title: Synchronized and concurrent experiments in Moving Tube NMR: using separate sample volumes for different pulse sequences.
abstract: This study presents a new application of sample shuttling with a long NMR tube (Moving Tube NMR, MT-NMR) as a method for collecting different experiments synchronously or even concurrently using separate sample regions. Synchronized experiments were performed using an automated shuttling apparatus to move different sample regions into the coil between transients such that each experiment was collected using a separate, specific sample segment. Additionally, a 2D NOESY spectrum and a double quantum filtered COSY (DQCOSY) spectrum were collected concurrently by shuttling between two different sample regions during the NOESY mixing time. These applications of the Moving Tube technique show that it is a useful platform for compounded data acquisition to optimize spectrometer time by minimizing measurement times and avoiding problems arising from instrument and sample instabilities. Furthermore, collecting a DQCOSY during a 2D NOESY mixing time opens a wide array of possibilities, as this principle can be applied to collect any experiment during a NOESY mixing time provided that the mixing period is longer than the sum of the sample shuttling time plus a complete scan of the intermittent experiment. While this methodology relies on the use of a long sample tube, it does not require excessive sample volumes, as two milliliters is enough to constitute multiple sample regions.
authors.affiliation: Department of Chemistry, University of California, Irvine, CA 92697-2025, USA. Electronic address: kjd@mit.edu.
authors.forename: Kevin J
authors.initials: KJ
authors.lastname: Donovan
mesh_terms: D004574:Electromagnetic Fields; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000295:instrumentation* / Q000379:methods*; D011789:Quantum Theory
keywords: Concurrent experiments; DQCOSY; Double quantum filtered COSY; HMBC; HSQC; MT-NMR; Moving Tube; Multiplexing; NOESY; Sample shuttling; Synchronized experiments