scholarly journals Hyperpolarised 1H–13C Benchtop NMR Spectroscopy

2019 ◽  
Vol 9 (6) ◽  
pp. 1173 ◽  
Author(s):  
Alastair Robinson ◽  
Peter Richardson ◽  
Meghan Halse
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Signal To Noise Ratio ◽  
Natural Abundance ◽  
Detection Methods ◽  
Natural Isotopic Abundance ◽  
Peak Overlap ◽  
Total Experiment Time ◽  
Weak Magnetic Fields ◽  
Low Sensitivity

Benchtop NMR spectrometers with sub-ppm spectral resolution have opened up new opportunities for performing NMR outside of the standard laboratory environment. However, the relatively weak magnetic fields of these devices (1–2 T) results in low sensitivity and significant peak overlap in 1H NMR spectra. Here, we use hyperpolarised 13C{1H} NMR to overcome these challenges. Specifically, we demonstrate the use of the signal amplification by reversible exchange (SABRE) parahydrogen-based hyperpolarisation technique to enhance the sensitivity of natural abundance 1D and 2D 13C{1H} benchtop NMR spectra. We compare two detection methods for SABRE-enhanced 13C NMR and observe an optimal 13C{1H} signal-to-noise ratio (SNR) for a refocused INEPT approach, where hyperpolarisation is transferred from 1H to 13C. In addition, we exemplify SABRE-enhanced 2D 13C benchtop NMR through the acquisition of a 2D HETCOR spectrum of 260 mM of 4-methylpyridine at natural isotopic abundance in a total experiment time of 69 min. In theory, signal averaging for over 300 days would be required to achieve a comparable SNR for a thermally polarised benchtop NMR spectrum acquired of a sample of the same concentration at natural abundance.

scholarly journals Searching for the weakest detectable magnetic fields in white dwarfs

2018 ◽  
Vol 618 ◽  
pp. A113 ◽  
Author(s):  
S. Bagnulo ◽  
J. D. Landstreet
Keyword(s):  
Magnetic Fields ◽  
White Dwarfs ◽  
Signal To Noise Ratio ◽  
Field Measurements ◽  
Weak Field ◽  
Magnetic Star ◽  
Weak Magnetic Fields ◽  
Medium Resolution ◽  
Magnetic Stars ◽  
Low Sensitivity

Our knowledge of the magnetism in white dwarfs is based on an observational dataset that is biased in favour of stars with very strong magnetic fields. Most of the field measurements available in the literature have a relatively low sensitivity, while current instruments allow us to detect magnetic fields of white dwarfs with sub-kG precision. With the aim of obtaining a more complete view of the incidence of magnetic fields in degenerate stars, we have started a long-term campaign of high-precision spectropolarimetric observations of white dwarfs. Here we report the results obtained so far with the low-resolution FORS2 instrument of the ESO VLT and the medium-resolution ISIS instrument of the WHT. We have considered a sample of 48 stars, of which five are known magnetic or suspected magnetic stars, and obtained new longitudinal magnetic field measurements with a mean uncertainty of about 0.6 kG. Overall, in the course of our survey (the results of which have been partially published in papers devoted to individual stars) we have discovered one new weak-field magnetic white dwarf, confirmed the magnetic nature of another, found that a suspected magnetic star is not magnetic, and suggested two new candidate magnetic white dwarfs. Even combined with data previously obtained in the literature, our sample is not sufficient yet to reach any final conclusions about the actual incidence of very weak magnetic fields in white dwarfs, but we have set the basis to achieve a homogeneous survey of an unbiased sample of white dwarfs. As a by-product, our survey has also enabled us to carry out a detailed characterisation of the ISIS and the FORS2 instruments for the detection of extremely weak magnetic fields in white dwarfs, and in particular to relate the signal-to-noise ratio to measurement uncertainty for white dwarfs of different spectral types. This study will help the optimisation of future observations.

scholarly journals Univariate Statistical Analysis as a Guide to 1H-NMR Spectra Signal Assignment by Visual Inspection

Metabolites ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 15 ◽  
Author(s):  
Chenglin Zhu ◽  
Beatrice Vitali ◽  
Gilbert Donders ◽  
Carola Parolin ◽  
Yan Li ◽  
...  
Keyword(s):  
Statistical Analysis ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Visual Inspection ◽  
Signal To Noise Ratio ◽  
1H Nmr Spectra ◽  
Proton Nuclear Magnetic Resonance ◽  
Signal Assignment ◽  
Hands On ◽  
Interested User

