SPAM-MQ-HETCOR: an improved method for heteronuclear correlation spectroscopy between quadrupolar and spin-1/2 nuclei in solid-state NMR.

Jerzy W Wiench; Gregory Tricot; Laurent Delevoye; Julien Trebosc; James Frye; Lionel Montagne; Jean-Paul Amoureux; Marek Pruski

doi:10.1039/b512246e

PubMed · 16482254

SPAM-MQ-HETCOR: an improved method for heteronuclear correlation spectroscopy between quadrupolar and spin-1/2 nuclei in solid-state NMR.

Jerzy W Wiench·Gregory Tricot·Laurent Delevoye·Julien Trebosc·James Frye·Lionel Montagne·Jean-Paul Amoureux·Marek Pruski

View original source ↗Export metadata ↓

Abstract

The recently introduced concept of soft pulse added mixing (SPAM) is used in two-dimensional heteronuclear correlation (HETCOR) NMR experiments between half-integer quadrupolar and spin-1/2 nuclei. The experiments employ multiple quantum magic angle spinning (MQMAS) to remove the second order quadrupolar broadening and cross polarization (CP) or refocused INEPT for magnetization transfer. By using previously unexploited coherence pathways, the efficiency of SPAM-MQ-HETCOR NMR is increased by a factor of almost two without additional optimization. The sensitivity gain is demonstrated on a test sample, AlPO(4)-14, using CP and INEPT to correlate (27)Al and (31)P nuclei. SPAM-3Q-HETCOR is then applied to generate (27)Al-(31)P spectra of the devitrified 41Na(2)O-20.5Al(2)O(3)-38.5P(2)O(5) glass and the silicoaluminophosphate ECR-40. Finally, the method allowed the acquisition of the first high resolution solid-state correlation spectra between (27)Al and (29)Si.

Explore related subjects

Aluminum Aluminum Compounds Nuclear Magnetic Resonance, Biomolecular Oxygen Radioisotopes Phosphates Phosphorus Silicon Journal Article Research Support, Non-U.S. Gov't Research Support, U.S. Gov't, Non-P.H.S.

Keep this discovery

Explore connections, maps & timelines

BibTeX RIS

Jerzy W Wiench, Gregory Tricot, Laurent Delevoye, Julien Trebosc, James Frye, Lionel Montagne, Jean-Paul Amoureux, Marek Pruski. 2005-10-27. SPAM-MQ-HETCOR: an improved method for heteronuclear correlation spectroscopy between quadrupolar and spin-1/2 nuclei in solid-state NMR.. https://doi.org/10.1039/b512246e

Cite the original work for its findings. Save a collection to share your selection of sources.

KEEP EXPLORING

Related citations

PubMed2007

Direct demonstration of enhanced diffusion in mesoporous ZSM-5 zeolite obtained via controlled desilication.

A 2 orders of magnitude gas transport improvement in a medium pore ZSM-5 zeolite has been achieved upon introduction of intracrystalline mesoporosity in gradient-free crystals by desilication post-treatment in alkaline medium.

Aluminum↗

PubMed2007

Estimates of ambient background concentrations of trace metals in soils for risk assessment.

Site-specific or soil type-specific ambient background concentrations (ABCs) of trace metals in soils are needed for risk assessment. We investigated three different methods for estimating ABCs in soils using a dataset of 5691 soil samples from England and Wales. The concentrations of Co, Cr and Ni were strongly associated with Al and Fe, and multiple regressions explained 62-85% of their variation, and Al and Fe can therefore be used to predict ABCs for these metals. Soil texture had a major influence on the concentrations of Cd, Co, Cr, Cu, Ni and Zn, and the medians were 3-5 fold higher in clayey than in sandy soils. This was used to predict texture-specific ABCs. Lead concentration was higher in acidic peaty soils than in other soils. A probability graph method was used to estimate ABC for Pb in a population of relatively uncontaminated soils. Potential applications of ABCs are discussed.

Aluminum↗

PubMed2007

Quantitative trait loci and candidate gene mapping of aluminum tolerance in diploid alfalfa.

Aluminum (Al) toxicity in acid soils is a major limitation to the production of alfalfa (Medicago sativa subsp. sativa L.) in the USA. Developing Al-tolerant alfalfa cultivars is one approach to overcome this constraint. Accessions of wild diploid alfalfa (M. sativa subsp. coerulea) have been found to be a source of useful genes for Al tolerance. Previously, two genomic regions associated with Al tolerance were identified in this diploid species using restriction fragment length polymorphism (RFLP) markers and single marker analysis. This study was conducted to identify additional Al-tolerance quantitative trait loci (QTLs); to identify simple sequence repeat (SSR) markers that flank the previously identified QTLs; to map candidate genes associated with Al tolerance from other plant species; and to test for co-localization with mapped QTLs. A genetic linkage map was constructed using EST-SSR markers in a population of 130 BC(1)F(1) plants derived from the cross between Al-sensitive and Al-tolerant genotypes. Three putative QTLs on linkage groups LG I, LG II and LG III, explaining 38, 16 and 27% of the phenotypic variation, respectively, were identified. Six candidate gene markers designed from Medicago truncatula ESTs that showed homology to known Al-tolerance genes identified in other plant species were placed on the QTL map. A marker designed from a candidate gene involved in malic acid release mapped near a marginally significant QTL (LOD 2.83) on LG I. The SSR markers flanking these QTLs will be useful for transferring them to cultivated alfalfa via marker-assisted selection and for pyramiding Al tolerance QTLs.

Aluminum↗