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Determination of PAHs in Solution with a Single Reference Standard by a Combination of 1H Quantitative NMR Spectroscopy and Chromatography

Kitamaki, Yuko, Saito, Naoki, Yamazaki, Taichi, Otsuka, Satoko, Nakamura, Satoe, Nishizaki, Yuzo, Sugimoto, Naoki, Numata, Masahiko, Ihara, Toshihide
Analytical chemistry 2017 v.89 no.13 pp. 6963-6968
benzo(a)pyrene, chromatography, nuclear magnetic resonance spectroscopy, polycyclic aromatic hydrocarbons, reference standards, uncertainty
We have applied a combination of ¹H quantitative NMR spectroscopy (¹H-qNMR) and chromatography (GC or LC) to establish reliable analytical methods (qNMR/GC and qNMR/LC) for organic compounds. In this method, a reference standard is used as an internal standard for both ¹H-qNMR and chromatography to estimate relative molar sensitivity (RMS) for analytes. The RMS values are calculated from the molar ratios between analytes and the reference standard obtained by ¹H-qNMR; and the response ratio between them obtained by chromatography. Concentrations of analytes in the organic solution can be simultaneously determined from the RMS and amount of the reference standard added in the sample solution. This analytical method is an innovative one because only one reference standard with International System of Units (SI)-traceable property value, purity, or concentration, is necessary to determine accurate concentrations of multiple organic components in organic solutions, without the respective certified reference standards for various analytes. To verify this method, a certified reference material, NIST SRM 1647f, was used. Among the 16 polycyclic aromatic hydrocarbons (PAHs) included in NIST SRM 1647f, naphthalene and benzo[a]pyrene were selected as analytes for this method, using 1,4-bis(trimethylsilyl)benzene-d₄ as the reference standard. Each quantitative value obtained by qNMR/GC and qNMR/LC agreed with each certified value within its expanded uncertainty.