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Mercury nmr spectrometer

Manufactured by Agilent Technologies

The Mercury NMR spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It employs a superconducting magnet to generate a strong magnetic field, allowing for the detection and analysis of nuclear magnetic resonances in samples. The core function of the Mercury NMR spectrometer is to provide high-resolution spectroscopic data for the identification and characterization of chemical compounds.

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7 protocols using mercury nmr spectrometer

1

Characterization of Organic Compounds

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Melting points were measured with a Stuart melting point apparatus and were uncorrected. Infrared (IR) Spectra were recorded as KBr disks using Schimadzu FT-IR 8400 S spectrophotometer. Mass spectral data are given by GCMS-QP1000 EX spectrometer at 70 e.V. NMR Spectra were recorded on a Varian Mercury NMR spectrometer. 1H spectrum was run at 400 MHz and 13 C spectrum was run at 100 MHz in deuterated dimethylsulfoxide (DMSO-d6). Chemical shifts are expressed in values (ppm) using the solvent peak as internal standard. All coupling constant (J) values are given in hertz. The abbreviations used are as follows: s, singlet; d, doublet; m, multiplet. Elemental analyses were carried out at the Regional Center for Microbiology and Biotechnology, Al-Azhar University, Cairo, Egypt. Analytical thin layer chromatography (TLC) on silica gel plates containing UV indicator was employed routinely to follow the course of reactions and to check the purity of products. Some representative NMR charts are provided in the Supplementary material.
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2

Extraction and Characterization of EGCG from Oolong Tea

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Dried Oolong tea leaves (26 g, Jin Xuang No. 12, Boonrod Farm, Chiang Mai, Thailand) were stirred with methanol (300 mL) at 55 °C for 3 h, then the mixture was cooled, and solid residues were filtered out. The liquid extract was evaporated under the reduced pressure at 50 °C to obtain the crude extract. The crude extract was partitioned with 40 mL of dichloromethane : methanol : water (3 : 1 : 0.2 v/v) mixture. The methanol/water layer was collected and evaporated under low pressure at 55 °C to obtain the extracted EGCG (5.04 g). The obtained EGCG was subjected to 1H NMR (DMSO-D6, 400 MHz Varian Mercury+ NMR spectrometer) and reverse phase HPLC analyses.
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3

Comprehensive Spectroscopic Analysis of Synthesized Compounds

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NMR (1H and 13C) spectra were obtained on a Varian Mercury NMR spectrometer (300 MHz) using deuterated chloroform (CDCl3), dimethyl sulfoxide (DMSO-d6), and methanol (CD3OD) as solvents and TMS as an internal standard. Chemical shifts were reported in parts per million (ppm). The following abbreviations were used to describe the peak multiplicities: s, singlet; d, doublet; and t, triplet. Low-resolution electrospray ionization mass spectra (ESI-MS) were recorded on a Bruker Esquire 3000 plus ion trap mass spectrometer equipped with an ESI (electrospray) ion source. The Fourier transform infrared (FT-IR) spectra of the synthesized compounds (NAP-NAP and SNAP-SNAP) were obtained on a PerkinElmer Spectrum 3 FT-IR spectrometer. The synthesized compounds were mixed into potassium bromide (KBr) with a ratio of 1:100, finely pulverized, and then formed into a transparent pellet under high pressure for the FT-IR analysis. The KBr pellet without the sample was used for background measurements. Each spectrum was collected over a wavenumber range of 450–4000 cm−1 with a resolution of 8 cm−1 and a scan rate of 16.
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4

Spectroscopic Analysis of Organic Compounds

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Melting points were measured with a Stuart melting point apparatus and were uncorrected. Infrared (IR) Spectra were recorded as KBr disks using Schimadzu FT-IR 8400S spectrophotometer (Shimadzu, Kyoto, Japan). Mass spectral data are given by GCMS-QP1000 EX spectrometer at 70 eV. NMR spectra were recorded on a Varian Mercury NMR spectrometer. 1H spectrum was run at 400 MHz and 13C spectrum was run at 100 MHz in deuterated dimethylsulphoxide (DMSO-d6). Chemical shifts are expressed in values (ppm) using the solvent peak as internal standard. All coupling constant (J) values are given in Hertz. The abbreviations used are as follows: s, singlet; d, doublet; m, multiplet. Elemental analyses were carried out at the Regional Center for Microbiology and Biotechnology, Al-Azhar University, Cairo, Egypt. Analytical thin layer chromatography (TLC) on silica gel plates containing UV indicator was employed routinely to follow the course of reactions and to check the purity of products.
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5

NMR Spectroscopy of DNA PEGylation

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The 1H NMR spectra of the solutions in D2O for the investigation of the DNA PEGylation and the sample in DMSO-d6 to ensure the identity as well as purity of ANI.HCl was recorded on a Varian Mercury NMR spectrometer operating at 400 MHz. The NMR spectra showing the imino regions with CD3OH as a solvent were recorded at 600 MHz using a Bruker Avance NMR spectrometer. Here, for the temperature-dependent experiments, the -OH peak was suppressed using a 3-9-19 pulse sequence with gradients (WATERGATE), the delay for binomial suppression was set to 250 μs. The other spectra showing the imino region were recorded using a 1-3-3-1 pulse sequence (jump-and-return method) with a delay for binomial water suppression of 90 μs. The relaxation delay was set to 2.0 s and the acquisition time to 3.6 s.
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6

Spectroscopic Characterization of Compounds

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Melting points were measured on Gallenkamp electrothermal melting point apparatus and are uncorrected. IR spectra were recorded as KBr discs using a Shimadzu FTIR-prestige 21 spectrophotometers. 1H NMR spectra were recorded in DMSO-d6 as solvents at 300 MHz on a Varian Mercury NMR spectrometer using TMS as internal standard. Chemical shifts δ are reported in parts per million units (ppm), and J values are given in hertz. The mass spectra were recorded on a GCeMS-QP1000 EX mass spectrometer at 70 eV. Elemental analyses were carried out at the Micro-analytical Centre of Cairo University, Giza, Egypt.
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7

Structural Elucidation of Compound via NMR

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To achieve secure proof of the molecular structure the 1 H, 13 C and 19 F nuclear magnetic resonance (NMR) spectrum of the compound was assigned. A solution of the powder in DMSO-d6 (20 mg in 750µL) was prepared in a Wilmad ® NMR tube (5 mm diameter) and sealed using a polypropylene cap. This sample was used for all three types ( 1 H, 13 C and 19 F) of NMR. All NMR spectra were recorded at 25 °C on a 300 MHz Varian Mercury NMR spectrometer and processed using the Varian VNMRJ 3.2 software package. Referencing of NMR spectra was carried out according to Gottlieb et al. (14) or IUPAC referencing with CFCl3 set to 0 ppm. 2.3.5.1 1 H NMR spectroscopy.
The spectrum was recorded at 300 MHz using 32 scans and was referenced to the signal of tetramethylsilane at 0 ppm. 2.3.5.2 13 C APT NMR spectroscopy.
The spectrum was recorded at 75.4 MHz in Attached-Proton-Test mode using 22500 scans and was referenced to the central peak of the DMSO-d6 multiplet at 39.52 ppm.
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