AVIII 500 SSNMR

500MHz Schedule

Request 500 MHz Instrument time

For new users

Researchers from departments across the University of Delaware, other academic institutions, and private industry are welcome to submit samples for solid state NMR analysis. Contact Dr. Caitlin Quinn (cmquinn@udel.edu) for more information.

AVIII 500 Solid-state NMR

The AVIII 500 MHz solid-state NMR spectrometer, equipped with the latest generation hardware and software, is a three-channel spectrometer. We have three probes for characterizing a wide range of nuclei in systems including biosolids, inorganic materials, and organic compounds.

• Bruker 4.0 mm HX probe
• Bruker 3.2 mm EFree HCN probe
• NHMFL 3.2 mm Low-E HXY probe

Bruker 4.0 mm HX probe

This 2-channel broadband probe can be used for the study of a wide range of nuclei including 13C, 15N, 23Na, 27Al, 29Si, 31P, 119Sn, and 207Pb. The X channel tuning range is 50-205 MHz. This probe uses sample amounts of up to 100 mg and a maximum spinning speed of 15 kHz. Some recent applications are highlighted below.

(a) 13C and (b) 207Pb spectra of pigments used in oil paintings from the 15th through 18th centuries indicate the formation of lead soaps, a process implicated in the aging of artwork from this era. From the Dybowski group, Department of Chemistry and Biochemistry (1)

(a) 29Si and (b) 27Al MAS NMR spectra of aluminosilicate zeolites, synthesized in fluoride media, for the preparation of novel catalytic materials. From the Lobo group, Department of Chemical and Biomolecular Engineering (2)

Bruker 3.2 mm EFree HCN probe

Triple resonance probe for 13C, 15N, and low resolution 1H experiments. The EFree probe is ideal for isotopically enriched and high salt samples. It uses up to 50 mg of sample and has a maximum spinning speed of 24 kHz.

13C-13C 2D CORD spectrum of HIV-1 capsid protein assemblies. From the Polenova group, Department of Chemistry and Biochemistry (3,4)

NHMFL 3.2 mm Low-E HXY probe

Broadband triple resonance probe ideal for heteronuclear correlation experiments and can tune to a wide range of nuclei including 2H, 13C, 15N, 23Na, 27Al, 29Si, 31P, 51V, 63/65Cu, 77Se, 79Br, 123Te, and 207 Pb. It uses up to 50 mg of sample and has a maximum spinning speed of 25 kHz.

Information regarding the current schedule for the 500MHz spectrometer can be viewed in the Google Calendar. We accept reservation requests on a rolling basis. Users without training who wish to acquire data or those interested in receiving training should review the new user information and contact Dr. Caitlin Quinn (cmquinn@udel.edu).

Funding Information

“Acquisition of an 850 MHz NMR Spectrometer for Interdisciplinary Research at the University of Delaware”, NSF MRI-R2 0959496 (Principal Investigator: Tatyana Polenova, Co-principal Investigators: Cecil Dybowski, and Sharon Rozovsky), 2010 – 2013

References

(1) Catalano J, Murphy A, Yao Y, Alkan F, Zumbulyadis N, Centeno SA, Dybowski. 207Pb and 119Sn solid-state NMR and relativistic density functional theory studies of the historic pigment lead-tin yellow type I and Its reactivity in oil paintings. J Phys Chem A. 2014, 118, 7952-7958.

(2) Moteki T, Lobo RF. A general method for aluminum incorporation into high-silica zeolites prepared in fluoride media. Chem Mater. 2016, 28, 638-649.

(3) Hou G, Yan S, Trebosc J, Amoureux JP, Polenova T. Broadband homonuclear correlation spectroscopy driven by combined R2nv sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids. J Mag Reson. 2013, 232, 18-30.

(4) Lu M, Hou G, Zhang H, Suiter CL, Ahn J, Byeon IJL, Perilla JP, Langmead CJ, Hung I, Gor’kov PL, Gan Z, Brey W, Aiken C, Zhang P, Schulten K, Gronenborn AM, Polenova T. Dynamic allostery governs cyclophilin A- HIV capsid interplay. Proc Nat Acad Sci. 2015, 112, 14617-14622.