Standard Reference Material for qNMR

NMR (Nuclear Magnetic Resonance) has been broadly used as a standard analysis method for structural determination of an organic compound. In NMR analysis, the ratio of the number of atomic nuclei in a compound corresponds to the ratio of the areas of the peaks in the spectrum. Therefore, the purity of the compound can be determined by performing a quantitative analysis.
In a purity determination using 1H NMR, a sample and a standard (an internal standard) having a known purity are mixed together and dissolved in a deuterated solvent. A quantitative value of the sample's purity can be calculated from the relationship among the areas of the spectral peaks originated from the sample and the standard, the number of protons, the prepared masses, and the molecular weights of the sample and the standard using Formula 1.

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In quantitative analysis using 1H NMR (quantitative NMR), the areas of the peaks of hydrogen atoms observed in the spectrum can be quantitatively compared. Therefore, determination of the purity and quantity of many compounds containing a hydrogen atom is possible with one standard as long as the signals of the sample and the standard do not overlap each other. Highly reliable purity and quantity measurement based on the amount of substance (moles) is possible using a standard certified to be traceable to the International System of Units (SI).

Features

  • Reliability:
    Absolute quantitation method with SI (International System of Unites) traceability)
  • Quickness:
    Calibration curve for quantitation is not required
  • Efficiency:
    It’s possible to quantify all materials by only one CRM for qNMR: Certified Reference Material for qNMR.

Official analytical method

  • The Japanese Pharmacopoeia
    The Japanese Pharmacopoeia 16th Ed., Supplement II (Feb. 2014) Geniposide, Peonol, Magnol and Magnoflorine iodide
  • Japan’s Specifications and Standards for Food Additives
    Specifications and Standards for Food and Food Additives (Ministry of Health, Labor and Welfare: Notification No.307, 011) (issued on August 31,2011) Azoxystrobin, Pyrimethanil and Fludioxonil

Internal Standards for qNMR

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As a producer of internal standards for quantitative NMR, we acquired accreditation by the ASNITE (Accreditation System of the National Institute of Technology and Evaluation) accreditation program operated by the National Institute of Technology and Evaluation (NITE / IA Japan), and provide the standards as certified reference materials (TraceSure).
The certification gives an uncertainty value as proof of reliability and is attached to every ASNITE accredited and certified reference standard. The certified value described in the certification is internationally accepted through a mutual recognition agreement of APLAC (the Asia Pacific Laboratory Accreditation Cooperation).
We determine a characteristic value of the standard by adding uncertainty obtained from our uniformity evaluation, stability evaluation, etc. to the value of purity (including uncertainty) obtained with a measurement method that is traceable to International System of Units (SI) by the National Metrology Institute of Japan (NMIJ), and we provide the internal standard for quantitative NMR as a reference standard with a certification. Therefore, the characteristic value of the reference standard is traceable to SI through the NMIJ analysis value, and the traceability of the measurements can be shown.

NOTE: TraceSure is our series of standards accredited by ASNITE "Reference material producer accreditation" from NITE. ASNITE: Accreditation system of NITE. Accreditation System of National Institute of Technology and Evaluation.

CRMs for qNMR

Internal Standard for Quantitative NMR

1H NMR Spectrum (NOTE: The chemical shift may vary to some degree depending on conditions.)

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Solubility (1,000 ppm each when dissolving)

Maleic Acid Dimethyl Sulfone 1,4-BTMSB-d4 DDS-d6
Acetone-d6 ×
CDCl3 × ○* ×
D2O ×
DMSO-d6
CD3OD ○*
CD2Cl2 × ×

* There are possibilities they will be decompose in detreated solvents.

Experimental Scheme

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Internal Standards for Quantitative NMR

Standard Solutions for Quantitative NMR

Solvents for Quantitative NMR [High purity NMR solvent with peaks from impurities suppressed]

NMR Test Tubes

National Metrology Institute of Japan - Certified Reference Materials -

Standard for qNMR

Product content may differ from the actual image due to minor specification changes etc.

Author: T. Miura

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