1H NMR spectra were recorded on Bruker AMX-500 MHz and Bruker DPX-300 MHz spectrometers as solutions in deuterated solvents by using the solvent peak as the internal standard. UV-Vis absorption spectra were measured on a Shimadzu UV-1700 spectrophotometer using 10 mm path-length cuvettes. IR spectra were recorded on Bruker IFS 66 spectrometer.
Ifs66 spectrometer
Manufactured by Bruker
Sourced in United States, Germany
The IFS66 spectrometer is a Fourier Transform Infrared (FTIR) spectrometer designed for high-performance infrared spectroscopy. It offers a wide spectral range and high-resolution capabilities for various analytical applications.
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Lab products found in correlation
Uv 1700 spectrophotometer, by Shimadzu (1 mentions)
Amx 500 mhz, by Bruker (1 mentions)
Dpx 300 mhz, by Bruker (1 mentions)
Alpha 300, by WITec (1 mentions)
Jem 3010, by JEOL (1 mentions)
Tristar system, by Micromeritics (1 mentions)
D max 2200 ultima, by Rigaku (1 mentions)
Dpx 400 spectrometer, by Bruker (1 mentions)
Ftir spectrometer, by Bruker (1 mentions)
Jem 2100 electron microscope, by JEOL (1 mentions)
Avance 3 spectrometer, by Bruker (1 mentions)
Topspin, by Bruker (1 mentions)
Lcms it tof, by Shimadzu (1 mentions)
Spectrum two, by PerkinElmer (1 mentions)
Vnmrs 400 mr, by Agilent Technologies (1 mentions)
Mat 711 spectrometer, by Agilent Technologies (1 mentions)
Avance drx spectrometer, by Bruker (1 mentions)
Cary 500 uv vis nir spectrophotometer, by Agilent Technologies (1 mentions)
Fls920 spectrofluorometer, by Edinburgh Instruments (1 mentions)
13 protocols using ifs66 spectrometer
1
Spectroscopic Characterization of Samples
2
Probing Lipid Phase Transitions with FTIR
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The Fourier transform infrared spectra were recorded using an IFS66 spectrometer (Bruker, Billerica, MA, USA) equipped with a DTGS detector. A sample was placed between the window made of CaF2 and separated by a 50 µm Teflon spacer. The cuvette was thermostated at temperatures varying between 24 and 50 °C by changing the temperature of water circulating inside the cuvette body, and the corresponding temperature of the sample was controlled by a CHY502 electronic thermometer. Each spectrum was the average of 10 measurements, each with 16 scans and 2 cm−1 resolution. Background spectrum of the phosphate buffer solution was removed from the recorded spectra of the samples. The wavenumber positions for the symmetric and asymmetric CH2 stretching modes were measured using a peak fitting module in OriginPro 2018 software (Northampton, MA, USA). The symmetric CH2 stretching frequencies were plotted against the temperature. According to the first derivative of this relation, the main phase transition temperature of DPPG and DPPC liposomes before and upon binding of lipopeptide was found.
3
FTIR Analysis of PLLA/PU Blends
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FTIR spectra of
the PLLA/PU blends and insoluble sample fractions were recorded at
room temperature using a Bruker IFS66 spectrometer equipped with an
attenuated total reflectance (ATR) accessory. A total of 32 spectra
with a resolution of 4 cm–1 were acquired for each
sample in the range 500–4000 cm–1.
the PLLA/PU blends and insoluble sample fractions were recorded at
room temperature using a Bruker IFS66 spectrometer equipped with an
attenuated total reflectance (ATR) accessory. A total of 32 spectra
with a resolution of 4 cm–1 were acquired for each
sample in the range 500–4000 cm–1.
4
Characterization of Heterogeneous Catalysts
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The X-ray diffraction (XRD) patterns of these prepared catalysts were obtained from a Rigaku D/MAX-2200 ultima equipped with Cu Kα radiation (λ = 1.54 Å) at 30 kV and 40 mA. N2 adsorption–desorption isotherms were obtained using a Micromeritics Tristar system at liquid N2 temperature. Before measurements, samples were degassed at 323 K for 12 h. The Brunauer–Emmett–Teller (BET) and Barrett–Joyner–Halenda (BJH) methods were utilized to calculate the BET surface area and pore size distribution, respectively. Scanning electron microscopy (SEM) image was obtained using a Hitachi UHR S 5500 FE-SEM operated at an accelerating voltage of 15 kV. Transmission electron microscopy (TEM) images were collected using JEOL JEM 3010 at an accelerating voltage of 200 kV. Raman spectra were recorded under ambient conditions at room temperature (RT) using WITEC Alpha300. The excitation line of the laser was at 532 nm. Fourier transform infrared spectroscopy (FT-IR) spectra were measured using KBr wafer technique with Bruker IFS-66 spectrometer. H2-Temperature programmed reduction (H2-TPR) was performed in a fixed-bed reactor. Sample (20 mg) was put in a quartz microreactor, and pretreated with He up to 100 °C at a rate of 10 °C min−1 for 1 h for pretreatment. Then 10 vol% H2 in a He flow of 40 mL min−1 was maintained at RT for 30 min. Finally, the sample was ramped to 900 °C at 10 °C min−1.
