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600 MHz Solid State NMR

Location and Contact Information

  • Hours: Open 24/7 to all qualified users.
  • Scheduling calendar: click here

Fees

The following user fees are effective as of 03/01/17

Federal Users - $9.50/h
Non-federal Users - $19.00/h
CCNY subsidized - $4.00/h

Images

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About the instrument

Description

The Agilent (Varian) DD2 600 MHz Solids NMR spectrometer is a mixed-use instrument  that is capable of  carrying out NMR experiments in solution, semi-solid, as well as solid states.  The main focus, however, is in solid state research.

The instrument operates with an actively-shielded 14.7 Tesla superconducting magnet.  It has a small 5-Gauss stray field boundary with a radius of 6 ft.  The proton NMR frequency is at 600 MHz.

The instrument contains 4 radio frequency (RF) channels, and is capable of carrying out sophisticated multi-nuclear, multi-dimensional experiments in structural biology, polymer science and materials science.  Two of the channels are equipped with kilowatt amplifiers and the other two with 300 watt amplifiers to deliver sufficient power to the probe for demanding solid state experiments.

Most solid state experiments are carried out under magic-angle-spinning (MAS) conditions.  In solids, dipolar interactions broaden the linewidth such that the spectral features cannot be discerned.  Spinning at 54.7 deg with respect to the magnetic field averages out these interactions and peaks become sharp.  Our fastest spinning probe is capable of spinning up to 40 kHz. (See Probes section.)

Our solid state NMR spectrometer is a sophisticated instrument that requires extensive training to operate.  All of our solids probes (see below) are of HXY-type magic angle-spinning probes, with two broadbanded channels from P31 to N15.  Current research interests include structural biology studies of isotopically labeled (C13, N15, and H2) proteins, natural-abundance as well as isotopically labeled plant and fungal materials, P31 studies of lipids and protein phosphorylation, as well as Li7 and B11 studies of energy storage materials.

Services

  • Multi-dimensional, multi-nuclear solid state NMR research on protein
  • Solid state NMR research on materials, such as natural or synthetic polymers, and energy storage material
  • Study of Semi-solid materials such as biological tissues or swollen polymers

Probes

  1. 3.2 mm BioMAS Probe: A 3 channel (HXY) MAS probe that spins up to 25 kHz.  It has a scroll coil that is designed to minimize electric field heating in samples that have high salt content, with some compromise in sensitivity.
  2. 1.6 mm FastMAS Probe: A 3 channel (HXY) MAS probe that spins up to 40 kHz.  The probe could offer higher resolution with reduced dipolar coupling because of the high spinning speed.  Despite the small size of sample rotor (1.6 mm), the probe has excellent sensitivity.
  3. 3.2 mm T3HXY probe: A 3 channel (HXY) MAS probe that spins up to 25 kHz.  It has a traditional solenoid coil with excellent sensitivity.
  4. 4 mm gHX nano Probe: A 2 channel (HX) probe that spins at magic angle up to 3 kHz and equipped with a z-pulsed field gradient.  It can run most of the solution state NMR experiments on solution or semi-solid samples, such as tissue samples or swollen polymer samples.
  5. 5 mm IDQG Probe: A 4 channel (H1, C13, N15, and P31) probe that is equipped with z-pulsed field gradient as well as deuterium decoupling capabilities.  It is designed for multidimensional, multinuclear protein research in solution.
  6. 5 mm Dual Broadband Probe: A 2 channel (H1/F19, X) probe with X nuclei in the inner coil to provide high X-nuclei sentivity.  It is a versatile probe for a wide range of nuclei in solution

Recent Publications

  1. W. Huang, O. Serra, K. Dastmalchi, L. Jin, L. Yang, and R. E. Stark, “Comprehensive MS and Solid-state NMR Metabolic Profiling Reveals Molecular Variations in Native Periderms from Four Solanum tuberosum Potato Cultivars,” J. Agric. Food Chem., 65, 2258–2274 (2017).
  2. P.-J. Hatton,*  S. Chatterjee,* T. Filley, K. Dastmalchi, A. F. Plante, S. Abiven, X. Gao, C. A. Masiello, S. Leavitt, K. J. Nadelhoffer, R. E. Stark, and J. A. Bird, "Tree Taxa and Pyrolysis Temperature Interact to Control the Efficacy of Pyrogenic Organic Matter Formation," Biogeochemistry, 130, 103-116 (2016).
  3. C. Fernandes, R. Prados-Rosales, B. Silva, A. Nakouzi-Naranjo, S. Chatterjee, R. E. Stark, A. Casadevall, and T. Gonçalves, “Activation of Melanin Synthesis in Alternaria infectoria by Antifungal Drugs,” Antimicrobial Agents and Chemotherapy, 60(3), 1216–1225 (2016).
  4. S. Chatterjee, A. J. Matas, T. Isaacson, C. Kehlet, J. K.C. Rose, and R. E. Stark, “Solid-state 13C NMR Delineates the Architectural Design of Biopolymers in Native and Genetically Altered Tomato Fruit Cuticles,” Biomacromolecules, 17(1), 215–224 (2016).
  5. R. Prados-Rosales, S. Toriola, A. Nakouzi, S. Chatterjee, R.E. Stark, G. Gerfen, P. Tumpowsky, E. Dadachova, and A. Casadevall, "Structural Characterization of Melanin Pigments from Commercial Preparations of the Edible Mushroom Auricularia auricula," J. Agric. Food Chem., 63(33), 7326-7332 (2015).
  6. K. Dastmalchi, L. Kallash, I. Wang, C.V. Phan, W. Huang, O. Serra, and R. E. Stark, “Defensive Armor of Potato Tubers: Nonpolar Metabolite Profiling, Antioxidant Assessment, and Solid-State NMR Compositional Analysis of Suberin-enriched Wound-Healing Tissues,” J. Agric. Food Chem., 63(30), 6810–6822 (2015).
  7. S. Chatterjee, R. Prados-Rosales, B. Itin, A. Casadevall, and R.E. Stark, “Solid-state NMR Reveals the Carbon-based Molecular Architecture of Melanized Cryptococcus neoformans Fungal Cells,” J. Biol. Chem., 290, 13779-13790 (2015).
  8. S. Chatterjee, R. Prados-Rosales, B. Itin, S. Tan, A. Casadevall, and R.E. Stark, “Demonstration of a Common Indole-based Aromatic Core in Natural and Synthetic Eumelanins by Solid-state NMR,” Org. Biomol. Chem., 12(34), 6730 - 6736 (2014).
  9. K. Dastmalchi, Q. Cai, K. Zhou, W. Huang, O. Serra, and R.E. Stark, “Completing the Jigsaw Puzzle of Wound-Healing Potato Cultivars: Metabolite Profiling and Antioxidant Activity,” J. Agric. Food Chem., 62, 7963-7975 (2014).
  10. O. Serra,* S. Chatterjee,* M. Figueras, M. Molinas, and R.E. Stark, “Deconstructing a plant macromolecular assembly: chemical architecture, molecular flexibility, and mechanical performance of natural and engineered potato suberins," Biomacromolecules, 15, 799-811 (2014).
  11. T.H. Yeats, W. Huang, S. Chatterjee, H. M-F. Viart, M.H. Clausen, R. E. Stark, and J.K.C. Rose, “Biochemical characterization of CD1 and Putative Orthologs Reveals an Ancient Family of Cutin Synthase-like (CUS) Proteins that are Conserved Among Land Plants,” The Plant J., 77, 667-675 (2014).