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

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

doi:10.1039/C7DT00182G

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

Journal Article · Fri Feb 17 00:00:00 EST 2017 · Dalton Transactions

DOI:https://doi.org/10.1039/C7DT00182G· OSTI ID:1374744

Kobayashi, Takeshi ^[1]; Perras, Frederic A. ^[1]; Murphy, Anna ^[2]; Yao, Yao ^[2]; Catalano, Jaclyn ^[3]; Centeno, Silvia A. ^[4]; Dybowski, Cecil ^[2]; Zumbulyadis, Nicholas ^[5];

^[6]

Ames Lab., Ames, IA (United States)
Univ. of Delaware, Newark, DE (United States)
Montclair State Univ., Montclair, NJ (United States)
The Metropolitan Museum of Art, New York, NY (United States)
Independent Researcher, Rochester, NY (United States)
Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)

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. As a result, 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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Research Organization:: Ames Lab., Ames, IA (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1374744

Report Number(s):: IS-J-9296; ICHBD9

Journal Information:: Dalton Transactions, Vol. 46, Issue 11; ISSN 1477-9226

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 20 works

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