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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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Mass Spectrometry: Isotope Effect01:13

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Most elements exist in nature as a mixture of isotopes. The isotopes differ in weight due to their respective number of neutrons. The molecular weight of a molecule is different depending on the specific isotope of its elements involved. As a result, the mass spectrum of the molecule exhibits peaks from the same fragment at multiple positions. The positions of these mass signals depend on the difference between the molecular mass. Furthermore, the intensity of these signals is dependent on the...
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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.
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Noble Gases02:54

Noble Gases

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The elements in group 18 are noble gases (helium, neon, argon, krypton, xenon, and radon). They earned the name “noble” because they were assumed to be nonreactive since they have filled valence shells. In 1962, Dr. Neil Bartlett at the University of British Columbia proved this assumption to be false.
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Isotopes and Radioisotopes01:28

Isotopes and Radioisotopes

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In the early 1900s, English chemist Frederick Soddy realized that an element could have atoms with different masses that were chemically indistinguishable. These different types are called isotopes — atoms of the same element that differ in mass. Isotopes differ in mass because they have different numbers of neutrons but are chemically identical because they have the same number of protons. Soddy was awarded the Nobel Prize in Chemistry in 1921 for this discovery.
An isotope containing...
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The Equilibrium Constant03:10

The Equilibrium Constant

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Consider the oxidation of sulfur dioxide:
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Automated, High-resolution Mobile Collection System for the Nitrogen Isotopic Analysis of NOx
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Isotopically characterised N2 O reference materials for use as community standards.

Joachim Mohn1, Christina Biasi2, Samuel Bodé3

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New nitrous oxide (N2O) isotope reference materials (RMs) were developed to improve source identification. These RMs enhance data accuracy and laboratory compatibility for N2O isotope analysis.

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Area of Science:

  • Environmental Science
  • Analytical Chemistry
  • Isotope Geochemistry

Background:

  • Understanding nitrous oxide (N2O) sources and sinks relies on its isotopic composition.
  • Advancements in mass spectrometry and laser spectroscopy for N2O analysis require reliable isotope reference materials (RMs).

Purpose of the Study:

  • To develop and characterize a set of N2O isotope reference materials (RMs).
  • To establish robust N2O isotope reference scales for improved source apportionment and analytical accuracy.

Main Methods:

  • Seven pure N2O isotope RMs were synthesized and analyzed for 15N/14N, 18O/16O, 17O/16O ratios, and 15N site preference (SP).
  • Specialized laboratories performed analyses, focusing on site-specific isotopic composition, linking measurements to existing isotope reference materials.

Main Results:

  • The N2O RMs exhibit a wide range of delta (δ) values: δ15N (0 to +104‰), δ18O (+39 to +155‰), and δ15NSP (-4 to +20‰).
  • Robust estimates for δ15N(N2O) and δ18O(N2O) were achieved with uncertainties of ~0.05‰ and ~0.15‰, respectively.
  • An offset of >1.5‰ was detected for δ15NSP compared to previous calibrations, highlighting the need for further investigation.

Conclusions:

  • A set of seven N2O isotope RMs anchored to international scales was successfully developed.
  • These RMs will facilitate the implementation of recommended two-point calibration and improve data quality for N2O isotope analysis.
  • The availability of δ17O data is expected to enhance δ15NSP and δ15N measurements, fostering inter-laboratory compatibility and research advancement.