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A 1 μL aliquot of a sample containing a mixture of cis- and trans-4-methylcyclohexanols (0.125 μg/μL for each) was measured using a gas chromatograph (GC) combined with a quadrupole EI–MS (GCMS-QP2010..., Shimadzu, Kyoto, Japan). These stereoisomers were obtained from Tokyo Chemical Industry and were used as different chemicals because of a large enthalpy change for transition (ΔH_t = 1.7 ± 0.5 kJ mol^<–1>). (26) The temperature of the sample injection port was set at 250 °C and was used as the splitless mode. The flow rate of helium was adjusted at 1 mL/min. The analyte was separated using a DB-5 ms column (length 30 m, inner diameter 0.25 mm, and film thickness 0.25 μm). The temperature program of the GC oven was as follows; the initial temperature of the capillary column was 50 °C and was held for 1 min, a ramp of 25 °C/min to 125 °C, and then the temperature was increased to 200 °C at a rate of 8 °C/min and was finally held for 10 min. The electron energy was set at 70 eV. The temperatures of the ion source and the interface between the GC and MS were kept at 230 and 280 °C, respectively. 質量分析において、フラグメント化を抑制させることは重要である。シスとトランスの4-メチルシクロヘキサノールに対して可変紫外と近赤外フェムト秒レーザー(35 fs)をイオン化光源として用いる研究を行った。続きを見る
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