High resolution solid state nuclear magnetic resonance spectroscopy

E. Vinogradov and P.K. Madhu, High-Resolution Proton Nuclear Magnetic Resonance Spectroscopy in the Solid State , p. 297... 

Hays GR. 1982. High resolution carbon-13 solid-state nuclear magnetic resonance spectroscopy. Analyst 107 241-252. 

Fletton, R. A., Lancaster, R. W., Harris, R. K., Kenwright, A. M., Packer, K. J., Waters, D. N. and Yeadon, A. (1986). A comparative spectroscopic investigation of two polymorphs of 4 -methyl-2 -nitroacetanilide using solid-state infrared and high-resolution solid-state nuclear magnetic resonance spectroscopy. J. Chem. Soc. Perkin Trans. 2,1705-9. [224]... 

MacKenzie KJD, Brown IWM, Meinhold RH, Bowden ME (1985) Thermal reactions of pyrophyllite studied by high-resolution solid state Al and Si nuclear magnetic resonance spectroscopy. J Am Ceram Soc 68 266-272... 

R., A Study of Carbon and Hydrogen Aromaticity in Coals by High Resolution Solid State Nuclear Magnetic Resonance and Fourier Transform IR Spectroscopy, (to be published)... 

The instrumental analytical techniques discussed in this chapter are those used most frequently to identify plastics in collections. There are many techniques that are used in the plastics industry or university research laboratory which provide extensive information about synthetic materials, but which have not yet found a place in the conservation workshop. This may be attributed to the high cost of the instruments and their maintenance. For this reason they have not been included here. High resolution solid state nuclear magnetic resonance spectroscopy is one such technique which may well be found in many museum laboratories by 2015, but is not available to such institutions today (Lambert et al., 2000). Descriptions of instrumental analytical techniques have been divided into those used to identify polymers, those to examine fillers and those to characterize plasticizers, stabilizers and flame retardants. 

High-resolution H solid-state magic-anglespinning nuclear magnetic resonance spectroscopy has been used to identify the microenvironment of methanol molecules in sulfonated poly(phenylene ether ether sulfone) and Nafion 117 membranes. 

Belton P.S., Tanner S.F., Cartier N., and Chanzy H. 1989. High-resolution solid-state C nuclear magnetic resonance spectroscopy of tunicin, animal cellulose. Macromolecules 22 1615-1617. 

Nuclear magnetic resonance spectroscopy (NMR) is the determination of molecular structures by analysis of static and dynamic features of the materials [42]. In NMR experiments both a magnetic field and a radiofrequency field are applied to a solid sample or a solution resulting in an absorption of energy which is detected as a nuclear magnetic resonance. Spectrometers are also available for high resolution solid state NMR. Nuclei in different chemical environments resonate at different frequencies and thus differ in their chemical shift. Chemical shifts are used to assign these resonances to the specific structure of the sample. The nuclear environment of a nucleus results in multiple resonances that are also used to determine structural information. NMR studies are conducted to deter-... 

Takegoshi K, Hikichi K. Effects of blending on local chain dynamics and glass transition Polystyrene/polyfvinyl methyl ether) blends as studied by high-resolution solid-state 1 3C nuclear magnetic resonance spectroscopy. J Chem Phys 1991 94 3200. 

Mizuno M, Hirai A, Matsuzawa H, Endo K, Suhara M, Kemnotsu M, et al. Study of odd-even effect of flexible spacer length on the chain dynamics of main-chain thermotropic hquid-erystaUme polymers using high-resolution solid-state C-13 nuclear magnetic resonance spectroscopy. Macromolecules 2002 35 2595-601. 

In this chapter, three methods for measuring the frequencies of the vibrations of chemical bonds between atoms in solids are discussed. Two of them, Fourier Transform Infrared Spectroscopy, FTIR, and Raman Spectroscopy, use infrared (IR) radiation as the probe. The third, High-Resolution Electron Enetgy-Loss Spectroscopy, HREELS, uses electron impact. The fourth technique. Nuclear Magnetic Resonance, NMR, is physically unrelated to the other three, involving transitions between different spin states of the atomic nucleus instead of bond vibrational states, but is included here because it provides somewhat similar information on the local bonding arrangement around an atom. 

C.R.C. Press, 1983 (b) R.A. Komoroski (Ed), High Resolution NMR of Synthetic Polymers in Bulk, VCH Publishers, 1986 (c) V.J. McBriety and K.J. Packer, Nuclear Magnetic Resonance in Solid Polymers, Cambridge University Press, Cambridge, 1993 (d) K. Schmidt-Rohr and H.W. Spiess, Multidimensional Solid State NMR and Polymers, Academic Press, London, 1994 (e) G.A. Webb and I.Ando (Eds), Ann. Repts. NMR Spectroscopy (Special Issue NMR in Polymer Science), Vol. 34, Academic Press, London, 1997. 

We present a solid-state nuclear magnetic resonance (NMR) experiment that allows the observation of a high-resolution two-dimensional heteronuclear correlation (2D HETCOR) spectrum between aluminum and phosphorous in aluminophosphate molecular sieve VPI-5. The experiment uses multiple quantum magic angle spinning (MQMAS) spectroscopy to remove the second order quadrupolar broadening in Al nuclei. The magnetization is then transferred to spin-1/2 nuclei of P via cross polarization (CP) to produce for the first time isotropic resolution in both dimensions. 

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