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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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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Demonstrating the comparability of certified reference materials.

David L Duewer1, Katrice A Lippa, Stephen E Long

  • 1Analytical Chemistry Division, National Institute of Standards and Technology (NIST), 100 Bureau Drive, Stop 8390, Gaithersburg, MD 20899-8390, USA. david.duewer@nist.gov

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This summary is machine-generated.

Certified reference materials (CRMs) ensure measurement comparability. New methods assess if different CRMs provide equivalent results, enhancing the reliability of laboratory measurements and traceability.

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Area of Science:

  • Metrology
  • Analytical Chemistry
  • Clinical Laboratory Science

Background:

  • Certified reference materials (CRMs) are crucial for comparing measurement results across different times and locations.
  • Metrological traceability is established when CRMs calibrate or verify measurement systems.
  • Comparing results from systems using different CRMs necessitates that these materials are equivalent for the same measurand within stated uncertainty.

Purpose of the Study:

  • To detail experimental and data analysis techniques for establishing and demonstrating material comparability.
  • To develop tools for ensuring the reliability of clinical laboratory measurements.

Main Methods:

  • Uniform interpretation of CRM uncertainty statements.
  • Estimation of consistent measurement system response uncertainties from varied experimental designs.
  • Application of "errors-in-variables" analysis for comparability studies.
  • Development of graphical tools for communicating evaluation results.
  • Augmentation of comparability studies with new materials using certifying institution data.

Main Results:

  • Experimental and data analytic tools were developed to evaluate the comparability of different CRMs.
  • These methods address challenges in interpreting uncertainty statements and handling inconsistent experimental designs.
  • Novel graphical tools facilitate communication of comparability study outcomes.

Conclusions:

  • The developed techniques enhance the ability to establish and demonstrate the comparability of materials.
  • These tools support the Joint Committee for Traceability in Laboratory Medicine's goal of improving clinical laboratory measurement reliability.
  • The methods are applicable to any group of materials delivering the same nominal measurand, including clinical analytes like potassium and cholesterol.