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Solid-State 207Pb NMR Spectroscopy and Relativistic Quantum Chemical Calculations of Red Pigments: Identification in Cultural Heritage Materials

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Abstract

Solid-state \(^{207}\)Pb NMR spectroscopy was used to identify the pigments painted on the surface of a cultural heritage material. The \(^{207}\)Pb NMR magic-angle-spinning spectrum was measured under 18.8 T for the 1.0% lead-containing pigment sample of a historical clay doll. By comparing with the reference spectrum and NMR parameters, minium (Pb\(_3\)O\(_4\)) was determined to be used as a red pigment in the doll. Further, spectral simulation and relativistic density functional theory calculations were carried out for Pb\(_3\)O\(_4\) and related compounds. It was confirmed for the large chemical shift anisotropy of the Pb\(^\mathrm {II}\) species with the hemi-directed structure that the calculations with the minimum PbO\(_n\) moiety can generate incorrect values and that large size clusters are needed for improving accuracy even with the fully relativistic method.

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Acknowledgements

This work was supported by the NIMS microstructural characterization platform as a program of the Nanotechnology Platform of MEXT, Japan, Grant no. JPMXP09A19NM0173. Financial support from the JSPS [Grant-in-Aid for Scientific Research (C) No. 17K05741] is gratefully acknowledged. We would like to thank Editage for English language editing.

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  1. Institute of Arts and Sciences, Yamagata University, Yamagata, 990-8560, Japan

    Takahiro Iijima & Takahiro Abe

  2. NMR Station, National Institute for Materials Science, Tsukuba, 305-0003, Japan

    Kenzo Deguchi, Shinobu Ohki & Masataka Tansho

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  1. Takahiro Iijima
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Iijima, T., Abe, T., Deguchi, K. et al. Solid-State 207Pb NMR Spectroscopy and Relativistic Quantum Chemical Calculations of Red Pigments: Identification in Cultural Heritage Materials. Appl Magn Reson 53, 371–385 (2022). https://doi.org/10.1007/s00723-021-01449-5

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