In Proton Nuclear Magnetic Resonance (1H-NMR) spectroscopy, the signals assignment procedure is normally conducted by visual inspection of the spectra, by taking advantage of the innate predisposition of human eye for pattern recognition. In the case of untargeted metabolomics investigations on food and body fluids, the complexity of the spectra may lead the user to overlook signals, independently from their biological relevance. Here, we describe a four steps procedure that is designed to guide signals assignment task by visual inspection. The procedure can be employed whenever an experimental plan allows for the application of a univariate statistical analysis on a point-by-point basis, which is commonly the case. By comparing, as a proof of concept, 1H-NMR spectra of vaginal fluids of healthy and bacterial vaginosis (BV) affected women, we show that the procedure is also readily usable by non-experts in three particularly challenging cases: overlapping multiplets, poorly aligned signals, and signals with very poor signal-to-noise ratio. The paper is accompanied by the necessary codes and examples written in R computational language to allow the interested user gaining a hands-on impression of the procedure’s strengths and weaknesses.

The Electron Effect of Aromatic Group: Control Conformation of 2-Aromatic Cyclododecanone Derivatives

2020 ◽  
Vol 24 (10) ◽  
pp. 1139-1147
Author(s):  
Yang Mingyan ◽  
Wang Daoquan ◽  
Wang Mingan
Keyword(s):  
1H Nmr ◽  
13C Nmr ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
The Other ◽  
Repulsive Interaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Effect ◽  
Group Control

2-Phenylcyclododecanone and 2-cyclohexylcyclododecanone derivatives were synthesized and characterized by 1H NMR, 13C NMR, HR-ESI-MS and X-ray diffraction. Their preferred conformations were analyzed by the coupling constants in the 1H NMR spectra and X-ray diffraction, which showed the skeleton ring of these derivatives containing [3333]-2-one conformation, and the phenyl groups were located at the side-exo position of [3333]-2-one conformation due to the strong π-π repulsive interaction between the π- electron of benzene ring and π-electron of carbonyl group. The cyclohexyl groups were located at the corner-syn or the side-exo position of [3333]-2-one conformation depending on the hindrance of the other substituted groups. The π-π electron effect played a crucial role in efficiently controlling the preferred conformation of 2-aromatic cyclododecanone and the other 2-aromatic macrocyclic derivatives with the similar preferred square and rectangular conformations.

1H-NMR spectra of high-boiling adamantylaromatic compounds

1978 ◽  
Vol 43 (1) ◽  
pp. 250-256
Author(s):  
Jaroslava Podehradská ◽  
Milan Hájek ◽  
Slavoj Hála
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
1H Nmr Spectra

119Sn, 13C and 1H NMR Spectra of Tris(1-butyl)stannyl D-Glucuronate

1997 ◽  
Vol 62 (8) ◽  
pp. 1169-1176 ◽  
Author(s):  
Antonín Lyčka ◽  
Jaroslav Holeček ◽  
David Micák
Keyword(s):  
Chemical Shift ◽  
Carbonyl Group ◽  
1H Nmr ◽  
Equatorial Plane ◽  
Title Compound ◽  
Nmr Spectra ◽  
Hydroxyl Groups ◽  
Carboxylic Group ◽  
H Nmr ◽  
Oxygen Atoms

The 119Sn, 13C and 1H NMR spectra of tris(1-butyl)stannyl D-glucuronate have been measured in hexadeuteriodimethyl sulfoxide, tetradeuteriomethanol and deuteriochloroform. The chemical shift values have been assigned unambiguously with the help of H,H-COSY, TOCSY, H,C-COSY and 1H-13C HMQC-RELAY. From the analysis of parameters of 119Sn, 13C and 1H NMR spectra of the title compound and their comparison with the corresponding spectra of tris(1-butyl)stannyl acetate and other carboxylates it follows that in solutions of non-coordinating solvents (deuteriochloroform) the title compound is present in the form of more or less isolated individual molecules with pseudotetrahedral environment around the central tin atom and with monodentately bound carboxylic group. The interaction of tin atom with oxygen atoms of carbonyl group and hydroxyl groups of the saccharide residue - if they are present at all - are very weak. In solutions in coordinating solvents (hexadeuteriodimethyl sulfoxide or tetradeuteriomethanol), the title compound forms complexes with one molecule of the solvent. Particles of these complexes have a shape of trigonal bipyramid with the 1-butyl substituents in equatorial plane and the oxygen atoms of monodentate carboxylic group and coordinating solvent in axial positions.

