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

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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

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

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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

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

No Name - Surname Year/Degree/Major Group Signature 1 Miss Jennifer Osamede 1st year, Master's degree, Food Science and

Nutrition 1

2 Mr.Alam Surya Wijaya 1st year, Master's degree, Sustainable Energy Management

2

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 Fathurrohman

1st year, Doctor's degree, Polymer Technology 1

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 16 Mr.Nitipon Jeni 4th 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

IR Spectroscopy Training 1

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 1

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 2

Page 1

IR Spectroscopy Training 2

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 3

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 4

Graphics source: Wade, Jr., L.G. Organic Chemistry, 5th ed. Pearson Education Inc., 2003

Electromagnetic Radiation

Page 2

IR Spectroscopy Training 3

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

Infra = beyond

Infrared = beyond red region

Beyond the Visible

Infrared radiation = Thermal radiation

Courtesy NASA/JPL-Caltech, Linda Hermans-Killam

Infrared radiation

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 6

Dicovery of Infrared Radiation

Source: NASA

Page 3

IR Spectroscopy Training 4

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

= 1

Wave number,

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

Infrared light2.5-25 m

4000-500 cm-1

= 10000(m)

Wave number(cm-1),

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

What is Infrared Spectroscopy?

The Mid IR range

= 2-50 m

= 4000-500 cm-1

Infrared Spectroscopy is the analysis of infrared light

interacting with a molecule

Page 4

IR Spectroscopy Training 5

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 9

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 10

Chemicalsample

IRsource

Transmitted light Detector

detects the transmitted frequencies,

reveals the values of the absorbed frequencies.

absorb specific frequencies* Chemical Bonds *

4000-500 cm-1

Page 5

IR Spectroscopy Training 6

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

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 12

2 Different TypesFundamental vibration

Infrared radiation stimulates molecular vibrations.

Stretching vibration : change of bond length

Bending vibration : change of bond length

Page 6

IR Spectroscopy Training 7

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 13

Sources :© http://namrataheda.blogspot.com/2014/01/spectrophotometry-ir-spectroscopy.html

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 14

Bending Vibrations

Sources :© http://namrataheda.blogspot.com/2014/01/spectrophotometry-ir-spectroscopy.html

Page 7

IR Spectroscopy Training 8

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

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 16

The most common IR spectrum

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IR Spectroscopy Training 9

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 17

Absorbance IR

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

Specific bonds respond to (absorb) specific frequencies

Polar bonds

Page 9

IR Spectroscopy Training 10

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 19

Polar bonds display bands in the IR spectrum * IR actives *

bond strengthmass

C-H O-H N-H 3600 – 2700 cm-1

CC CN 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 20

Graphics source: Wade, Jr., L.G. Organic Chemistry, 5th ed. Pearson Education Inc., 2003

IR absorption range

Page 10

IR Spectroscopy Training 11

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 21

The intensity of the bands depends on the magnitude of the dipole moment

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 22

broad

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IR Spectroscopy Training 12

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 23

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

3400–3250 (m) N–H stretchprimary, secondary amines, amides

3300–2500 (m) O–H stretch carboxylic acids

3330–3270 (n, s) –CC–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) CN stretch nitriles

2260–2100 (w) –CC– stretch alkynes

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

Table of Characteristic IR Absorptions

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 24

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

1710–1665 (s) C=O stretchalpha,beta–unsaturated aldehydes, 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) N–O symmetric stretch nitro compounds

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IR Spectroscopy Training 13

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 25

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

1320–1000 (s) C–O stretchalcohols, carboxylic acids, esters, 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) –CC–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 26

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.

Each molecule has a unique IR spectrum.

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IR Spectroscopy Training 14

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 27

Examples of FTIR spectrum : Known compounds

Cl-CH2-CHCH3

CH3

CH3CH2CH2CH2CH2-C-O-H

O

O

C-O-CH2CH3

CH3-CH2-O-H

CH3-CH2CH2-C-H

O

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 28

Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/aldehydesir.html

Page 14

IR Spectroscopy Training 15

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 29

Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/carbacidsir.html

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 30

Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/estersir.html

Page 15

IR Spectroscopy Training 16

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 31

Source: http://orgchem.colorado.edu/Spectroscopy/irtutor/alcoholsir.html

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 32

Source:http://orgchem.colorado.edu/Spectroscopy/irtutor/ketonesir.html

Page 16

IR Spectroscopy Training 17

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

Identification of an organic compound1. 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 34

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.