5
Structural Characterization of Organometallic Compounds
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C, H, and N were determined using a Carlo Erba 1106 automatic analyzer available at the Australian National University whereas Pt was determined by graphite furnace atomic absorption spectroscopy (AAS). As QH4, QH7 and QH8, could not be obtained in crystalline form, IR, MS and 1H NMR spectra were used to aid in structural characterization. The IR spectra were obtained using a Varian FT-IR spectrometer (Bruker IFS66 spectrometer). To obtain mass spectra, solutions of QH4, QH7 and QH8 made in 90% methanol and 10% DMF were sprayed into a Finnigan LCQ mass spectrometer. To obtain 1H NMR spectra using a Bruker DPX400 spectrometer at 400.2 MHz. QH4 was dissolved in DMF, QH7 in CDCl3 and QH8 in D2O/DMF and prepared in 5 mm high precision Wilmad NMR tube. Spectra were referenced to internal solvent residues and all the spectra were recorded at 300 K (±1 K).
6
Ultrastructural Analysis of Epiphyseal Growth Plate
7
Lipid Phase Transition Analysis by FTIR
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Fourier transform infrared spectra were recorded on a IFS66 spectrometer (Bruker, Billerica, MA, USA) equipped with a DTGS detector. The samples were placed between two CaF2 windows separated with a 50 µm Teflon spacer. The spectra were measured between 3000 and 2500 cm−1 at 2 cm−1 resolution as the average of 10 measurements each with 16 scans. The cuvette was thermostated to the appropriate temperature in the range of 27–46 °C by using a Julabo F33 thermostat (Seelbach, Germany), and the sample temperature was controlled with a CHY502 thermometer. The spectrum of the phosphate buffer solution at the appropriate temperature was each time subtracted from the final spectra. The wavenumber positions for symmetric and asymmetric CH2 stretching modes of the lipid hydrocarbon chains were measured using a multiple Gaussian curve fitting procedure in OriginPro 2021 software. Finally, the frequency of the symmetrical CH2 stretching modes was plotted against the temperature. For a more precise determination of the temperature of the main phase transition of the lipids, Tm, the first derivatives of the relationships were calculated. The main phase transition temperature of the DPPC and DPPG was determined before and after binding of the lipopeptides.
8
Synthesis and Characterization of Chalcone-Derived Pyrazoles
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Liquid chromatography-mass spectrometry (LCMS) spectra were registered on an LCMS IT-TOF (Shimadzu, Japan) with an electrospray ionization (ESI) source in the positive ion mode. 1H-NMR spectra were acquired on a Bruker Avance III spectrometer at 500 MHz. The NMR data were processed and analyzed by TopSpin (Bruker, USA). Chemical shifts were expressed at δ value to the internal standard (TMS). IR spectra were measured on an IF S66 spectrometer (Bruker, USA) in KBr pellets at an absorption range of 400–4000 cm−1. Thin layer chromatography (TLC) was performed on Merck Kieselgel 60 F254 aluminum plates and visualized with UV and iodine.
Each compound was synthesized in two stages: condensation of the appropriately substituted benzaldehydes and acetophenones, and reaction with hydrazine hydrate to yield chalcone-derived pyrazoles.
Each compound was synthesized in two stages: condensation of the appropriately substituted benzaldehydes and acetophenones, and reaction with hydrazine hydrate to yield chalcone-derived pyrazoles.
9
Fourier Transform Infrared Spectroscopy
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IR spectra were recorded using an IFS66 spectrometer from BRUKER (Germany), performing Fourier transform infrared spectra with a resolution of 0.12 cm−1 for solid, liquid and gaseous samples in the entire range, i.e., MIR (4000 − 400 cm−1), FIR (700 − 4.0 cm−1). Spectra S53-S55 were recorded courtesy of Pro-Environment Polska Sp. z. o. o., which provided an FT-IR Spectrometer, model: Spectrum Two with ATR attachment (Spectrum Two FT-IR Spectrometer with LiTaO3 Detector, PerkinElmer, Inc., Waltham, MA, USA).
10
Characterization of Novel Synthetic Compounds
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The chemical reagents were supplied by Sigma-Aldrich (USA) and were used without further purification. Purity of the compounds was checked using thin layer chromatography (TLC) plates (silica gel G) in the appropriated system for each compound. The spots were located with short (254 nm)/long (365 nm) UV wavelength.
All melting points were measured in a capillary tube on a Quimis apparatus. Infrared spectra of 1% KBr pellets were recorded using a Bruker IFS66 spectrometer. 1H NMR and 13C NMR spectra were measured on a VARIAN VNMRS 400-MR, using 400 MHz for 1H and 75.4 MHz for 13C in CDCl3 and acetone-d6 maintained at 25°C using Me4Si (TMS) as an internal standard. The chemical shifts were reported in δ units and the coupling constants (J) were reported in hertz. The following abbreviations were used to indicate the peak multiplicity: s (singlet), d (doublet), dd (double doublet), t (triplet), and m (multiplet). C, H, N, and S analyses were performed with a Carlo Erba elemental analyzer, model EA1108. Mass spectra were recorded on a Varian MAT 711 spectrometer at an electron impact of 70 eV. The synthesized compounds are shown inScheme 1 , showing the respective substituent.
All melting points were measured in a capillary tube on a Quimis apparatus. Infrared spectra of 1% KBr pellets were recorded using a Bruker IFS66 spectrometer. 1H NMR and 13C NMR spectra were measured on a VARIAN VNMRS 400-MR, using 400 MHz for 1H and 75.4 MHz for 13C in CDCl3 and acetone-d6 maintained at 25°C using Me4Si (TMS) as an internal standard. The chemical shifts were reported in δ units and the coupling constants (J) were reported in hertz. The following abbreviations were used to indicate the peak multiplicity: s (singlet), d (doublet), dd (double doublet), t (triplet), and m (multiplet). C, H, N, and S analyses were performed with a Carlo Erba elemental analyzer, model EA1108. Mass spectra were recorded on a Varian MAT 711 spectrometer at an electron impact of 70 eV. The synthesized compounds are shown in
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