Cosa - Ai-60 - Aspect Brochure

The use of an NMR as a simple flow detector for bench top reaction monitoring, mixing monitoring, dilution monitoring, or conversion monitoring has been limited by the need to bring the "reaction" to the typical "supercon" NMR lab. With the Aspect AI-60 system continuous flow NMR can be now be performed “at the bench.” The system uses a high resolution 60 MHz permanent magnet with a simple flow cell and total system volumes of 2 to 5 ml depending on the length and diameter of the transfer tubing. Further, detection limits of analytes in the 200+ ppm range are possible without the use of typical deuterated NMR solvents. Analysis times of 5 to 20 seconds are achieved at flow rates of 1 to 20+ ml/minute. Here are examples of the data visualization and rapid reaction profiling at 60 MHz the reaction for the esterification of tert-butanol with acetic anhydride in the presence of acid obtained every 10 seconds (1 pulse) over the course of 25 minutes. The full width spectral plots in the upper right figure show the entire 25 minute reaction. As can be seen, the time dependent spectral changes are followed as the conversion reaction proceeds. In these spectra, the pH dependent change in the hydroxyl (OH) protons are readily observed. In the figure to the immediate right the expansion plots corresponding to the CH3 region of the 1H NMR spectrum are shown. Peak assignments corresponding to the constituents of the reaction are given. Excellent resolution of each CH3 resonance from each constituent in the reaction (t-butyl alcohol, acetic anhydride, t-butyl methyl ester, and, acetic acid) are well resolved. Integration of each peak allows quantitative determination of each constituent’s concentration over the course of the entire reaction. As shown in the lower right figure, reaction kinetics can be determined. The Aspect AI-60 system’s small footprint, high sensitivity, excellent resolution, and automated processing routines enable new opportunities and applications for reaction monitoring by NMR. 1H NMR Reaction Monitoring at 60 MHz Application Note AI-01 Aspect AI-60 60 MHz High Resolution FT-NMR System for Laboratory and At-Line Applications COSA Xentaur 84F Horseblock Rd 11980 Yaphank, NY Tel: +203-744-5905 paul@process-nmr.com www.cosaxentaur.com Advantages The Aspect AI-60’s permanent magnet design requires no cryogens as the system is powered by one standard wall outlet (110/220v). Samples can be run neat, in conventional protonated solvents, or, in deutertated NMR solvents. Deueterated solvents are not required. Probes accept standard 5 mm or 10 mm NMR tubes. Flow cell options are also available. Software operates under Windows® 7 or Windows® XP. Complete automation of all NMR tasks (Acquisition, Processing, Integration, Results Reporting) enable walk-up applications with minimum user training and/or experience. Spectral processing facilitates use of a variety of chemometric based routines for multiple property measurements. Specifications Field Strength at 45oC 1.4 Tesla Fringe Field Less than 1 gauss Clear Bore Size 30 mm diameter Operating Frequency 60.1± 1MHz 1H 54.6 ± 1MHz 19F 24.3 ± 1MHz 31P Dimensions (HxWxD) 37.5 x 22 x 24 inches 560 x 460 x 460 mm Weight ~325 lbs ~160 Kg Lab Probes 5 mm, 10 mm, and, Flow Through Non-Spin Resolution Less than 4 Hz at half height and less than 20 Hz at 1/10 height Line Shape (5 mm) Less than 80 Hz at the average peak height of 13C satellites (0.55%) 1H Sensitivity >25:1 (S/N), 1 pulse, 1% ethyl- benzene (CH3) in CDCl3 1H Pulse <20 µsec 90o flip angle at 7 watt RF power for 5mm probe (Q of 150)