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Avance 400 mhz nmr spectrophotometer

Manufactured by Bruker

The AVANCE 400 MHz NMR spectrophotometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It operates at a frequency of 400 MHz and is capable of providing detailed structural information about chemical compounds through the analysis of their nuclear magnetic properties.

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4 protocols using avance 400 mhz nmr spectrophotometer

1

Quantifying Sulfonation in Polymers via NMR

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The degree of sulfonation was calculated assuming all the sulfur to be present in the form of substituted sulfonic acid groups onto the polymer backbone. This analysis was performed using a Bruker Avance 400 MHz NMR spectrophotometer. This method was selected for the ease of determination of the degree of sulfonation compared with other previously reported methods. The sulfonation number and degree of sulfonation were calculated from the area under the NMR peaks of the SPEEK samples as per the formula given [12 (link)].
n122n=AHEAHx
where n is the sulfonation number, which when multiplied by 100 yields the degree of sulfonation.
AHE is the area under the peak of the hydrogen on the sulfonic acid group.
ΣAHx is the cumulative area of all the other peaks present in the spectra of the sulfonated polymer sample.
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2

Spectroscopic Characterization of Acetal Crosslinker

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1H NMR and 13C NMR analyses of synthesized acetal crosslinker in CDCl3 were carried out on a Bruker AVANCE 400 MHz NMR spectrophotometer. Reported chemical shifts (ppm) are relative to residual CDCl3 peak and coupling constants were reported in Hz. 1H NMR spectra were recorded at 400 MHz while 13C NMR spectra were recorded at 100 MHz. FT-IR spectrophotometric analysis of crosslinker was carried out using a Perkin Elmer Spectrum 100FT-IR spectrometer enabled with attenuated total reflectance (ATR) technology. This equipment does not require the preparation and use of potassium bromide pellets. The molecular weight of the crosslinker was determined by high resolution mass spectroscopy. Analyte was dissolved in Acetonitrile (50%) +Trifluoric acid (0.1%) and injected into Thermo LTQ Orbitrap XL tandem Mass Spectrometer by syringe pump, using Nano Electro Spray Ionization (NSI). Mass spectrometer was operated in FT positive ion mode with resolution 30,000.
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3

Spectroscopic Characterization of Acetal Crosslinker

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1H NMR and 13C NMR analyses of synthesized acetal crosslinker in CDCl3 were carried out on a Bruker AVANCE 400 MHz NMR spectrophotometer. Reported chemical shifts (ppm) are relative to residual CDCl3 peak and coupling constants were reported in Hz. 1H NMR spectra were recorded at 400 MHz while 13C NMR spectra were recorded at 100 MHz. FT-IR spectrophotometric analysis of crosslinker was carried out using a Perkin Elmer Spectrum 100FT-IR spectrometer enabled with attenuated total reflectance (ATR) technology. This equipment does not require the preparation and use of potassium bromide pellets. The molecular weight of the crosslinker was determined by high resolution mass spectroscopy. Analyte was dissolved in Acetonitrile (50%) +Trifluoric acid (0.1%) and injected into Thermo LTQ Orbitrap XL tandem Mass Spectrometer by syringe pump, using Nano Electro Spray Ionization (NSI). Mass spectrometer was operated in FT positive ion mode with resolution 30,000.
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4

Organic Synthesis and Characterization

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All solvents and chemicals were obtained commercially from fine chemicals PLC (Addis Ababa) and were used as received without further purification. Melting points were determined in an open capillary using digital melting point apparatus, expressed in °C. Reaction progress was checked on pre-coated TLC plates and spots were visualized using UV light at 254 nm. Silica gel (60–120 mesh, Merck grade) has been used for column chromatography. The column was subjected to gradient elution by increasing ethyl acetate in n-hexane and spots were visualized under UV lamp (254 nm). The synthesized compounds were characterized on the basis of physical and spectral analysis. The UV-Vis spectra of some compounds were recorded on Double-beam UV-Vis spectrophotometer using DCM and MeOH as blank solvents and λmax values were expressed by nm. The 1H and 13C NMR spectra of the compounds were recorded on Bruker avance 400 MHz NMR spectrophotometer using Chloroform-d or Methanol-d4 as the solvent and the values are expressed in δ ppm.
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