A method for improved quantification of 1H NMR signals under low-resolution conditions for solids

Avadhut, Yamini S.; Schneider, Denis; Günne, Jörn Schmedt auf der

doi:10.1016/j.jmr.2009.07.019

Cited by 25 publications

(24 citation statements)

References 23 publications

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“…Since all DMSO molecules present in these samples are found to be mobile at room temperature (based on 2 H-NMR data on deuterated samples, data not shown) and PAN proves to be completely immobile, we could obtain the number of DMSO molecules per PAN unit via a quantitative analysis of the 1 H MAS NMR spectra. Although we have to note that such an analysis may be biased to some extent [103] we can take the results (1-2 DMSO molecules per Li cation) as a rough estimate. In Fig.…”

Section: Polyacrylonitrile Based Electrolytesmentioning

confidence: 99%

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Wüllen¹,

Echelmeyer

Voigt

et al. 2010

Zeitschrift Für Physikalische Chemie

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Ionic TransportResearch on solid ionic conductors for use as electrolytes in all solid state batteries still constitutes a rather vivid branch of today's materials science. Despite enormous efforts, neither the development of a solid electrolyte fulfilling the key requirements such as mechanical stability and high ionic conductivity at ambient temperature has been successful nor has an extended understanding of the local Li coordination motifs in the often amorphous systems been obtained. In this contribution, recent progress both in the development of novel solid state electrolytes with high ionic conductivity and mechanical stability and in the characterization of the local Li coordination motifs in these electrolytes from our laboratory is presented. The work was performed as a project within the framework of the Collaborative Research Centre SFB 458 "Ionic Motion in Materials with Disordered Structures -From Elementary Steps to Macroscopic Transport". Results will be given for polymer electrolytes based on polyethylene oxide (PEO), polyphosphazene (PPZ) and polyacrylonitrile (PAN) with various Li salts, nano-composites of these polymer electrolytes and Al 2 O 3 as a ceramic filler, novel inorganic/organic hybrid electrolytes, in which a mixture of an ionic liquid and Li salt is confined within the pore system of a SiO 2 glass, and a crystalline electrolyte, Li 5 La 3 Nb 2 O 12 . Employing a range of advanced solid state NMR methodologies including dipolar based NMR techniques and pulsed field gradient (PFG) NMR and impedance spectroscopy we were able to obtain a detailed knowledge about the local Li cation coordination motifs and the mechanism of Li transport in these electrolytes. Especially the hybrid electrolytes and the salt rich PAN based polymer electrolytes were identified as rather promising materials which combine a high ionic conductivity and mechanical stability.

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Section: Polyacrylonitrile Based Electrolytesmentioning

confidence: 99%

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Wüllen¹,

Echelmeyer

Voigt

et al. 2010

Zeitschrift Für Physikalische Chemie

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“…[53] The quantitative 1 H NMR experiments and the error margins were obtained from ten spin-echo experiments with different echo delays up to 0.2 ms by following the protocol and data analysis steps described in ref. [54] and using adamantane as internal reference, with a mass ratio m analyte /m adamantane of 10.0 mg/ 1.77 mg. The raw data were corrected for off-resonance excitation and T 2 relaxation.…”

Section: Solid-state Nmr Measurementsmentioning

confidence: 99%

Oxonium Ions Substituting Cesium Ions in the Structure of the New High‐Pressure Borate HP‐Cs_1−x(H₃O)_xB₃O₅ (x=0.5–0.7)

Sohr

Neumair

Heymann

et al. 2014

Chemistry A European J

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The new high-pressure borate HP-Cs1-x (H3 O)x B3 O5 (x=0.5-0.7) was synthesized under high-pressure/high-temperature conditions of 6 GPa/900 °C in a Walker-type multianvil apparatus. The compound crystallizes in the monoclinic space group C2/c (Z=8) with the parameters a=1000.6(2), b=887.8(2), c=926.3(2) pm, β=103.1(1)°, V=0.8016(3) nm(3) , R1=0.0452, and wR2=0.0721 (all data). The boron-oxygen network is analogous to those of the compounds HP-MB3 O5 , (M=K, Rb) and exhibits all three structural motifs of borates-BO3 groups, corner-sharing BO4 tetrahedra, and edge-sharing BO4 tetrahedra-at the same time. Channels inside the boron-oxygen framework contain the cesium and oxonium ions, which are disordered on a specific site. Estimating the amount of hydrogen by solid-state NMR spectroscopy and X-ray diffraction led to the composition HP-Cs1-x (H3 O)x B3 O5 (x=0.5-0.7), which implies a nonzero phase width.

