Analytical Sciences

Abstract − Analytical Sciences, 34(8), 965 (2018).

Measuring Number of Free Radicals and Evaluating the Purity of Di(phenyl)-(2,4,6-trinitrophenyl)iminoazanium [DPPH] Reagents by Effective Magnetic Moment Method
Nobuhiro MATSUMOTO and Nobuyasu ITOH
National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), AIST Central-3, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan
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, high-resolution 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.