish scan

30
Page 46

12. Put sample

31

13. Click “Sample Single Channel” to analyst sample

- Sample data was


automatic save 32
Page 47

14. Click “Baseline correction” to take it straight

33

15. Click “Scale” to take full scale

34
Page 48

16. Interferogram will show, click “Smooth” if would


like to take smooth

35

36
Page 49

- Add “Annotation”

37

- Add “Annotation”

38
Page 50

- Peak picking

39

- Peak picking

40
Page 51

17. Import data by right click on frame, click “Copy”

41

- Paste interferogram in excel

42
Page 52

- Right click at sample name, choose Show Parameter

43

- Click at “TR” and right click to choose Copy to Clipboard

44
Page 53

- Paste data in excel

45

- Click save

46
Page 54

Other function
47

Manipulation : AB ↔ TR conversion
90
80
70
mittance [%]
60
Transm
50 40
30
20

4000 3500 3000 2500 2000 1500 1000 500

AB = - log (TR)
Wavenumber cm-1
0.7
0.6 0.5

Benefit of AB
AB--spectra
spectra::
Absorbance Units

peak intensity is proportional


0.4

to concentration
0.3 0.2
0.1

48
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber cm-1
Page 55

Manipulation : Baseline Correction

Before
Baseline Correction

49

Manipulation: Straight line generation

50
Page 56

Manipulation: Cut

Cut out range spectrum


Original spectrum

51

Evaluation : Spectrum search

52
Page 57

Evaluation : Spectrum search

Unknown
Library

Unknown Drug
Library

53

Evaluation : Create own library

54
Page 58

Evaluation : Library Browser


Spectrum list

Structure Information

Spectrum

55

Evaluation : Quantitative

56
Page 59

Print

‡ Quick Print
Prints current content of spectrum
window
d without
th t preview

‡ Print Spectra
Print spectra via menue

High measurment: Evaluate Æ Integration


‡ Change to Absorbance
‡ Click: Evaluate Æ Integration
‡ Click Icon Æ click “Setup Method“
‡ Click type “K“ (Single peak)
‡ Label
‡ Interaction
‡ If more than one, click
‡ Store method
‡Click “INTEG” Æ Show Report
‡ If it is multi peak (crack head) Æ Type R
‡ Click right grey box -> Zoom IR
‡Report Æ Append (don’t save on old data) 58
Page 60

Take out the logo:


‡ Click “Print” menu

‡ Click: Open Layout


‡ Choose file “defaultx.PLE”
‡Right Click >> Choose file “Properties”
Item Limits
‡ Check >> Show Bruker Logo 59

‡ Save >> Close Windows

Guidance FTIR Using

60
Page 61

Guidance FTIR using


‡ Avoid looking laser. This may cause damage to the
y
eyes.
‡ Keep water away from the instrument.
‡ Do not place objects on the cooling of the light
source.
‡ The optimum temperature is 18-30 C and humidity
less than 70 in work time.
‡ Replace the Moisture Absorber regularly.
‡
61

Thank for your


attention.

62
Page 62

Workshop
Operator name : ….…………………………….……..… Code ………….………
Workshop 1 Preparation of sample
- Prepare unknown A and B powder by press with KBr powder

Workshop 2 Analyst unknown A - E


- A and B powder by press with KBr powder by transmission
- C and D 0.5 - 1 drop between KBr pellet by transmission
- A, B and E by ATR

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
*****************************************
Page 63

Installation of
OPUS Program
1

Insert CD program >> Right click at “Setup.exe” icon


choose “Run as administrator”

2
Page 64

Program will run several second, Use “Next Technology”

4
Page 65

Use “Next Technology”

Use “Next Technology”

6
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Use “Next Technology”

Click “Install” and wait foe several minute

8
Page 67

Finish>> Happy ending

Happy Ending ^_^

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