CHROMATOGRAPHY, Vol. 24 (2003), No. 3, pp. 117-120
Evaluation of Accuracy for the Quantitative Analysis Using Nuclear Magnetic Resonance as a Detector of HPLC
Takeshi Saito*, Ryoko Iwasawa, Toshihide Ihara, Shinichi Kinugasa, Akira Nomura and Tsuneaki Maeda
National Metrology Institute of Japan, AIST Higashi 1-1-1, Tsukuba Central 5-2, Tsukuba, Ibaraki 305-8565, Japan
Continuous.flow LC.NMR technique was applied for the purity assessment of o.xylene. Two consecutive LC.NMR runs of a sample and a standard were measured. The purity was calculated by the ratio of the set of data. With such an approach, sources of NMR problems were overcome because identical condition can be obtained for both the standard and the sample during NMR measurements. As a result, significant reduction of dispersion and considerable improvement of accuracy in the results were obtained compared to the previous work reported. Comparison of the result of purity assessment obtained with LC.NMR to GC.FID and differential scanning calorimeter (DSC) showed excellent agreement. With such an NMR experimental condition, on.flow NMR can provide accurate and precise results as a detector of HPLC.