The DOI matches its Crossref record; 38 of the 38 references it cites were found in a registry or an index.
In Situ Time-Dependent Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy of a Powdered Specimen in a Controlled Atmosphere: Monitoring Sorption and Desorption of Water Vapor
Abstract
Attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy is a powerful instrumental method of chemical analysis of solids and liquids. The majority of published studies by in situ ATR FT-IR spectroscopy describe analysis of homogeneous samples, such as liquid solutions under circulation, or films on the ATR crystal that react with the gas of interest. The in situ ATR FT-IR spectroscopic studies of specimens in physical shape of crystals or powder that react with a gas or vapor are rare. This work describes a modification of in situ time-dependent ATR FT-IR spectroscopy to allow monitoring heterogeneous reaction "solid-gas" of powder in controlled atmosphere and in the time domain. Also, we describe a new facile gas flow chamber attachment to ATR FT-IR spectrometer which allows creating controlled atmosphere surrounding the specimen on the ATR crystal. Additionally, the capabilities of the described in situ time-dependent ATR FT-IR spectroscopy experiment in controlled atmosphere are enhanced by the sensor for in situ time-dependent monitoring the relative humidity (RH) of air surrounding the specimen. The operation of the setup for in situ time-dependent ATR FT-IR spectroscopy in controlled atmosphere is demonstrated by monitoring reaction of gradual desorption of water vapor from color-indicating molecular sieves under controlled low air humidity. Further, the described spectroscopic method and apparatus is applied to monitor the reverse process, namely sorption of water vapor by color-indicating molecular sieves under controlled elevated air humidity. Water molecules are found to reversibly interact with two distinct sorption sites in the sorbent: the Si-O backbone and the color-indicating Co(II) centers. The reported variant of in situ time-dependent ATR FT-IR spectroscopy in controlled atmosphere is powerful, yet facile and straightforward. It is promising for mechanistic, in situ studies of sorption, desorption, chemosensing, heterogeneous catalysis and photocatalysis, and analysis of chemical kinetics of various "solid-gas" reactions.
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“Two classes of such devices are flow-through ATR cells, where the sample stream flows through the measurement chamber of the FTIR spectrometer [230], and autoclavable optical fibres with ATR crystals at the tip [231].”
From Multi-Sensing Monitoring of the Microalgae Biomass Cultivation Systems for Biofuels and Added Value Products Synthesis—Challenges and Opportunities (2025) · cites this paper as [230]
Citations
Cites
In-Situ ATR-FTIR Spectroscopic Study of Electro-oxidation of Methanol and Adsorbed CO at Pt−Ru Alloy
Yajima, T., Uchida, H., & Watanabe, M. (2004) · The Journal of Physical Chemistry B · doi:10.1021/jp037215q · Cited by 348
Swellable, Water- and Acid-Tolerant Polymer Sponges for Chemoselective Carbon Dioxide Capture
Woodward, R. T., Stevens, L. A., Dawson, R., Vijayaraghavan, M., Hasell, T., Silverwood, I. P., Ewing, A. V., Ratvijitvech, T., Exley, J., Chong, S. Y.-L., et al. (2014) · Journal of the American Chemical Society · doi:10.1021/ja5031968 · Cited by 240
The Structures of Synthetic Molecular Sieves
Broussard, L., & Shoemaker, D. P. (1960) · Journal of the American Chemical Society · doi:10.1021/ja01490a007 · Cited by 238
In Situ ATR and DRIFTS Studies of the Nature of Adsorbed CO 2 on Tetraethylenepentamine Films
Wilfong, W. C., Srikanth, C. S., & Chuang, S. S. C. (2014) · ACS Applied Materials & Interfaces · doi:10.1021/am5031006 · Cited by 231
In Situ FT-IR/ATR Spectroelectrochemistry of Prussian Blue in the Solid State
Kulesza, P. J., Malik, M. A., Deńca, A., & Strojek, J. W. (1996) · Analytical Chemistry · doi:10.1021/ac950380k · Cited by 165
Blum, M., & John, H. (2011) · Drug Testing and Analysis · doi:10.1002/dta.374 · Cited by 105
Flichy, N. M. B., Kazarian, S. G., Lawrence, C. J., & Briscoe, B. J. (2001) · The Journal of Physical Chemistry B · doi:10.1021/jp012597q · Cited by 101
Wang, Y., & Yang, R. T. (2019) · ACS Sustainable Chemistry & Engineering · doi:10.1021/acssuschemeng.8b05339 · Cited by 72
Schuttlefield, J. D., Al-Hosney, H. A., Zachariah, A., & Grassian, V. H. (2007) · Applied Spectroscopy · doi:10.1366/000370207780220868 · Cited by 71
Chen, J., Sankar, G., Thomas, J. M., Xu, R., Greaves, G. N., & Waller, D. (1992) · Chemistry of Materials · doi:10.1021/cm00024a045 · Cited by 63
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Dębowski, M., Kazimierowicz, J., & Zieliński, M. (2025) · Applied Sciences · doi:10.3390/app15137324 · Cited by 30
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Self-citationUllah, S., McKee, M. L., & Samokhvalov, A. (2023) · Physical Chemistry Chemical Physics · doi:10.1039/d3cp03779g · Cited by 5
Self-citationLuo, Z., Hu, W., Pan, Y., Wang, Z., Wang, S., & Liu, M. (2026) · Journal of Spectroscopy · doi:10.1155/jspe/5184138 · Cited by 1
Banga-Bothy, G.-A., & Samokhvalov, A. (2023) · Nanomaterials · doi:10.3390/nano13091529 · Cited by 1
Self-citationLei, Y., & Huo, J. (2024) · Polymer Science Series B · doi:10.1134/s1560090424601195 · Cited by 1
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Wang, X., Yan, C., Huo, Z., Dai, P., & Yao, D. (2025) · Photonics · doi:10.3390/photonics12030219
Study on the Adsorption Performance of Nitrite Nitrogen by Biomass Ash Filter Media
Yu, Z., Yu, J., Qu, Z., Zhang, H., Gao, Y., Niu, W., Ai, P., Feng, Y. X., Zhang, P., & Liu, N. (2026) · ACS Omega · doi:10.1021/acsomega.6c03634
Metadata
- Authors
- Samokhvalov, A., & McCombs, S.
- Affiliations
- Morgan State University (US)
- Corresponding author
- Samokhvalov, Alexander
- Venue
- Applied Spectroscopy
- Publisher
- SAGE Publications
- Published
- 2023-01-25
- Volume
- 77
- Issue
- 3
- Pages
- 308-319
- ISSN
- 0003-7028 (ISSN-L)
- 1943-3530
- OpenAlex
- W4311822526
- Cited by
- 9
- References
- 38
- Citations by year
- 2026: 2 · 2025: 2 · 2024: 2 · 2023: 3
- FWCI
- 0.78
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Applied Spectroscopy (publishedVersion)
- PubMed (publishedVersion)
- Funders
- Army Research Office (W911NF-20-1-0290, W911NF-21-2-0213)
- Topics
- Life Sciences › Biochemistry, Genetics and Molecular Biology › Biophysics › Spectroscopy Techniques in Biomedical and Chemical Research
- Physical Sciences › Chemistry › Spectroscopy › Spectroscopy and Laser Applications
- Physical Sciences › Chemistry › Analytical Chemistry › Spectroscopy and Chemometric Analyses
- Keywords
- controlled atmosphere, water vapor adsorption, water vapor desorption, relative humidity monitoring, gas-solid reactions, chemosensing, heterogeneous catalysis
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