Page 17

IR Spectroscopy Training 18

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 35

Alkane

- Finger print region- compare with authentic sample

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 36

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IR Spectroscopy Training 19

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 37

OHOH

OH

- Finger print region- compare with authentic sample

AlcoholC4H9OH

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

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IR Spectroscopy Training 20

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

What functional groups are present ?

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

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IR Spectroscopy Training 21

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

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

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IR Spectroscopy Training 22

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

Computer Search System

Virtually all infrared instrument manufactures now offercomputer search systems to assist chemist in identifyingcompounds from stored infrared spectral data.

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

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IR Spectroscopy Training 23

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 45

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

• the characteristic band (specific wave number)• calibration curve

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

Infrared Spectrometer

The dispersive Infrared Spectrometer : Dispersive IR

Interferometer = multi-chromatic light

Monochromater = monochromatic IR light

Fourier transform infrared spectrometer : FTIR

Page 23

IR Spectroscopy Training 24

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

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 48

IR-spectrometer Continuous Wave

Source : K. Gable, Department of Chemistry, Oregon State University http://chemistry.oregonstate.edu/courses/ch361-464/ch362/irinstrs.htm

Page 24

IR Spectroscopy Training 25

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 49

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 50

Preparation of sample

• Gas• Liquid• Solid

Polystyrene Reference Materials

Page 25

IR Spectroscopy Training 26

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 51

Gas sample

- gas cell

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 52

Liquid samples

• Solution

using a liquid cell

• 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

Page 26

IR Spectroscopy Training 27

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 53

The solvent must not affect the material, (sodium chloride, the cell)

IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 54

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)

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IR Spectroscopy Training 28

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

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 56

•Nujol mulls

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

Nujol by itself shows a characteristic spectrum!

• solution

• thin film

Page 28

IR Spectroscopy Training 29

Polystyrene

TetrachlorideCarbon

CCl Cl

Cl

Cl

no C-H!

C-Cl stretch

Page 29

IR Spectroscopy Training 30

59

IR solution Cell (Quantitative analysis)

Page 30

Part 2

Using and Maintenance of FTIR

(Bruker Tensor 27)

Using Bruker Tensor27 FTIRBruker Tensor27 FTIR

Pisipong MeunprasertdeeScientistScientist

Instrument CenterFaculty of Science and Technology 1

Sample PreparationSample Preparation

2

Page 31

Solid Solid and Powder sampleand Powder sample

Organic and Inorganic compounds

- Organic Powder - Metal complexg p- Ingredients in cosmetic - Pharmaceutical- Food and Diary product - Polymer - Azo dye - Catalyst- Packaging - Gemstone- Rubber- Rubber - Electronic

3

Gas sample

4

Page 32

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

5

Transmission Technique

Transmission is the basic and popular technique for analyzing samples in FT-IR spectroscopy

sampleIR lightdetector

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

6

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Transmission: Liquid SampleLiquid film : - is the simplest method

- sample (1-2 drops) is pressed between twoIR-transparent windows (sandwich)

volatile, scentlessquantitative application

- great viscosity such as oil

7

Transmission: Solid sample

Magnetic film holder :i th i l t f l fil- is the simplest accessory for polymer film

- a very thin film is placed over magnetic holder & held in place with a magnetic rubber strip

8

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Transmission KBr-pellet :

-sample is ground into a find powder in a mortar and pestlep-dry KBr (or other alkaline halide) powder, then added and mixture ground further- pressed it to from pellet

9

Reflectance Technique

sample

There are especially samples that are difficultly

IR light

detector

examinedby transmission technique

Used for most samples with the exception of gases 10

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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.

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

θ1 : incidence angleθ2 : refraction angle

η1 : refraction index of medium 1 (crystal)

η2 : refraction index of medium 2 (sample)

η1 • sinθ1 = η2 • sinθ2

θ1 : incidence angleθ2 : refraction angle

η1 : refraction index of medium 1 (crystal)

η2 : refraction index of medium 2 (sample)

(Medium 1)Crystal n1

Substance n2

ΘΘ Θ

Φ Φ

a) b) c) d)

sample is placed on crystal

The angle of incidence beam is higher than the critical angle of crystal

θ2 = 90°θc (critical angle) = θ1

θ2 = 90°θc (critical angle) = θ1

11

Sample

n2

Sample

ATR crystal

Θn1

2

Refraction indexn1 > n2

η1 > η2

sample is placed on crystal

ATR crystal

- some of IR beam is absorbed by sample

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 ofmeasured. It is used to analyze a wide variety of solid samples.

