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Related Concept Videos

Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

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Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other...
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
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NMR Spectrometers: Resolution and Error Correction01:14

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When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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Other Nuclides: 31P, 19F, 15N NMR01:16

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Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a...
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NMR Spectroscopy: Chemical Shift Overview01:15

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The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
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Coaxial-Tube Quantitative Nuclear Magnetic Resonance for Various Solutions Using SI-Traceable Concentration

Tatsuki Ogura1, Masataka Wakayama2

  • 1Institute for Advanced Biosciences, Keio University, 246-2 Mizukami, Kakuganji, Tsuruoka, Yamagata 997-0052, Japan.

Analytical Chemistry
|July 8, 2024
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Summary

This study introduces an effective volume ratio (EVR) method for coaxial-tube quantitative nuclear magnetic resonance (qNMR). This technique enables accurate analyte quantification without mixing, preserving sample integrity and allowing for reuse.

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy

Background:

  • Quantitative nuclear magnetic resonance (qNMR) is a standard technique for determining analyte concentrations.
  • Conventional qNMR requires mixing analytes with reference substances, which can alter sample properties.
  • Coaxial-tube NMR offers a way to analyze separate solutions but lacks a standardized protocol.

Purpose of the Study:

  • To establish an effective volume ratio (EVR) measurement method for coaxial-tube qNMR.
  • To develop a general analytical protocol for coaxial-tube qNMR.
  • To enable accurate quantification of analytes without sample alteration.

Main Methods:

  • Development of an effective volume ratio (EVR) measurement method combining weight density and qNMR.
  • Utilizing coaxial tubes with varying diameters for qNMR analysis.
  • Employing an SI-traceable reagent for accurate concentration determination.

Main Results:

  • An effective volume ratio (EVR) measurement method was successfully established for coaxial-tube qNMR.
  • The method achieved a coefficient of variation (CV) of <1% for inner tubes ≤3 mm.
  • Accurate quantification of various analytes, including hygroscopic substances, was demonstrated.
  • Coaxial tubes were shown to prevent pH and structural changes by eliminating the need for mixing.

Conclusions:

  • Coaxial-tube qNMR, with the established EVR method, provides a reliable and non-invasive quantification technique.
  • Understanding peak-specific partial structural characteristics and T1 relaxation times is crucial for accurate qNMR.
  • This method allows for the reuse of analytes, enhancing efficiency in analytical testing.