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Investigation of the hydrozincite structure by infrared and solid-state NMR spectroscopy

Roberta Sanna, Giovanni De Giudici, Andrea Mariano Scorciapino, Costantino Floris and Mariano Casu
Investigation of the hydrozincite structure by infrared and solid-state NMR spectroscopy
American Mineralogist (July 2013) 98 (7): 1219-1226

Abstract

To better understand lattice disorder in hydrozincite, natural hydrozincite samples and synthetic analogues were investigated by XRD, FTIR, (super 13) C MAS, and (super 13) C CPMAS NMR. The size of coherent diffraction domains ranges between approximately 10 nm (Synth1) and approximately 30 nm (Synth2). FTIR peaks from the antisymmetric CO (sub 3) (super 2-) stretching nu 3 mode were observed at 1383 and 1515 cm (super -1) in all samples. Peaks due to OH vibrations were observed for all the samples at 3234, 3303, and 3363 cm (super -1) , and were sharp only for the samples having larger crystal domains. The (super 13) C MAS and CPMAS NMR spectra showed a main carbon signal at 164 ppm in the Synth2 sample, while two main signals were observed at approximately 164 and approximately 168 ppm in the Synth1 sample. The intensity ratio of the latter signals were found to be independent of contact time, in the investigated range between 0.2 and 30 ms. In addition, (super 13) C CPMAS dynamics indicates that the Synth1 sample has shorter T (sub 1rho ) with respect to Synth2. This indicates a more effective process of spin diffusion of proton magnetization in the former due to different structural properties of Synth1 and Synth2 samples. In addition, chemical shift anisotropy analysis was attributed to a structural change in the carbonate group or hydrogen bonding for Synth1 and Synth2. This was interpreted as a deviation from the ideal structure generated by linear and planar lattice defects and/or grain boundaries.


ISSN: 0003-004X
EISSN: 1945-3027
Coden: AMMIAY
Serial Title: American Mineralogist
Serial Volume: 98
Serial Issue: 7
Title: Investigation of the hydrozincite structure by infrared and solid-state NMR spectroscopy
Affiliation: Complesso Universitario, Dipartimento di Scienze Chimiche e Geologiche, Cagliari, Italy
Pages: 1219-1226
Published: 201307
Text Language: English
Publisher: Mineralogical Society of America, Washington, DC, United States
References: 50
Accession Number: 2013-061393
Categories: Mineralogy of non-silicates
Document Type: Serial
Bibliographic Level: Analytic
Illustration Description: illus. incl. 1 table
Country of Publication: United States
Secondary Affiliation: GeoRef, Copyright 2017, American Geosciences Institute. Abstract, copyright, Mineralogical Society of America. Reference includes data from GeoScienceWorld, Alexandria, VA, United States
Update Code: 201337
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