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

YAMAZAKI Taichi, OHTSUKI Takashi, MIURA Toru, SUEMATSU Takako, HORINOUCHI Takaaki, MURAKAMI Masayo, SAITO Takeshi, IHARA Toshihide, TADA Atsuko, TAHARA Maiko, GODA Yukihiro, AKIYAMA Hiroshi, NAKAO Shinji, YAMADA Yuko, KOIKE Ryo, SUGIMOTO Naoki

doi:10.2116/bunsekikagaku.63.323

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<sup>1</sup>H NMRによる精確な定量分析のための内標準液を用いる試料調製法の検討
¹H NMRによる精確な定量分析のための内標準液を用いる試料調製法の検討
¹ H NMR ニヨルセイカクナテイリョウブンセキノタメノナイヒョウジュンエキオモチイルシリョウチョウセイホウノケントウ

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Abstract

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.

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BUNSEKI KAGAKU

BUNSEKI KAGAKU 63 (4), 323-329, 2014

The Japan Society for Analytical Chemistry

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