Study on KBr pellet preparation for FT-IR spectroscopy using hydraulic pellet press & Data Analysis

1. Study on KBr pellet preparation for FT-IR spectroscopy using hydraulic pellet press & Data Analysis MdRiazurRahman ID: 2019210009 College of Textiles Zhongyuan University of Technology Xinzheng, Zhengzhou, Henan, China Date: 2019,DEC-05

2. OUTLINE • General Information about FT-IR Spectroscopy • Instrumentation • Sample Preparation • Applications of FTIR • Data analysis.

3. What is Spectroscopy? spectrometer is an optical instrument used to measure properties of light over a specific portion of the electromagnetic spectrum. FTIR (Fourier Transform InfraRed) spectrometer is a obtains an infrared spectra by first collecting an interferogramof a sample signal using an interferometer, then performs a Fourier Transform on the interferogram to obtain the spectrum. An interferometer is an instrument that uses the technique of superimposing (interfering) two or more waves, to detect differences between them. The FTIR spectrometer uses a Michelson interferometer. Figure1 : interaction between matter and energy

4. Figure 2 : electromagneticspectrum

5. Why FT-IR spectroscopy? • Non-destructive technique • Good precision • No external calibration • High speed • Signal-Noise ratio • Mechanically simple • ernal calibration • High speed • Signal-Noise ratio Mechanically simple

6. What information can FT-IR provide? • Identify unknown material • Determine quality or consistency of sample • Determine amount of components in mixture

7. Apparatus & instruments1. Hydraulic press.2.mortar & pestle.3. polyester powder.4. cotton blended (60:40)% fibre.5. FT-IR tester.6. Dry kBr.

8. Sample Preparation • KBr Pellet Preparation or sample preparation the most important part for IR spectroscopy. Sample should be transparent to IR radiations so it allows the radiations to pass through them. So salts like KBr, NaCl, AgCl are used for mixing of sample in order to obtain the accurate IR spectrum of a sample with sharp peaks, good intensity with high resolution. • For powdered samples one of the way is to disperse it in Infrared Transparent medium such as Potassium Bromide (KBr) by pressing it into disc. • Firstly we cleaned all the parts of die with chloroform or lubricant spray or tissue thoroughly to get rid of any dirt and dry them with tissue • Clean the mortar and pestle with chloroform or acetone thoroughly to get rid of any dirt and dry them with tissue. • Transfer a speck of sample into the mortar.  Be careful of not adding too much sample which may cause over saturation. • Scoop out dry KBr(3:1) into the mortar. Grind  using the pestle. Continue for few minutes to get a homogenous mix. • Fix the pellet press together.  Insert the die into the cavity

9. .Transfer the ground sample mix into the cavity using a metal spatula. Make sure it’s evenly spread.  Depending on the thickness of pellet we want to achieve we put the amount of powder. Putting excess makes it more thick..Insert the bolt press and rotate into the cavity to distribute the particles. . Transfer the whole die set to the hydraulic pellet press and rotate the wheel to secure it tightly.. Close the valve of the hydraulic press.  Pull the level to put pressure until 20kpa pressure..To release the die first need to loosen the pressure,  then move up the upper wheel of the press and then take out the die. .Take out the bottom Plunger and place the die in the ejector.   Apply pressure to release the pellet from the die.

10. Working procedure of FT-IR1. The Source: Infrared energy is emitted from a glowing black-body source. This beam passes through an aperture which controls the amount of nergypresented to the sample (and, ultimately, to the detector). 2. The Interferometer: The beam enters the interferometer where the “spectral encoding” takes place. The resulting interferogram signal then exits the interferometer. 3. The Sample: The beam enters the sample compartment where it is transmittedthrough or reflected off of the surface of the sample, depending on the type of analysisbeing accomplished. This is where specific frequencies of energy, which are uniquelycharacteristic of the sample, are absorbed.

11. 3.DetectorsThe beam finally passes to the detector for final measurement. The detectors used are specially designed to measure the special interferogram signal.4.The Computered.Measured signal is digitized and sent to the computer where the Fourier transformation takes place. The final infrared spectrum is then presented to theuser for interpretation and any further manipulation.

12. TheSampleAnalysisProcess Figure : FTIR spectrometeranalysis process

13. Data analysis of Blended & polyester fibre

14. FTIR BENEFITSReal-time measurement results.• Simultaneous analysis of multiple gaseous compounds.• Measures a wide variety of volatile compounds (Inorganic and Organic).• Sensitivity from very low parts per million to high percent levels.• Provides a precise measurement method which requires no rigorous external calibration.• Speed. Measurements take only seconds

15. Applications of FT-IR • Pharmaceutical research • Forensic investigations • Polymer analysis • Lubricant formulation and fuel additives • Foods research • Quality assurance and control • Environmental and water quality analysis methods • Biochemical and biomedical research • coatings and surfactants

16. Thank You