Specular Energy

Diffuse Energy

SAMPLE CUP

14

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2) Diffuse Reflectance Accessory

rough surface solid, soil, cloth, coal15

Using Bruker Tensor27 FTIR

16

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Turning on FTIR1. Turn on UPS and computer

17

Turning on HPLC2. Open “OPUS” software by clicking OPUS

icon, password is “OPUS” then click “Login”

18

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- Click “OK” to next page Workplace

19

OPUS workplace

20

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3. Click “Advance measurement” icon

4 Cli k “L d” t h 4. Click “Load” to choose technique

21

5. Choose technique such as “MIR_ATR.XPM” or “MIR_TR.XPM”, then click Open

22

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6. Click “Check Signal” and record Amplitude

Click “Save Peak Position

23

7. Back to “Advanced”

24

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

25

9. Set parameter in “Advanced”

26

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27

10. Click “Basic” and type sample name (Sample description) then click Background single channel

28

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11. Analyst blank or nothing (air)

29

- Wait to finish scan

30

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12. Put sample

31

13. Click “Sample Single Channel” to analyst sample

- Sample data was automatic save 32

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14. Click “Baseline correction” to take it straight

33

15. Click “Scale” to take full scale

34

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16. Interferogram will show, click “Smooth” if would like to take smooth

35

36

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- Add “Annotation”

37

- Add “Annotation”

38

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- Peak picking

39

- Peak picking

40

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

41

- Paste interferogram in excel

42

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- Right click at sample name, choose Show Parameter

43

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

44

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- Paste data in excel

45

- Click save

46

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Other functionOther function

47

6070

80

90

mitta

nce [

%]

Manipulation : AB ↔ TR conversion

AB = - log (TR)5001000150020002500300035004000

Wavenumber cm-1

2030

40

50

Tra

nsm

0.6

0.7

5001000150020002500300035004000

Wavenumber cm-1

0.1

0.2

0.3

0.4

0.5

Absorb

ance U

nits Benefit of Benefit of ABAB--spectraspectra::

peak intensity is proportional peak intensity is proportional

to concentration to concentration

48

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Manipulation : Baseline Correction

Before

Baseline Correction

49

Manipulation: Straight line generation

50

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Manipulation: Cut

Cut out range spectrum

Original spectrum

51

Evaluation : Spectrum search

52

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Evaluation : Spectrum search

Unknown DrugLibrary

Unknown Library

53

Evaluation : Create own library

54

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Evaluation : Library Browser

Spectrum list

StructureInformation

Spectrum

55

Evaluation : Quantitative

56

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Print

Quick PrintPrints current content of spectrum

d th twindow without preview

Print SpectraPrint spectra via menue

High measurment: Evaluate IntegrationChange to Absorbance

Click: Evaluate Integration

Click Icon click “Setup Method“Click type “K“ (Single peak)

Label

Interaction

If more than one, click

Store method

Click “INTEG” Show Report

If it is multi peak (crack head) Type RClick right grey box -> Zoom IR

Report Append (don’t save on old data)58

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Take out the logo:Click “Print” menu

Click: Open Layout

Choose file “defaultx.PLE”

Right Click >> Choose file “Properties”

Check >> Show Bruker Logo

Save >> Close Windows

Item Limits

59

Guidance FTIR Using

60

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Guidance FTIR using

Avoid looking laser. This may cause damage to the eyes. y

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 Thank for your attention.

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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 3. Ethylbenzoate 4. Eugenol 5. Glycerol 6. Palmitic acid 7. Polyethylene 8. Polypropylene 9. Polystyrene 10. Polyvinylchloride 11. Salicylic acid 12. Steroid 13. TritonX 14. Toluene

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

Answer A = B = C = D = E =

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Installation ofInstallation of

1

OPUS ProgramOPUS Program

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

choose “Run as administrator”

2

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Program will run several second, Use “Next Technology”

3

4

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Use “Next Technology”

5

Use “Next Technology”

6

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Use “Next Technology”

7

Click “Install” and wait foe several minute

8

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Finish>> Happy ending

Happy Ending ^_^

9

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