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Attenuated Total Reflection Acknowledgments 24 Abbreviations and Acronyms 24 Fourier Transform Infrared Related Articles 24 Spectroscopy References 24 Georg Ramer and Bernhard Lendl Vienna University of Technology, Vienna, Austria Attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy is now the most widespread implementation of mid-infrared (MIR) spectroscopy. 1 Introduction 1 While the FTIR technique allows the fast and stable 1.1 Introduction to Attenuated Total collection of MIR spectra, the ATR technique allows Reflection Spectroscopy 1 mechanically stable, robust, and quick sampling. ATR- FTIR spectroscopy is routinely used in industrial and 1.2 History of ATR Spectroscopy 2 research laboratories. The ATR-FTIR technique finds 1.3 A Short Introduction to Mid-infrared application in, e.g. biology, medicine, forensics, process Fourier Transform Spectroscopy 3 analytical chemistry and organic chemistry. Even though 2 Theoretical Aspects of Attenuated Total ATR spectroscopy is often treated as a routine technique, Reflection Spectroscopy 5 it has several intricacies that users should be aware of to 2.1 Reflection, Total Reflection, and the avoid measurement errors and artifacts. Attenuated Total Reflection Signal 5 In this article, starting from the theoretical underpinnings 2.2 Influence of the Measurement of ATR spectroscopy, we aim to give novices in ATR- Parameters on the Attenuated Total FTIR spectroscopy the knowledge to successfully use this Reflection Signal 9 technique and to avoid common errors. The theoretical 3 Practical Aspects of Attenuated Total treatment of ATR spectroscopy is complemented by Reflection Spectroscopy 13 practical information about the routine and advanced uses 3.1 Materials 13 of ATR spectroscopy. Furthermore, the reader will find descriptions of future trends in ATR-FTIR and evanescent 3.2 Number of Reflections 13 wave spectroscopy. Finally, a list of literature for further 3.3 Sample Preparation and Measurement reading and a list of vendors of ATR accessories and Protocols 14 their product lines are given to facilitate using the ATR 3.4 Angle of Incidence 16 technique. 3.5 Surface Modification 17 4 Differences Between Attenuated Total Reflection Spectroscopy and Transmission 1 INTRODUCTION Spectroscopy 18 4.1 Comparison of Attenuated Total 1.1 Introduction to Attenuated Total Reflection Reflection Spectra and Transmission Spectroscopy Spectra 18 4.2 Sample Preparation 19 The attenuated total reflection (ATR) technique is the most frequently used sampling technique for infrared (IR) 5 Applications 19 spectroscopy.(1) IR light traveling in an optically denser 5.1 Biological and Medical Samples 19 medium is totally reflected at the interface to an optically 5.2 Process Analytical Chemistry 20 rarer medium. Although the light rays as such do not 5.3 Microscopy 20 propagate into the optically rarer medium, an evanescent 5.4 Depth Profiling 21 field forms there. Through this evanescent field, the light 6 Vendors 22 can interact with samples placed at the interface, making absorption measurements possible. 7 Further Reading 22 The ATR technique usually needs hardly any sample 8 Future Trends 23 preparation. It allows quick and robust measurements 8.1 Hand-held Attenuated Total Reflection of solid as well as of liquid samples, including pastes Instruments 23 and samples otherwise difficult to handle. Therefore, 8.2 Waveguide Sensors 23 since its invention in the 1960s, the ATR technique has Encyclopedia of Analytical Chemistry, Online © 2006–2013 John Wiley & Sons, Ltd. This article is © 2013 John Wiley & Sons, Ltd. This article was published in the Encyclopedia of Analytical Chemistry in 2013 by John Wiley & Sons, Ltd. DOI: 10.1002/9780470027318.a9287 2 INFRARED SPECTROSCOPY gradually replaced other sampling methods for solid and Several great minds have investigated total reflection over liquid samples for many applications of IR spectroscopy. the course of the following centuries. E. Hall notes, at the In principle, ATR spectroscopy can also be applied to beginning of The penetration of totally reflected light into the measurement of gases; however, due to the short the rarer medium(3): interaction length of the evanescent field with the sample, gas measurements are of low sensitivity. The problem [attenuated total reflection] was both This article aims at giving a practical and theoret- experimentally and theoretically studied by Fresnel, and more or less treated by Verdet, Young, Huygens, Biot, ical introduction to ATR spectroscopy. An overview of Babinet, Billet, Stokes, and other. The first reliable common applications and designs of ATR accessories quantitative work was published by G. Quincke in 1886. for MIR spectroscopy is given. Practical aspects of ATR spectroscopy, including sample preparation, sampling, and common errors are explained. The current applica- Total reflection was, however, first used in the twentieth tions of the ATR technique in a wide range of fields are century for absorption measurements.