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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 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
Page 8
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
Page 11
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
Page 12
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.
Page 13
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
Page 18
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
Page 19
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
Page 20
IR Spectroscopy Training 21
IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 41
IR Spectroscopy Training Asst.Prof.Dr. Vanida Chairgulprasert 42
Page 21
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
Page 22
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)
Page 27
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
Page 33
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
Page 34
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
Page 35
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
Page 36
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
Page 37
2) Diffuse Reflectance Accessory
rough surface solid, soil, cloth, coal15
Using Bruker Tensor27 FTIR
16
Page 38
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
Page 39
- Click “OK” to next page Workplace
19
OPUS workplace
20
Page 40
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
Page 41
6. Click “Check Signal” and record Amplitude
Click “Save Peak Position
23
7. Back to “Advanced”
24
Page 42
8. Choose your folder to save IR data, click OK
25
9. Set parameter in “Advanced”
26
Page 43
27
10. Click “Basic” and type sample name (Sample description) then click Background single channel
28
Page 44
11. Analyst blank or nothing (air)
29
- Wait to finish scan
30
Page 45
12. Put sample
31
13. Click “Sample Single Channel” to analyst sample
- Sample data was automatic save 32
Page 46
14. Click “Baseline correction” to take it straight
33
15. Click “Scale” to take full scale
34
Page 47
16. Interferogram will show, click “Smooth” if would like to take smooth
35
36
Page 48
- Add “Annotation”
37
- Add “Annotation”
38
Page 49
- Peak picking
39
- Peak picking
40
Page 50
17. Import data by right click on frame, click “Copy”
41
- Paste interferogram in excel
42
Page 51
- Right click at sample name, choose Show Parameter
43
- Click at “TR” and right click to choose Copy to Clipboard
44
Page 52
- Paste data in excel
45
- Click save
46
Page 53
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
Page 54
Manipulation : Baseline Correction
Before
Baseline Correction
49
Manipulation: Straight line generation
50
Page 55
Manipulation: Cut
Cut out range spectrum
Original spectrum
51
Evaluation : Spectrum search
52
Page 56
Evaluation : Spectrum search
Unknown DrugLibrary
Unknown Library
53
Evaluation : Create own library
54
Page 57
Evaluation : Library Browser
Spectrum list
StructureInformation
Spectrum
55
Evaluation : Quantitative
56
Page 58
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
Page 59
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
Page 60
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.
62
Page 61
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 =
Page 62
Installation ofInstallation of
1
OPUS ProgramOPUS Program
Insert CD program >> Right click at “Setup.exe” icon
choose “Run as administrator”
2
Page 63
Program will run several second, Use “Next Technology”
3
4
Page 64
Use “Next Technology”
5
Use “Next Technology”
6
Page 65
Use “Next Technology”
7
Click “Install” and wait foe several minute
8
Page 66
Finish>> Happy ending
Happy Ending ^_^
9
Page 67
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