The derivatives of the reaction liquid for synthesizing N-（phosphonomethyl） iminodiacetic acid （PMIDA） were synthesized with 9-fluorenyl methyl chlomformate （FMOC-C1） as the derivatization reagent. The separatio...The derivatives of the reaction liquid for synthesizing N-（phosphonomethyl） iminodiacetic acid （PMIDA） were synthesized with 9-fluorenyl methyl chlomformate （FMOC-C1） as the derivatization reagent. The separation of the derivatives was performed on a Gemini C18 column at room temperature by isocratic elution. The mobile phase was composed of 60% 0.05 M Nail2 PO4 （pH = 3.5） and 40% CH3 CN at a flow rate of 1 ml/min. The injection volume was 10 td, and the detection wavelength was 265 nm. The linear ranges of the derivatives of iminodiacetonitrile, iminodiacetic acid （IDA） and ammonia were, respectively, 0.02-1.2, 0.02-1.2 and 0.1 -2. 0 mg/ml with correlation coefficients not smaller than 0. 999 8. The detection limits for the derivatives were, respectively, 0. 000 4, 0. 000 4 and 0.003 mg/ml. The average recoveries of 3 derivatives were respectively 99.96%, 99. 86% and 99.89%, respectively, with relative standard deviation values not smaller than 1.6%. The method developed in the present paper could be used for monitoring the reaction system for preparation of PMIDA by IDA.展开更多
High-quality poly（N-（9-fluorenylmethoxycarbony）-glycine） （PFG）, a new kind of soluble polyfluorene deriva- tive, was successfully synthesized electrochemically by direct anodic oxidation of N-（9-fluorenylmethox...High-quality poly（N-（9-fluorenylmethoxycarbony）-glycine） （PFG）, a new kind of soluble polyfluorene deriva- tive, was successfully synthesized electrochemically by direct anodic oxidation of N-（9-fluorenylmethoxycar- bony）-glycine （FG） in boron trifluoride diethyl etherate （BFEE）. The onset oxidation potential of FG in BFEE was only 0.6 V vs. Pt, which was much lower than that in acetonitrile ＋0.1 mol/L tetrabutylammonium tetrafluoro- borate （TBATFB）. PFG film obtained from BFEE showed good electrochemical activity and thermal stability. It in- dicates that BFEE is a better medium for the electrosynthesis of PFG film. PFG is highly soluble in common or- ganic solvents, facilitating potential applications as a blue-light-emitting material. Fluorescent spectra revealed that PFG was a good blue-light emitter. Results of FT-IR and IH NMR spectra indicated the polymerization location of N-（9-fluorenylmethoxycarbony）-glycine occurred mainly at C（2） and C（7） positions of the fluorine ring.展开更多
文摘The derivatives of the reaction liquid for synthesizing N-（phosphonomethyl） iminodiacetic acid （PMIDA） were synthesized with 9-fluorenyl methyl chlomformate （FMOC-C1） as the derivatization reagent. The separation of the derivatives was performed on a Gemini C18 column at room temperature by isocratic elution. The mobile phase was composed of 60% 0.05 M Nail2 PO4 （pH = 3.5） and 40% CH3 CN at a flow rate of 1 ml/min. The injection volume was 10 td, and the detection wavelength was 265 nm. The linear ranges of the derivatives of iminodiacetonitrile, iminodiacetic acid （IDA） and ammonia were, respectively, 0.02-1.2, 0.02-1.2 and 0.1 -2. 0 mg/ml with correlation coefficients not smaller than 0. 999 8. The detection limits for the derivatives were, respectively, 0. 000 4, 0. 000 4 and 0.003 mg/ml. The average recoveries of 3 derivatives were respectively 99.96%, 99. 86% and 99.89%, respectively, with relative standard deviation values not smaller than 1.6%. The method developed in the present paper could be used for monitoring the reaction system for preparation of PMIDA by IDA.
文摘High-quality poly（N-（9-fluorenylmethoxycarbony）-glycine） （PFG）, a new kind of soluble polyfluorene deriva- tive, was successfully synthesized electrochemically by direct anodic oxidation of N-（9-fluorenylmethoxycar- bony）-glycine （FG） in boron trifluoride diethyl etherate （BFEE）. The onset oxidation potential of FG in BFEE was only 0.6 V vs. Pt, which was much lower than that in acetonitrile ＋0.1 mol/L tetrabutylammonium tetrafluoro- borate （TBATFB）. PFG film obtained from BFEE showed good electrochemical activity and thermal stability. It in- dicates that BFEE is a better medium for the electrosynthesis of PFG film. PFG is highly soluble in common or- ganic solvents, facilitating potential applications as a blue-light-emitting material. Fluorescent spectra revealed that PFG was a good blue-light emitter. Results of FT-IR and IH NMR spectra indicated the polymerization location of N-（9-fluorenylmethoxycarbony）-glycine occurred mainly at C（2） and C（7） positions of the fluorine ring.