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“…Furthermore, choosing a nucleus possessing both high natural abundance and high gyromagnetic ratio assures that a sufficient signal to noise ratio can easily be obtained for accurate quantification. Unfortunately, the obvious choice in the solution state, 1 H-qNMR, is not an easy task in the solid state because of the small proton chemical shift range and the network of strong homonuclear 1 H dipolar couplings, resulting in broad overlapping resonances, even under magic-angle-spinning conditions [63]. However, 19 F magic-angle-spinning solidstate NMR has emerged as powerful method for quanti fication studies, as it combines the advantage of the high sensitivity of 19 F nuclei due to their high gyromagnetic ratio with high selectivity, i.e.…”

Section: Introductionmentioning

confidence: 99%

Metrologically traceable quantification of trifluoroacetic acid content in peptide reference materials by¹⁹F solid-state NMR

Brinkmann

Raza

2019

Metrologia

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Although solution-state NMR is frequently used in metrologically-traceable quantification studies, this is not the case for solid-state NMR. However, solid-state NMR allows quantification of substances without the need of dissolution, providing a truly non-destructive approach, and extending metrologically-traceable quantitative NMR to sample classes that are difficult to characterize in solution. In this contribution we present a thorough and rigorous protocol for 19 F quantitative solid-state NMR employing a certified reference material as external calibrant to provide metrological traceability to absolutely quantify the content of trifluoroacetic acid (TFA) in a peptide sample, typically the major impurity in synthetic peptides. The protocol includes determining the quantitative volume of the solid-state NMR sample holder (rotor), the ERETIC (electronic reference to access in vivo concentrations) method (Akoka et al 1999 Anal. Chem. 71 2554) to compensate for variations in the sensitivity of the radio frequency resonant circuit when an external calibrant is used, and the EASY (elimination of artefacts in NMR spectroscopy) method (Jaeger and Hemmann 2014 Solid State Nucl. Magn. Reson. 57-58 22) to effectively suppress the 19 F NMR background signal from the probe head. We applied the protocol to quantify the amount of TFA in a candidate NRC certified reference material of the peptide angiotensin II. The results obtained by 19 F quantitative solid-state NMR are in excellent agreement with those obtained by quantitative NMR in solution employing an internal calibrant.

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A method for improved quantification of 1H NMR signals under low-resolution conditions for solids

Cited by 25 publications

References 23 publications

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Oxonium Ions Substituting Cesium Ions in the Structure of the New High‐Pressure Borate HP‐Cs_1−x(H₃O)_xB₃O₅ (x=0.5–0.7)

Metrologically traceable quantification of trifluoroacetic acid content in peptide reference materials by¹⁹F solid-state NMR

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A method for improved quantification of 1H NMR signals under low-resolution conditions for solids

Cited by 25 publications

References 23 publications

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Local Li Cation Coordination and Dynamics in Novel Solid Electrolytes

Oxonium Ions Substituting Cesium Ions in the Structure of the New High‐Pressure Borate HP‐Cs1−x(H3O)xB3O5 (x=0.5–0.7)

Metrologically traceable quantification of trifluoroacetic acid content in peptide reference materials by19F solid-state NMR

Contact Info

Product

Resources

About

Oxonium Ions Substituting Cesium Ions in the Structure of the New High‐Pressure Borate HP‐Cs_1−x(H₃O)_xB₃O₅ (x=0.5–0.7)

Metrologically traceable quantification of trifluoroacetic acid content in peptide reference materials by¹⁹F solid-state NMR