DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science

Takeshi Kobayashi, Frédéric A. Perras, Anna Murphy, Yao Yao, Jaclyn Catalano, Silvia A. Centeno, Cecil Dybowski, Nicholas Zumbulyadis, Marek Pruski

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

Dynamic nuclear polarization (DNP) is used to enhance the (ultra)wideline 207Pb solid-state NMR spectra of lead compounds of relevance in the preservation of cultural heritage objects. The DNP SSNMR experiments enabled, for the first time, the detection of the basic lead carbonate phase of the lead white pigment by 207Pb SSNMR spectroscopy. Variable-temperature experiments revealed that the short T′2 relaxation time of the basic lead carbonate phase hinders the acquisition of the NMR signal at room temperature. We additionally observe that the DNP enhancement is twice as large for lead palmitate (a lead soap, which is a degradation product implicated in the visible deterioration of lead-based oil paintings), than it is for the basic lead carbonate. This enhancement has allowed us to detect the formation of a lead soap in an aged paint film by 207Pb SSNMR spectroscopy; which may aid in the detection of deterioration products in smaller samples removed from works of art.

Original languageEnglish
Pages (from-to)3535-3540
Number of pages6
JournalDalton Transactions
Volume46
Issue number11
DOIs
StatePublished - 1 Jan 2017

Fingerprint

Nuclear magnetic resonance spectroscopy
Polarization
Soaps (detergents)
Deterioration
Nuclear magnetic resonance
Spectroscopy
Lead compounds
Palmitates
Painting
Pigments
Paint
Relaxation time
Oils
Experiments
Degradation
Temperature
Lead
lead carbonate

Cite this

Kobayashi, Takeshi ; Perras, Frédéric A. ; Murphy, Anna ; Yao, Yao ; Catalano, Jaclyn ; Centeno, Silvia A. ; Dybowski, Cecil ; Zumbulyadis, Nicholas ; Pruski, Marek. / DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy : an application to cultural heritage science. In: Dalton Transactions. 2017 ; Vol. 46, No. 11. pp. 3535-3540.
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abstract = "Dynamic nuclear polarization (DNP) is used to enhance the (ultra)wideline 207Pb solid-state NMR spectra of lead compounds of relevance in the preservation of cultural heritage objects. The DNP SSNMR experiments enabled, for the first time, the detection of the basic lead carbonate phase of the lead white pigment by 207Pb SSNMR spectroscopy. Variable-temperature experiments revealed that the short T′2 relaxation time of the basic lead carbonate phase hinders the acquisition of the NMR signal at room temperature. We additionally observe that the DNP enhancement is twice as large for lead palmitate (a lead soap, which is a degradation product implicated in the visible deterioration of lead-based oil paintings), than it is for the basic lead carbonate. This enhancement has allowed us to detect the formation of a lead soap in an aged paint film by 207Pb SSNMR spectroscopy; which may aid in the detection of deterioration products in smaller samples removed from works of art.",
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Kobayashi, T, Perras, FA, Murphy, A, Yao, Y, Catalano, J, Centeno, SA, Dybowski, C, Zumbulyadis, N & Pruski, M 2017, 'DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science', Dalton Transactions, vol. 46, no. 11, pp. 3535-3540. https://doi.org/10.1039/c7dt00182g

DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy : an application to cultural heritage science. / Kobayashi, Takeshi; Perras, Frédéric A.; Murphy, Anna; Yao, Yao; Catalano, Jaclyn; Centeno, Silvia A.; Dybowski, Cecil; Zumbulyadis, Nicholas; Pruski, Marek.

In: Dalton Transactions, Vol. 46, No. 11, 01.01.2017, p. 3535-3540.

Research output: Contribution to journalArticle

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T1 - DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy

T2 - an application to cultural heritage science

AU - Kobayashi, Takeshi

AU - Perras, Frédéric A.

AU - Murphy, Anna

AU - Yao, Yao

AU - Catalano, Jaclyn

AU - Centeno, Silvia A.

AU - Dybowski, Cecil

AU - Zumbulyadis, Nicholas

AU - Pruski, Marek

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