The 1H NMR spectra were recorded at 500 MHz with a JEOL JNM-ECA 500 NMR spectrometer. The FGMAS NMR spectra were recorded at 400 MHz with a JEOL JNM-ECA 400 NMR spectrometer. The sample spinning rate was 8 kHz. In all NMR measurements, chemical shifts were referenced to the solvent values (δ = 2.49 ppm and 4.79 ppm for DMSO-d6 and D2O, respectively). The contact angles were measured by a Dynamic Contact Angle Analyzer (DCA-700, Kyowa Interface Science Ltd.). The IR spectra of the gels were measured using a JASCO FT/IR-410 spectrometer with a KBr disc, while those of the substrates were measured using a JASCO FT/IR-6000 spectrometer via the attenuated total reflection method (ATR). The mechanical properties of the gels were measured by a mechanical tension testing system (Rheoner, RE-33005, Yamaden Ltd.), while the dynamic viscoelasticity was measured using an Anton Paar MCR301 rheometer. X-ray photoelectron spectroscopy (XPS) data were collected with an AXIS 165 (KRATOS ANALYTICAL) using a monochromatic Al-Kα X-ray source.
Jnm eca500 nmr spectrometer
Manufactured by JEOL
Sourced in Japan
The JNM-ECA500 NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument developed by JEOL. It is designed to analyze the structural and chemical properties of materials by detecting and measuring the resonance frequencies of atomic nuclei within a sample. The JNM-ECA500 operates at a magnetic field strength of 500 MHz, providing high-resolution data for various applications.
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5 protocols using jnm eca500 nmr spectrometer
1
Comprehensive Characterization of Gel Materials
2
Extraction and Characterization of Polyhydroxyalkanoates
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Extraction and estimation of PHA was performed following the procedures reported (Law and lepecky, 1960 ; Venkata Mohan and Venkateswar Reddy, 2013; Venkateswar Reddy et al. 2016 ). 1 H (500 MHz) NMR spectra was recorded on a JNM-ECA500 NMR spectrometer (JEOL, Japan) at 20 °C to know the structure of polymer. Samples of produced PHA and standard P3HB/ P(3HB-co-3HV) (Aldrich) were prepared by dissolving in deuterated chloroform (CDCl3), and then were filtrated with cotton. The signals of tetramethylsilane (TMS) and CDCl3 were used as the standards for chemical shift of 1 H spectra.
Number and weight average molecular mass (Mn and Mw) of standard and sample P3HB/ P(3HB-co-3HV) were measured using GPC 900-1 (JASCO, Japan) equipped with two Shodex K-806L columns and an RI detector. Chloroform was used as an eluent at 40 ºC and polystyrene standards (Mn = 1,680-3,065,000) were employed for calibration.
Number and weight average molecular mass (Mn and Mw) of standard and sample P3HB/ P(3HB-co-3HV) were measured using GPC 900-1 (JASCO, Japan) equipped with two Shodex K-806L columns and an RI detector. Chloroform was used as an eluent at 40 ºC and polystyrene standards (Mn = 1,680-3,065,000) were employed for calibration.
3
Deacetylation and NMR Characterization
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The polysaccharide was de-O-acetylated completely using 0.1 M NaOH at 37℃ for 4 h, following the procedure reported by Bhattacharjee et al. 10) . 1 H NMR spectra were recorded with a JNM-ECA500 NMR spectrometer(JEOL, Tokyo, Japan) using solutions in D2 O at 90℃. Sodium 3-(trimethylsilyl) -1-propanesulfonate was used as the external standard.
4
NMR Spectral Analysis of PHA
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1 H (500 MHz) NMR spectra was recorded on a JNM-ECA500 NMR spectrometer (JEOL, Japan) at 20 °C. Samples of produced PHA and standard P3HB/ P(3HB-co-3HV) (Aldrich) were prepared by dissolving in deuterated chloroform (CDCl3), and then were filtrated with cotton. The signals of tetramethylsilane (TMS) and CDCl3 were used as the standards for chemical shift of 1 H spectra.
5
NMR Characterization of Produced PHB
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1 H (500 MHz) and 13 C (125 MHz) NMR spectra were recorded on a JNM-ECA500 NMR spectrometer (JEOL, Japan) at 20°C. Samples of produced PHB and standard PHB (Aldrich) were prepared by dissolving in deuterated chloroform (CDCl3), and then were filtrated with cotton. The signals of tetramethylsilane (TMS) and CDCl3 were used as the standards for chemical shift of 1 H and 13 C spectra, respectively.
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