Skip to Content
Merck
  • Chemical shift powder spectra enhanced by multiple-contact cross-polarization under slow magic-angle spinning.

Chemical shift powder spectra enhanced by multiple-contact cross-polarization under slow magic-angle spinning.

Journal of magnetic resonance (San Diego, Calif. : 1997) (2013-01-15)
Jésus Raya, Barbara Perrone, Jérôme Hirschinger
ABSTRACT

A simple multiple-contact cross-polarization (CP) scheme is applied to a powder sample of ferrocene and β-calcium formate under static and magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. We show that multiple equilibrations-re-equilibrations with the proton spin bath improves the polarization transfer efficiency at short contact times and provides higher signal enhancements than state-of-the art techniques such as adiabatic passage through the Hartmann-Hahn condition CP (APHH-CP) when MAS is applied. The resulting chemical shift powder spectra then are identical to the ones obtained by using ROtor-Directed Exchange of Orientations CP (APHH-RODEO-CP) with intensity gains of a factor 1.1-1.3.

MATERIALS
Product Number
Brand
Product Description

Supelco
Calcium formate, Standard for quantitative NMR, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Cesium formate, 98%
Sigma-Aldrich
Calcium formate, BioUltra, ≥99.0% (T)
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Thallium(I) formate, 97%
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Sodium formate, reagent grade, 97%
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Sodium formate, ACS reagent, ≥99.0%
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Sodium formate-13C, 99 atom % 13C
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Sigma-Aldrich
Potassium formate, ReagentPlus®, 99%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Sodium formate, 99.998% trace metals basis
Sigma-Aldrich
Ferrocene, 98%
Sigma-Aldrich
Potassium formate, BioUltra, ≥99.0% (NT)
Sigma-Aldrich
Sodium formate, BioUltra, ≥99.0% (NT)