Study of Sample Preparation Method Using Internal Standard Solution to Accurate Quantitative Analysis with 1H NMR Spectroscopy

Since nuclear magnetic resonance (NMR) spectroscopy obtains a quantitative value on the basis of a nucleus, the quantitative NMR technique does not require an identical standard. For this reason, it is expected to be a universal quantitative method. Recently, the quantitative NMR method was adopted also as a regulating method. However, the quantification using an NMR requires a high-resolution balance in the sample preparation for accurate weighing of the mass of samples. This is the biggest problems to disseminate a quantitative NMR as a generally used method. In this paper, we discuss the quantitative NMR method using the internal standard solution in order to resolve the problem. We examined two methods of sample preparation: the gravimetric method and the volumetric method. The influence of the preparation method and condition was evaluated using a standard solution. Additionally, some organizations have used this method to measure the purity of a high-purity reference material for the validation of this standard solution method. The accuracy of the results was evaluated using an internal standard solution by the volumetric method, and measured at 1 % or less.