A 15N, 13C, and 1H NMR study of reaction products from arylguanidines and chloroformate esters

1991 ◽  
Vol 56 (7) ◽  
pp. 1505-1511 ◽  
Author(s):  
Antonín Lyčka ◽  
Karel Palát
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Reaction Products ◽  
H Nmr ◽  
Nmr Study

The 15N, 13C, and 1H NMR spectra of the reaction products from arylguanidines with two mols of chloroformate esters have been measured. With application of the corresponding 15N isotopomer it has been proved that the reaction products have the structures IIIa-IIIc.

scholarly journals Detectivity optimization to detect of ultraweak light fluxes with an EM-CCD as binary photon counter array

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Ibtissame Khaoua ◽  
Guillaume Graciani ◽  
Andrey Kim ◽  
François Amblard
Keyword(s):  
Dynamic Range ◽  
Signal To Noise Ratio ◽  
Photon Counting ◽  
Detection Methods ◽  
Strong Nonlinearity ◽  
Wide Range ◽  
Depth Analysis ◽  
Spatially Extended ◽  
Extended Sources ◽  
Photon Counting Mode

AbstractFor a wide range of purposes, one faces the challenge to detect light from extremely faint and spatially extended sources. In such cases, detector noises dominate over the photon noise of the source, and quantum detectors in photon counting mode are generally the best option. Here, we combine a statistical model with an in-depth analysis of detector noises and calibration experiments, and we show that visible light can be detected with an electron-multiplying charge-coupled devices (EM-CCD) with a signal-to-noise ratio (SNR) of 3 for fluxes less than $$30\,{\text{photon}}\,{\text{s}}^{ - 1} \,{\text{cm}}^{ - 2}$$ 30 photon s - 1 cm - 2 . For green photons, this corresponds to 12 aW $${\text{cm}}^{ - 2}$$ cm - 2 ≈ $$9{ } \times 10^{ - 11}$$ 9 × 10 - 11 lux, i.e. 15 orders of magnitude less than typical daylight. The strong nonlinearity of the SNR with the sampling time leads to a dynamic range of detection of 4 orders of magnitude. To detect possibly varying light fluxes, we operate in conditions of maximal detectivity $${\mathcal{D}}$$ D rather than maximal SNR. Given the quantum efficiency $$QE\left( \lambda \right)$$ Q E λ of the detector, we find $${ \mathcal{D}} = 0.015\,{\text{photon}}^{ - 1} \,{\text{s}}^{1/2} \,{\text{cm}}$$ D = 0.015 photon - 1 s 1 / 2 cm , and a non-negligible sensitivity to blackbody radiation for T > 50 °C. This work should help design highly sensitive luminescence detection methods and develop experiments to explore dynamic phenomena involving ultra-weak luminescence in biology, chemistry, and material sciences.

scholarly journals Rapid and Sensitive Detection of miRNA Based on AC Electrokinetic Capacitive Sensing for Point-of-Care Applications

Sensors ◽  
2021 ◽  
Vol 21 (12) ◽  
pp. 3985
Author(s):  
Nan Wan ◽  
Yu Jiang ◽  
Jiamei Huang ◽  
Rania Oueslati ◽  
Shigetoshi Eda ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Point Of Care ◽  
Low Cost ◽  
Clinical Diagnostics ◽  
Detection Methods ◽  
Capacitive Sensing ◽  
Application Potential ◽  
Mirna Detection ◽  
Mirna 25 ◽  
Low Sensitivity

A sensitive and efficient method for microRNAs (miRNAs) detection is strongly desired by clinicians and, in recent years, the search for such a method has drawn much attention. There has been significant interest in using miRNA as biomarkers for multiple diseases and conditions in clinical diagnostics. Presently, most miRNA detection methods suffer from drawbacks, e.g., low sensitivity, long assay time, expensive equipment, trained personnel, or unsuitability for point-of-care. New methodologies are needed to overcome these limitations to allow rapid, sensitive, low-cost, easy-to-use, and portable methods for miRNA detection at the point of care. In this work, to overcome these shortcomings, we integrated capacitive sensing and alternating current electrokinetic effects to detect specific miRNA-16b molecules, as a model, with the limit of detection reaching 1.0 femto molar (fM) levels. The specificity of the sensor was verified by testing miRNA-25, which has the same length as miRNA-16b. The sensor we developed demonstrated significant improvements in sensitivity, response time and cost over other miRNA detection methods, and has application potential at point-of-care.

scholarly journals 13C and 1H NMR Spectra of Synthetic (25R)-5α-Spirostanes

1999 ◽  
Vol 23 (1) ◽  
pp. 48-49
Author(s):  
Martín A. Iglesias Arteaga ◽  
Carlos S. Pérez Martinez ◽  
Roxana Pérez Gil ◽  
Francisco Coll Manchado
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
1H Nmr Spectra ◽  
H Nmr ◽  
C 23 ◽  
Main Effects ◽  
Nmr Signals

The assignment of 13C and 1H NMR signals of synthetic (25 R)-5α-spirostanes is presented; the main effects on chemical shifts due to substitution at C-23 are briefly discussed.

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