Industrial & Engineering Chemistry Research
Industrial & Engineering Chemistry Research
5 years ago

Real-Time Mass Spectrometric Analysis of Hydrothermal Reaction Products

Real-Time Mass Spectrometric Analysis of Hydrothermal Reaction Products
Yukihiko Matsumura, Takahisa Tajima, Yutaka Nakashimada, Yoshiko Okamura, Tsunehiro Aki, Shuhei Inoue, Pattasuda Duangkaew
This is the first work that describes the application of mass spectrometry to the real-time observation of liquid products of hydrothermal reactions in a continuous reactor. A real-time mass spectrometric analysis (real-time MS analysis) system was developed and designed to elucidate products of glucose decomposition during the hydrothermal treatment process. This was achieved by connecting a continuous-flow reactor with a quadrupole mass analyzer using custom-built connection fittings. The effects of residence time and temperature of hydrothermal treatment on glucose decomposition products were investigated. The temperatures were between 140 and 220 °C, and reaction times were between 5 and 20 min. The real-time MS method investigated the products of glucose decomposition, and cold samples were characterized using high-performance liquid chromatography (HPLC). At 140 °C, glucose decomposition is not complete, which was confirmed by a mass spectrum of a glucose standard. At a temperature of 180 °C or above, fragmentation peaks of fructose at m/z = 131 and 149, ring compound products like 5-hydroxymethylfurfural (5-HMF) at m/z = 97 and 126, and furfural at m/z = 96 and 67 were obtained. Retro-aldol products like glyceraldehyde and glycolaldehyde were also observed, confirmed by m/z = 90, 72, and 61 and an increasing ion current at m/z = 60, 29, and 31, respectively. No fructose was observed using a conventional HPLC at 200 °C for 10 min. The effectiveness of real-time MS analysis is strong, collated with a conventional HPLC method.

Publisher URL: http://dx.doi.org/10.1021/acs.iecr.7b02663

DOI: 10.1021/acs.iecr.7b02663

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