Vibrational Spectroscopy of Biological and Polymeric Materials

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Not only has pressure demonstrated great promises for producing new structures and materials but also many known hydrogen-rich materials have exhibited new transformations as well as totally different thermodynamic and kinetic behaviors under higher pressures than under ambient conditions. Hydrides in a wide range of different categories, such as calcium borohydride, sodium amide and ammonia borane, have been extensively investigated under high pressures by vibrational spectroscopy, X-ray diffraction and theoretical calculations [ 18 — 21 ].

Here ammonia borane NH 3 BH 3 is chosen as an example to demonstrate that vibrational spectroscopy can be an effective tool to elucidate novel high-pressure structures [ 18 , 21 ]. Using in situ Raman and synchrotron IR spectroscopy, the pressure behavior of ammonia borane complex as a promising hydrogen storage material was investigated up to 14 GPa [ 18 ].

With increasing pressure, the Raman and IR spectra suggest several solid-to-solid transformations at about 2. Upon decompression, these pressure-induced transformations are found completely reversible with intact chemical structure of the NH 3 BH 3 complex, but possible modifications to the crystal structures. The solid lines crossing the solid symbols are based on linear fit.

Infrared Spectroscopy of Polymers

The vertical dashed lines indicate the proposed phase boundaries. Reproduced with permission from reference [18]. The assignments are labeled for selected Raman mode at selected pressures. Reproduced with permission from reference [21]. Solid symbols are experimental data from this study, with squares for I4mm phase, circles for Pmn21 phase and diamonds for Cmc21 phase. The open squares are adopted from reference [22]. The solid lines denote the rough boundaries among the three known phases. The P1 phase labeled is considered tentative. Subsequently, ammonia borane was investigated at simultaneous high pressures up to 15 GPa and low temperatures down to 80 K by in situ Raman spectroscopy [ 21 ].

Upon cooling to K from room temperature at ambient pressure, ammonia borane transforms from I 4 mm to Pmn 2 1. Upon isothermal compression to 15 GPa at K, another three pressure-induced structural transformations were observed. These transitions can be evidenced by the change in the Raman profile as well as the pressure dependence of the major Raman modes Figure Upon decompression and warming-up, these P-T-induced transformations are found completely reversible.

With the aid of factor group analysis, the phases above 1. Further compression above 15 GPa leads to the gradual transformation to an amorphous phase. When combined with previously reported high-pressure and room-temperature data, our Raman measurements from multiple runs covering various P-T paths allowed the significant update of the P-T phase diagram of ammonia borane in the pressure range of 0—15 GPa and the temperature range of 80— K Figure Pressure-induced polymerization is a chemical process pertaining to green chemistry as the reactions can be carried out in the absence of any solvent or catalyst, which implies a lesser environmental impact.

Poly acrylic acid is a well-known polymer with a wide variety of industrial applications such as being super absorbent materials, biocompatible polymers, poly-electrolytes and nanopolymers in molecular devices. Therefore, it is very significant in the polymer industry to explore pressure-induced polymerization from this monomer, as the polymer product with improved properties distinct from that obtained using conventional synthetic methods might be obtained.

The first pressure-induced structural and polymeric transformations of acrylic acid were studied by in situ Raman spectroscopy [ 23 ]. Upon compression to 0. The two new high-pressure crystalline phases are labeled as phase I and II, respectively Figure 16a. Phase I had a possibly similar structure that resembles low-temperature phase reported previously. Phase II can be interpreted as a denser phase with strong intermolecular interactions leading to polymerization or oligomerization ultimately.

When compressed to above 8 GPa, acrylic acid transforms into a disordered polymeric phase Figure 16b. Upon decompression to ambient pressure, the retrieved polymeric phase exhibits a significant amount of acrylic acid monomers or oligomers. Comparative Raman measurements on standard commercial poly acrylic acid Figure 17 allowed the understanding of possible structures of the polymeric phase of acrylic acid produced in this study.

Raman spectra of acrylic acid at selected pressures upon compression in the pressure region of 0. Reproduced with permission from reference [23].

FTIR Analysis (FTIR Spectroscopy)

Using combined high-pressure and photon excitations especially in the UV range has demonstrated strong potential to produce new molecular materials in a highly efficient way. Upon UV irradiation, IR spectra of EG show two sets of distinctive profiles after specific reaction time, indicating multiple photon-induced chemical reactions, which can be designated as primary and secondary processes Figure Careful spectral analysis allows the identification of primary reaction products that include glycolaldehyde, acetaldehyde and methanol. Further photoreactions of these primary products led to the formation of the secondary products, which were identified as methane, formaldehyde, methoxymethanol, methylformate and carbon dioxide.

