All reactions and manipulations were carried out under dry pure N2 using standard Schlenk techniques. All solvents were distilled from sodium/benzophenone and stored under nitrogen before use. The NMR spectra were recorded on a Bruker MSL-400 spectrometer (1H 400 MHz, 31P 161.7 MHz, 13C 100.6 MHz). SiMe4 was used as internal reference for 1H NMR chemical shifts, and 85% H3PO4 as external reference for 31P NMR. The elemental analyses were carried out at the microanalysis laboratory of the Arbuzov Institute of Organic and Physical Chemistry, Russian Academy of Sciences.
Msl 400 spectrometer
Manufactured by Bruker
Sourced in Japan
The MSL-400 spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 400 MHz and is capable of analyzing a wide range of chemical samples to provide detailed information about their molecular structure and composition.
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Lab products found in correlation
3 protocols using msl 400 spectrometer
1
Schlenk Techniques for Organophosphorus Synthesis
2
NMR and GPC Analysis of PHA
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About 5 to 10 mg of the extracted product was dissolved in 0.5 mL of deuterated chloroform. 1H-NMR spectroscopy of polymer PHA was conducted on a Bruker MSL 400 spectrometer (400 MHz) at 90 °C, a pulse of 4 ms, a spectral width of 3000 Hz and a repetition rate of 4 s.
20 mg of purified PHA product was added into 10 mL of deuterated chloroform and let stand at room temperature for more than 12 h until thoroughly mixed. After being filtered through a 0.22 μm membrane, the sample was subjected to GPC detection using a Shimadzu gel chromatograph at 30 °C. HPLC grade chloroform was used as the mobile phase, and polystyrene was used as the standard sample. The flow rate was 1 mL·min−1, and the injection volume was 50 μL.
20 mg of purified PHA product was added into 10 mL of deuterated chloroform and let stand at room temperature for more than 12 h until thoroughly mixed. After being filtered through a 0.22 μm membrane, the sample was subjected to GPC detection using a Shimadzu gel chromatograph at 30 °C. HPLC grade chloroform was used as the mobile phase, and polystyrene was used as the standard sample. The flow rate was 1 mL·min−1, and the injection volume was 50 μL.
3
Polymer Characterization by GC-FID and NMR
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Polymer composition and accumulation were analyzed using a GC-2010 capillary GC system (Shimadzu Co., Kyoto, Japan) equipped with a flame ionization detector and a Zebron ZB-1 GC capillary column (0.25 mm i.d. × 30 m; Phenomenex Inc., CA, USA). Samples were prepared as follows. Polymer (~10 mg) or dried microbial cells (50 mg) were treated with a solution of methanol (1.7 mL), sulfuric acid (0.3 mL), and chloroform (2 mL) at 100 °C for 140 min to convert the constituents to their methyl esters. Water (1 mL) was then added to the reaction mixture, and the chloroform layer was used for GC analysis.
The 1 H nuclear magnetic resonance (NMR) spectra of the polymers were obtained using a Bruker MSL400 spectrometer (400 MHz; Bruker BioSpin K.K., Yokohama, Japan) at 25 °C and a 90° pulse, with a 4 ms, 3,000 Hz spectral width and a 4 s repetition rate.
Chemical shifts were reported in ppm using tetramethylsilane (TMS) as an internal reference.
The molecular weights of the obtained polymers were determined by gel permeation chromatography (GPC) using tandem TSKgel Super HZM-H columns (6.0 mm I.D. × 150 mm; TOSOH, Tokyo, Japan) with chloroform as the eluent. Calibration was performed using polystyrene samples as standards.
Ultraviolet (UV) light irradiation of samples was carried out using a UVP Black Ray UV bench lamp XX-15BLB (UVP, LLC, CA, USA).
The 1 H nuclear magnetic resonance (NMR) spectra of the polymers were obtained using a Bruker MSL400 spectrometer (400 MHz; Bruker BioSpin K.K., Yokohama, Japan) at 25 °C and a 90° pulse, with a 4 ms, 3,000 Hz spectral width and a 4 s repetition rate.
Chemical shifts were reported in ppm using tetramethylsilane (TMS) as an internal reference.
The molecular weights of the obtained polymers were determined by gel permeation chromatography (GPC) using tandem TSKgel Super HZM-H columns (6.0 mm I.D. × 150 mm; TOSOH, Tokyo, Japan) with chloroform as the eluent. Calibration was performed using polystyrene samples as standards.
Ultraviolet (UV) light irradiation of samples was carried out using a UVP Black Ray UV bench lamp XX-15BLB (UVP, LLC, CA, USA).
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