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

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.
Authors:
 [1] ;  [1] ;  [2] ;  [2] ;  [3] ;  [4] ;  [2] ;  [5] ; ORCiD logo [6]
  1. Ames Lab., Ames, IA (United States)
  2. Univ. of Delaware, Newark, DE (United States)
  3. Montclair State Univ., Montclair, NJ (United States)
  4. The Metropolitan Museum of Art, New York, NY (United States)
  5. Independent Researcher, Rochester, NY (United States)
  6. Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)
Publication Date:
Report Number(s):
IS-J-9296
Journal ID: ISSN 1477-9226; ICHBD9
Grant/Contract Number:
AC02-07CH11358
Type:
Accepted Manuscript
Journal Name:
Dalton Transactions
Additional Journal Information:
Journal Volume: 46; Journal Issue: 11; Journal ID: ISSN 1477-9226
Publisher:
Royal Society of Chemistry
Research Org:
Ames Lab., Ames, IA (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
OSTI Identifier:
1374744

Kobayashi, Takeshi, Perras, Frederic A., Murphy, Anna, Yao, Yao, Catalano, Jaclyn, Centeno, Silvia A., Dybowski, Cecil, Zumbulyadis, Nicholas, and Pruski, Marek. DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science. United States: N. p., Web. doi:10.1039/C7DT00182G.
Kobayashi, Takeshi, Perras, Frederic 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. United States. doi:10.1039/C7DT00182G.
Kobayashi, Takeshi, Perras, Frederic A., Murphy, Anna, Yao, Yao, Catalano, Jaclyn, Centeno, Silvia A., Dybowski, Cecil, Zumbulyadis, Nicholas, and Pruski, Marek. 2017. "DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science". United States. doi:10.1039/C7DT00182G. https://www.osti.gov/servlets/purl/1374744.
@article{osti_1374744,
title = {DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science},
author = {Kobayashi, Takeshi and Perras, Frederic A. and Murphy, Anna and Yao, Yao and Catalano, Jaclyn and Centeno, Silvia A. and Dybowski, Cecil and Zumbulyadis, Nicholas and Pruski, Marek},
abstractNote = {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.},
doi = {10.1039/C7DT00182G},
journal = {Dalton Transactions},
number = 11,
volume = 46,
place = {United States},
year = {2017},
month = {2}
}