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Structure Verification of molecules in Protonated Solvents

Structure Verification of molecules in Protonated Solvents Structure verification and elucidation using NMR is a routine analysis in many synthetic laboratories, where chemists collect and analyze a suite of 1D and 2D NMR experiments to confirm they have indeed synthesized their desired products, or to elucidate the structure of unexpected side products in their reactions. …

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Transesterification of Pinacol Arylboronic Ester – How to monitor heterogeneous reactions online by benchtop NMR

A growing application for Spinsolve benchtop NMR spectrometers is reaction monitoring, where chemists can follow their reactions on-line and get real-time feedback about the reaction progress, observe short-lived intermediates, or detect other physical and chemical changes in the reaction mixture. The implementation of closed-loop sample transfer systems to follow chemical reactions with homogenous liquid mixtures …

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Can benchtop NMR detect 15N at natural abundance?

Can benchtop NMR detect 15N at natural abundance? Nuclear magnetic resonance (NMR) relies on powerful multidimensional and multinuclear experiments such as COSY, HSQC, and HMBC, among others, to obtain useful information for molecular structure verification and elucidation. These methods are routinely collected on high-field NMR systems to explore and confirm the couplings between homo and …

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Honey Adulteration and Floral Origin Analysis by benchtop NMR spectroscopy

Natural honey is considered of high nutritional value and consumed every day in households and food industry. The market demand for honey far exceeds global production. The EU, for example, being the second largest honey producer in the world, is only approximately 60 % self-sufficient. This motivated honey fraud, such as mislabelling or adulteration with …

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Let your NMR signal shine – Automated photoCIDNP experiments with a Spinsolve benchtop NMR

Several hyperpolarization techniques have emerged over the past few decades to address the sensitivity limitations of NMR. Among these techniques, Photochemically Induced Dynamic Nuclear Polarization (photoCIDNP) is one of the easiest to implement. In a simplistic way, all what is needed to enhance the signal in a photoCIDNP experiment is the addition of a photosensitizer …

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Monitoring the deuteration of cinnamyl alcohol in a flow reactor with a Spinsolve Benchtop NMR

Introduction In previous blog posts, we have reported on the potential of using a Spinsolve benchtop NMR spectrometer to monitor on-line different hydrogenations conducted on an H-Cube® Pro flow reactor. here. As a follow-up, in this application note, we demonstrate how straightforward it is to perform deuteration reactions employing the H-Cube Pro® flow reactor. This …

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Molecular weight determination of silicone oils via 29Si on Spinsolve NMR systems

In both academic polymer research and industrial polymer production, it is crucial to regulate the molecular weight of polymers. This necessity arises from the fact that the macroscopic properties of polymers are predominantly dictated by their molecular structure and chain length. Therefore, understanding the molecular weight itself becomes imperative. While size-exclusion chromatography (SEC) is frequently …

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Optimizing a two-step hydrogenation reaction in a flow reactor using a Spinsolve Benchtop NMR

Introduction In a recent blog post, we demonstrated that coupling a Spinsolve benchtop NMR spectrometer to a continuous flow reactor can dramatically accelerate the optimization of the reaction parameters. Benchtop NMR spectroscopy provides online access to quantify the reaction conversion in real time as the reaction parameters are adjusted. The example chosen to test the …

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Quantifying residual solvents in active pharmaceutical ingredients

Detecting residual solvents in pharmaceutical processes is crucial for pharmacopeial purposes. First, it ensures product quality by confirming that harmful or unwanted solvents are removed or below risk levels, preventing potential health hazards. Second, regulatory compliance often mandates limits on residual solvents to ensure product safety. Additionally, understanding and controlling solvent levels contribute to process …

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Determining the molecular weight of polymers by Pulsed Field Gradient NMR on a Spinsolve 80 MHz

Molecular weight plays a critical role defining the physical properties of a polymer, like mechanical strength, degradation rate, and solubility. The two methods most commonly used method for determining molecular weight are size exclusion chromatography (SEC) and end group analysis, which are frequently employed to measure the number-averaged molecular weight (Mn) of a polymer. However, …

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