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400 mr dd2 nmr spectrometer

Manufactured by Agilent Technologies

The 400-MR DD2 NMR spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It provides high-resolution NMR spectroscopy capabilities for the identification and characterization of chemical compounds.

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4 protocols using 400 mr dd2 nmr spectrometer

1

NMR and Mass Spectrometry Analysis

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1H-NMR spectra were collected on an Agilent 400-MR DD2 NMR spectrometer. Chemical shifts were reported in ppm using tetramethylsilane as an internal standard. HPLC/ESI-MS analysis of the purified compound was carried out on a Thermo Electron LTQ-Orbitrap XL mass spectrometer connected to an Agilent HP 1100 HPLC system. All solvents used were of analytical grade purchased from J. T. Baker.
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2

Structural Analysis of MOF Crystals

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All reagents were purchased from commercial sources and used without further purification. PXRD data (2θ angle) were recorded using a Bruker D2 Phaser automated diffractometer at room temperature with a step size of 0.02°. 1H NMR spectra were obtained using an Agilent 400-MR DD2 NMR spectrometer operating at 400 MHz for 1H. Raman mapping was performed with a WITec alpha300 R Confocal Raman microscope equipped with a 532 nm laser and a 600 g/mm grating. Data analysis was conducted using WITec Project 2.10. Cold field-emission SEM (Cold FE-SEM) was performed using a Hitachi SU-8220 at an accelerating voltage of 15 kV. EDS elemental mapping images were captured using an Octane Elect EDS system (Ametek EDAX) to confirm the distribution of metallic elements. MOF crystals were epoxy-fixed at 70 °C overnight and cut with an EM UC7 ultramicrotome (Leica) prior to the SEM and EDS analyses.
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3

Proton NMR Spectroscopy of Analyzed Complexes

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Proton NMR
spectra were collected in 5 mm outside diameter NMR tubes on an Agilent
400MR DD2 NMR spectrometer operating in the pulse Fourier transform
mode. Calibrated autopipettes were used to prepare solutions that
were nominally 2–5 mM for variable temperature NMR measurements
by dissolution of elementally analyzed complexes. The sample temperature
was maintained by blowing chilled nitrogen over the NMR tube in the
probe. Proton chemical shifts were measured relative to the internal
solvent but are reported relative to tetramethylsilane. Coupling constants
are reported in hertz. Line—fitting analyses were performed
with Acorn NMR Utility Transform Software.55
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4

NMR Analysis of nBA Compounds

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Proton
NMR spectroscopy was used for all nBA compounds to
check the successful synthesis of the compounds with the formation
of amide groups. 1H NMR spectra were recorded on an Agilent
400-MR DD2 NMR spectrometer equipped with a 5 mm ONE NMR
Probe. The nBA compounds were dissolved in DMSO-d6 (dimethyl sulfoxide d6) 5 wt % at 80 °C, and tetramethylsilane (TMS) was used
as an internal reference. The resolution of the spectra was compromised
due to the poor solubility of nBA compounds in almost
any solvent.
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