Determination of standard sample purity using the high-precision 1H-NMR process.

This paper discusses the technique for high-precision quantification using (1)H-NMR to determine the purity of analytical standard samples. The procedure described is based on the use of internal reference samples in an (1)H NMR experiment in our laboratories. The sample preparation and all relevant NMR parameters were optimized for minimum uncertainty. The validation of accuracy and precision was performed by comparing different certified reference materials. It was shown that the high-precision measurement is applicable even for relatively small sample amounts down to 2.5 mg. The relative combined uncertainty of measurement was found to be 0.15%. Two different approaches for uncertainty calculation were compared; a complete uncertainty budget was calculated.