Based on these reaction products, possible reaction mechanisms and production pathways were proposed. We also found that the initial loading pressure of EG plays an important role in influencing the reaction kinetics as well as in controlling the accessibilities for some reaction channels such as for CH 4 Figure 19a. Quantitative analysis of the antisymmetric stretching mode of CO 2 formed at different loading pressures suggests the formation of CO 2 clathrate hydrates well as CO 2 clusters.


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The stabilities as well as relative abundance of these CO 2 species are found to be dependent on both pressure and radiation time Figure 19b. These observations revealed interesting pressure-induced CO 2 sequestration behaviors as a result of photochemical reactions of ethylene glycol. The most characteristic new IR bands emerged at Reproduced with permission from reference [24]. The pressures labeled for each sample indicate the final system pressure. ZIF-8 is a representative member of the zeolitic imidazolate framework ZIF family, an emerging class of porous materials with promising applications in gas storage and catalysis, etc.

As a result, substantial interest has been focused on the investigation of its structure and properties under different conditions. Pressure tuning has proven an important and effective means to modify the structures and thus the associated properties of porous materials. Upon compression to 1. However, further compression to higher pressures led to irreversible structural transitions to an amorphous phase characterized by the very broad IR profiles Figure 20b.

Nevertheless, the chemical structure of the framework was found to sustain extreme compression without permanent breaking down. Overall, the high-pressure behavior and especially the surprising chemical stability probed by in situ IR spectroscopy demonstrate strong promises storage applications of ZIF-8 under extreme conditions. In a subsequent study, ZIF-8 framework was investigated when loaded with CO 2 in a diamond anvil cell at high pressures of 0.

Upon loading, CO 2 molecules in two types of environment i. Furthermore, pressure was found to play a regulating role in the migration of CO 2 molecules with respect to the framework even at room temperature.


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The strong interactions between CO 2 and framework are evident from the IR features of the framework e. As guest molecules, CO 2 in turn can substantially enhance the structural stability of the ZIF-8 framework as compared to the empty framework Figure Reproduced with permission from reference [25].

Reproduced with permission from reference [26]. These far-IR spectra suggest that pressure can significantly modify the crystal structures of empty ZIF-8 framework irreversibly. As a promising candidate for the application of gas storage and separation, metal-organic framework MOF MIL has unique structural topology that contains two types of channels with distinct pore sizes. Using in situ IR spectroscopy, the behavior of as-made and activated MIL In and their structural reversibilities were investigated under high pressures [ 27 ].

Overall, the structures of both frameworks were found highly stable upon compression to 9 GPa. The structural modifications are found to be completely reversible upon decompression for as-made MIL In but irreversible for the activated framework.

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The different reversibility of framework is most likely associated with the solvent DMF molecules contained in the framework channels. Furthermore, the stability of the activated framework was investigated using PTM to achieve hydrostatic compression. As a result, structural modifications of the framework with PTM are completely reversible upon decompression Figure 23a. Our results show that at relative low pressures such as below 0.

Such pressure-regulated CO 2 occupation in different channels of the MIL framework is completely reversible between compression and decompression Figure 23c. The unique adsorption behavior of CO 2 in the MIL is strongly correlated with the OH units contributing as the primary binding sites through hydrogen bonding with CO 2.

Molecular dynamics simulations further support our analysis Figure The high framework stability and enhanced CO 2 adsorption of MIL In under high pressure make it a promising candidate for greenhouse gas storage. Reproduced with permission from reference [27]. Simulated contour plots of the CO2 probability density distributions along the hexagonal and triangular channels of MIL In framework at a 1 bar, b bar or 0.

In summary, this chapter demonstrated the application of in situ vibrational spectroscopy including Raman and FTIR spectroscopy in the elucidation of molecular structures and transformation mechanism for a wide variety of materials rendered under high-pressure conditions. Specifically, conformational changes, pressure-mediated hydrogen bonding interactions, molecular and crystal structural transitions, polymerizations and photon-assisted chemical reactions, as well as guest-host interactions of respective selected systems can be efficiently and accurately probed and characterized using in situ high-pressure Raman spectroscopy, FTIR spectroscopy or combination of both.

These spectroscopic data provided enormously valuable information for us to understand the pressure-induced phenomena at microscopic level in-depth. The methods that are described here are again not very common in books on infrared spectroscopy. In this chapter, the subject of two-dimensional correlation spectroscopy 2D-IR is also discussed.

Description of Research Areas Chemistry - UW Dept. of Chemistry

The principles of the technique along with selected examples of the applications of the 2D-IR treatment are presented. For researchers and graduate students in chemistry, materials science, chemical engineering, industrial chemistry, food science, pharmaceutical science, biophysics, molecular biology, polymer science and environmental science.

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