كيمياء تحليلية كتب FTIR -Fourier Transform Infrared Spectrometry

المصدر: كتب FTIR -Fourier Transform Infrared Spectrometry
في منتدى : قسم الكيمياء

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كتاب​

Fourier Transform Infrared Spectrometry​

By Peter R. Griffiths, James A. De Haseth​

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Fourier Transform Infrared Spectroscopy (FTIR) is a powerful tool for identifying types of chemical bonds in a molecule by producing an infrared absorption spectrum that is like a molecular "fingerprint".

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FTIR - Introduction

FTIR is most useful for identifying chemicals that are either organic or inorganic. It can be utilized to quantitate some components of an unknown mixture. It can be applied to the analysis of solids, liquids, and gasses. The term Fourier Transform Infrared Spectroscopy (FTIR) refers to a fairly recent development in the manner in which the data is collected and converted from an interference pattern to a spectrum. Today's FTIR instruments are computerized which makes them faster and more sensitive than the older

dispersive instruments.​

Qualitative Analysis​

FTIR can be used to identify chemicals from spills, paints, polymers, coatings, drugs, and contaminants. FTIR is perhaps the most powerful tool for ​

identifying types of chemical bonds (functional groups). The wavelength of light absorbed is characteristic of the chemical bond as can be seen in this annotated spectrum.

By interpreting the infrared absorption spectrum, the chemical bonds in a molecule can be determined. FTIR spectra of pure compounds are generally so unique that they are like a molecular "fingerprint". While organic compounds have very rich, detailed spectra, inorganic compounds are usually much simpler. For most common materials, the spectrum of an unknown can be identified by comparison to a library of known compounds. WCAS has several infrared spectral libraries including on-line computer libraries. To identify less common materials, IR will need to be combined with nuclear magnetic resonance, mass spectrometry, emission spectroscopy, X-ray diffraction, and/or other techniques. ​

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Quantitative Analysis​

Because the strength of the absorption is proportional to the concentration, FTIR can be used for some quantitative analyses. Usually these are rather simple types of tests in the concentration range of a few ppm up to the percent level. For example, EPA test methods 418.1 and 413.2 measure the C-H absorption for either petroleum or total hydrocarbons. The amount of silica trapped on an industrial hygiene filter is determined by FTIR using NIOSH method 7602.
Physical Principles​

Molecular bonds vibrate at various frequencies depending on the elements and the type of bonds. For any given bond, there are several specific ​

frequencies at which it can vibrate. According to quantum mechanics, these frequencies correspond to the ground state (lowest frequency) and several excited states (higher frequencies). One way to cause the frequency of a molecular vibration to increase is to excite the bond by having it absorb light energy. For any given transition between two states the light energy (determined by the wavelength) must exactly equal the difference in the energy between the two states [usually ground state (E0) and the first excited state (E1)].

The energy corresponding to these transitions between molecular vibrational states is generally 1-10 kilocalories/mole which corresponds to the infrared portion of the electromagnetic spectrum.​

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Difference in
Energy States

=

Energy of
Light Absorbed

E1 - E0

=

h c / lWhere h=Planks constantc=speed of light, andl=the wavelength of light.
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Sample Preparation​

Samples for FTIR can be prepared in a number of ways. For liquid samples, the easiest is to place one drop of sample between two plates of sodium chloride (salt). Salt is transparent to infrared light. The drop forms a thin film between the plates. Solid samples can be milled with potassium bromide (KBr) to form a very fine powder. This powder is then compressed into a thin pellet which can be analyzed. KBr is also transparent in the IR. Alternatively, solid samples can be dissolved in a solvent such as methylene chloride, and the solution placed onto a single salt plate. The solvent is then evaporated off, leaving a thin film of the original material on the plate. This is called a cast film, and is frequently used for polymer identification.
Solutions can also be analyzed in a liquid cell. This is a small container made from NaCl (or other IR-transparent material) which can be filled with liquid, such as the extract for EPA 418.1 analysis. This creates a longer path length for the sample, which leads to increased sensitivity. Sampling methods include making a mull of a powder with a hydrocarbon oil (Nujol) or pyrolyzing insoluble polymers and using the distilled pyrolyzate to cast a film. Matrials can be placed in an Attenuated Total Reflectance (ATR) cell and gases in gas cells. ​

FTIR-Microscope​

For small samples or samples with surface contamination visible to the naked eye, a microscope attachment can be used to obtain reflectance or transmitance spectra on particles as small as 20 microns.​

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FTIR-Microscope​

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كتاب​

Liquid Chromatography FTIR Microspectroscopy Microwave Assisted Synthesis ​

(Advances in Polymer Science)​

By R. Bhargava, D. Bogdal, T. Chang, D. Hunkeler, J.L. Koenig, T. Macko, P. Penczek, J. Pielichowski, A. Prociak, S.-Q. Wang​

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كتاب​

Fourier Transforms in Spectroscopy​

Jyrki Kauppinen, Jari Partanen​

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Liquid Chromatography / FTIR Microspectroscopy / Microwave Assisted Synthesis

 

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