Electron spin resonance and raman scattering spectroscopy of multi-walled carbon nanotubes: a function of acid treatment.

We compare the fundamental transport mechanism in multi-walled carbon nanotubes (MWNTs) by means of electron spin resonance (ESR) and Raman spectroscopy as a function of acid treatment. The ESR and Raman results show that the acid treatment reduces the density of states at the Fermi level. Defects introduced through the acid treatment move the Fermi level closer to the K points in the valence band, and consequently conduction is reduced. These defects are identified as Stone-Wales type from the Raman results.

NMR spectroscopy of hydrogen adsorption on single-walled carbon nanotubes after exposure to high pressure.

Hydrogen storage properties of single-walled carbon nanotubes (CNTs) after exposure to a pressure of 14.3 MPa are studied by (1)H nuclear magnetic resonance spectroscopy. The nanotubes were carefully pre-characterized using inductively coupled plasma mass spectrometry (ICP-MS), transmission electron microscopy (TEM), and Raman spectroscopy. We have shown previously that at ambient temperature in the pressure range from 0 to 1.5 MPa, hydrogen adsorption is fast and reversible and must be described as physisorption. However, exposure to a much higher pressure (14.3 MPa) of hydrogen leads to slower desorption kinetics where longer exposure causes greater hydrogen uptake. Our data suggest that interstitial sites and the tube interior may be identified as these strong adsorption sites.

129Xe and 131Xe NMR of gas adsorption on single- and multi-walled carbon nanotubes.

129Xe and 131Xe nuclear magnetic resonance (NMR) spectroscopy was used to study the adsorption of xenon gas on as-produced single-walled and multi-walled carbon nanotubes. Overall, the adsorption was weak, with slightly stronger interaction between xenon and multi-walled nanotubes. Temperature-dependent spectra, relaxation times, line widths, and signal intensities provide evidence that xenon forms a multilayer bulk phase rather than a homogeneous surface coating. The estimated adsorption energy of 1.6 kJ/mol is significantly lower than 23 kJ/mol predicted for monolayer adsorption but is in keeping with the Xe-Xe attractive potential. Xenon preferentially adsorbs on metallic particles in single-walled tubes, while defects are the nucleation sites for the stronger adsorption on multi-walled tubes.

Continuous-flow optical pumping NMR in a closed circuit system.

In a typical continuous-flow optical pumping setup, the chemical shift of xenon in the adsorbed phase depends on the gas flow rate due to warming of the sample surface by the gas stream. Calibration of the system using the (207)Pb resonance of solid lead nitrate is necessary to determine the actual sample temperature. Optimum pulse repetition rates are strongly affected by gas flow and spin-lattice relaxation rates. The interplay of flow and pulse repetition rate alters signal intensity ratios and may lead to the complete suppression of signals.

Surface selective 1H/29Si CP NMR by NOE enhancement from laser polarized xenon

The surface proton spin polarization created by the spin-polarization-induced nuclear Overhauser effect from optically polarized xenon can be transferred in a subsequent step by solid-state cross polarization to another nuclear spin species such as 29Si. The technique exploits the dipolar interactions of xenon nuclear spins with high gamma nuclei such as 1H, and is experimentally simpler than direct polarization transfer from 129Xe to heteronuclei such as 13C and 29Si. Copyright 1998 Academic Press.

31P to 77Se cross polarization in beta-P4Se3.

Cross polarization from 31P to 77Se is demonstrated in beta-P4Se3. This material, an inorganic glass, is readily synthesized from the elements and serves as a convenient sample for setting the Hartmann-Hahn condition.

NMR of laser-polarized xenon in human blood.

By means of optical pumping with laser light it is possible to enhance the nuclear spin polarization of gaseous xenon by four to five orders of magnitude. The enhanced polarization has allowed advances in nuclear magnetic resonance (NMR) spectroscopy and magnetic resonance imaging (MRI), including polarization transfer to molecules and imaging of lungs and other void spaces. A critical issue for such applications is the delivery of xenon to the sample while maintaining the polarization. Described herein is an efficient method for the introduction of laser-polarized xenon into systems of biological and medical interest for the purpose of obtaining highly enhanced NMR/MRI signals. Using this method, we have made the first observation of the time-resolved process of xenon penetrating the red blood cells in fresh human blood-the xenon residence time constant in the red blood cells was measured to be 20.4 +/- 2 ms. The potential of certain biologically compatible solvents for delivery of laser-polarized xenon to tissues for NMR/MRI is discussed in light of their respective relaxation and partitioning properties.