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Measuring Number of Free Radicals and Evaluating the Purity of Di(phenyl)-(2,4,6-trinitrophenyl)iininoazaniuin [DPPH] Reagents by Effective Magnetic Moment Method

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Abstract

Di(phenyl)-(2,4,6-trinitrophenyl)iminoazanium [DPPH] is widely used as a standard for measuring the number of free radicals. Here, we evaluated the number of free radicals of “DPPH” reagents from three manufacturers by effective magnetic moment method. Interestingly, the reagents from different manufacturers had varying temperature dependencies for both magnetic moment and g-value at low temperatures. As a result, the maximum relative difference among the three reagents on the number of free radicals per unit mass was 20%. Carbon hydrogen nitrogen (CHN) analyses, highresolution EPR measurements, FT-IR measurement, and NMR measurement confirmed that a major component of only one among the three reagents was “pure” DPPH. The evaluated purity based on free radical content was 0.998 kg kg–1 with expanded uncertainty of 0.036 kg kg–1. The other two reagents were found to be contaminated by several % of benzene in the DPPH crystal structure.

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Acknowledgments

A major part of this work was conducted at the Institute for Molecular Science, National Institutes of Natural Sciences, supported by the Nanotechnology Platform Program (Molecule and Material Synthesis) of the Ministry of Education, Culture, Sports, Science and Technology (MEXT), Japan. Part of the SQUID measurements was conducted at the AIST Nano- Processing Facility, supported by the Nanotechnology Platform Program of the same ministry. The authors would like to thank Dr. K. Yamazaki (AIST) for the NMR measurements. An Excel macro program formulated by Dr. T. Shimosaka (AIST) was used for data fitting of magnetic moment via least-squared method. This work was supported by JSPS KAKENHI Grant Number JP17K05918.

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  1. National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), AIST Central-3 I-1-1 Umezono, Tsukuba, Ibaraki, 305-8563, Japan

    Nobuhii O. Matsumoto & Nobuyasu Itoh

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  1. Nobuhii O. Matsumoto
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  2. Nobuyasu Itoh
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Correspondence to Nobuhii O. Matsumoto.

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Matsumoto, N.O., Itoh, N. Measuring Number of Free Radicals and Evaluating the Purity of Di(phenyl)-(2,4,6-trinitrophenyl)iininoazaniuin [DPPH] Reagents by Effective Magnetic Moment Method. ANAL. SCI. 34, 965–971 (2018). https://doi.org/10.2116/analsci.18P120

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  • DOI: https://doi.org/10.2116/analsci.18P120

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