(4) In 1926, C.V. reviewed. To make it easy for the reader to start using the Raman,(5) who went on to discover the Raman effect ATR technique, a list of vendors of ATR accessories and a few years later, reexamined the principles of total their respective products is given at the end of the article. reflection. In the early 1930s, the principles of ATR As this article is introductory in nature, several sources absorption measurements were worked out by Taylor recommended for further reading are provided. and Glover,(6) Taylor and Durfee,(7) and Taylor and King(8) and employed to determine the birefringence of layers of organic acids. In their work, the principles of 1.2 History of ATR Spectroscopy ATR spectroscopy are laid out correctly and employed to Isaac Newton famously remarked: ‘If I have seen farther measure absorption spectra, to study surface layers, and (4) it is by standing on the shoulders of giants’. It is therefore to determine refractive indices. fitting that we start this short overview over the history of The next major steps in the development of the the ATR technique and its giants with his work entitled ATR technique happened in quick succession in the late Opticks: Or, A Treatise of the Reflections, Refractions, 1950s and the early 1960s. At the Fourth International Inflections and Colours of Light.(2) Starting with Opticks Conference on Molecular Spectroscopy (Bologna, 1959), has another significance as well: N.J. Harrick, one of the Jacques Fahrenfort of the Royal Dutch Shell Laboratories (4) inventors of the ATR technique, begins his fundamental presented a paper on the ATR technique. In December work on ATR spectroscopy entitled Internal Reflection of the same year, at the Second International Conference Spectroscopy by quoting a passage from Opticks: Or, A on Semiconductor Surfaces (Maryland), Nicolas James Treatise of the Reflections, Refractions, Inflections and Harrick of the Philips Laboratories suggested in a Colours of Light (book III, part 1, query 29), where comment on a talk about ‘Infrared Methods Applied Newton describes total reflection of light at the interface to Surface Phenomena’ (R.P. Eischens) to use ATR between a glass prism and air: measurements to study molecules adsorbed on the surface.(4) Harrick had been studying internal reflection The Rays of Light in going out of the Glass into a Vacuum, and total internal reflection in semiconductors before.(9) are bent towards the Glass; and if they fall too obliquely At this point, however, he presumably did know neither on the Vacuum, they are bent backwards into the Glass, of the works of Taylor et al. nor of Fahrenfort’s and totally reflected;[...] talk.(4) In 1961, ‘Attenuated total reflection’(84) by Fahren- fort was published in Spectrochimica Acta.Inthis and also notes, that light that should be totally reflected work, Fahrenfort introduced the theoretical underpin- will pass into a second optically dense material when the nings of ATR spectroscopy. He showed two different interfaces of both objects are placed close enough to each experimental setups using either a hemicylindric KRS-5 other, even though they do not touch: (Thallium Bromoiodide) or AgCl element to collect ATR And this is still more evident by laying together two Prisms spectra using a focused or a collimated beam. In the of Glass, or two Object-glasses of very long Telescopes, same paper, Fahrenfort also showed the possibility for the one plane, the other a little convex, and so compressing quantification in ATR spectra using Beer’s law and its them that they do not fully touch, nor are too far asunder. limitations. Finally, he suggested using this new technique For the Light which falls upon the farther Surface of the to determine refractive index spectra of samples. first Glass where the Interval between the Glasses is not above the ten hundred thousandth Part of an Inch, will In 1967, Harrick published Internal Reflection Spectro- (10) go through that Surface, and through the Air or Vacuum scopy, which included a thorough treatment of the between the Glasses, and enter into the second Glass,[...] theoretical foundations and practical considerations Encyclopedia of Analytical Chemistry, Online © 2006–2013 John Wiley & Sons, Ltd. This article is © 2013 John Wiley & Sons, Ltd. This article was published in the Encyclopedia of Analytical Chemistry in 2013 by John Wiley & Sons, Ltd. DOI: 10.1002/9780470027318.a9287 ATTENUATED TOTAL REFLECTION FOURIER TRANSFORM INFRARED SPECTROSCOPY 3 400 to determine depth profiles of thin layers and to determine the orientation of molecules adsorbed on a surface. 300 200 1.3 A Short Introduction to Mid-infrared Fourier Transform Spectroscopy 100 1.3.1 The Mid-infrared Region of the Electromagnetic Number of publications 0 1960 1980 2000 Spectrum Year ATR spectroscopy is most often used in the MIR region Figure 1 Plot of the number of publications on ATR of the electromagnetic spectrum. The MIR region is spectroscopy over the past 50 years. Data were collected usually defined as the wavenumber ν˜ region from 4000 to from Scopus.
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