The IR spectra in KBr pellets were recorded with a FT-IR FSM 1201 spectrometer in the range 400–4000 cm−1. UV–vis spectra from the 10−4 M freshly prepared solutions in freshly distilled MeOH were recorded on an Agilent 8453 instrument. Powder X-ray diffraction was carried out using a Rigaku Ultima IV X-ray powder diffractometer. The parallel beam mode was used to collect the data (λ = 1.54184 Å). Elemental analyses were performed with a Thermo Scientific FLASH 2000 CHNS analyzer (Waltham, MA USA).
Flash 2000 chns analyzer
Manufactured by Thermo Fisher Scientific
Sourced in United States
The FLASH 2000 CHNS Analyzer is a laboratory instrument designed for the determination of carbon, hydrogen, nitrogen, and sulfur content in a wide range of organic and inorganic materials. It employs the dynamic flash combustion method to perform rapid and accurate elemental analysis.
Automatically generated - may contain errors
Lab products found in correlation
Ultima 4 x ray powder diffractometer, by Rigaku (1 mentions)
Dionex ics 5000, by Thermo Fisher Scientific (1 mentions)
Multiwave pro, by Anton Paar (1 mentions)
Icp oes 5110 vdv, by Agilent Technologies (1 mentions)
Nicolet is10 fourier transform infraredspectrometer, by Thermo Fisher Scientific (1 mentions)
Uv 2450 uv vis spectrophotometer, by Shimadzu (1 mentions)
400 mhz spectrometer, by Bruker (1 mentions)
Avance 400 mhz nmr spectrometer, by Bruker (1 mentions)
6530bq tof mass spectrometer, by Agilent Technologies (1 mentions)
Uv 2450 spectrophotometer, by Shimadzu (1 mentions)
Multiwave eco, by Anton Paar (1 mentions)
400 mhz nmr spectrometerat, by Bruker (1 mentions)
Calibrated ph meter, by Mettler Toledo (1 mentions)
Ssc 5200, by Seiko Instruments (1 mentions)
Jsm 6335f, by JEOL (1 mentions)
Supra 35 vp microscope, by Zeiss (1 mentions)
Spectrum one, by PerkinElmer (1 mentions)
Accupyc 2 1340, by Micromeritics (1 mentions)
Avance 2 400 mhz spectrometer, by Bruker (1 mentions)
11 protocols using flash 2000 chns analyzer
1
Spectroscopic Characterization of Compounds
2
Elemental Analysis of Plant Samples
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Elemental analysis was performed using inductively coupled plasma-optical emission spectrometry (ICP-OES, 5110 VDV, Agilent, CA, United States) with prior microwave acid sample digestion (Multiwave Pro, Anton Paar, Les Ulis, France) [8 ml of concentrated HNO3, 2 ml of H2O2, and 15 ml of Milli-Q water for 100 mg dry weight (DW)]. The quantification of each element was carried out with an external standard calibration curve. Analysis of N was realized using an elemental FLASH 2000 CHNS analyzer (Thermo Fisher Scientific, Waltham, MA, United States) according to the instructions of the manufacturer from 2.5 mg of homogenized and lyophilized plant material. NH4+, NO3, and sulfate (SO42–) were extracted and analyzed according to Réthoré et al. (2020) (link) using high pressure ion chromatography with a conductivity detector (Dionex ICS5000 +, Thermo Fisher Scientific, Villebon-sur- Yvette, France).
3
Synthesis of N-Alkoxy Carboxamide-Type Ligands and Their Tantalum Complexes
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All manipulations were performed
under a dry, oxygen-free nitrogen or argon atmosphere using standard
Schlenk techniques or in a glovebox. All solvents were purified by
the Innovative Technology PS-MD-4 solvent purification system. All
reagents were purchased from Sigma-Aldrich and/or Acros. A series
of N-alkoxy carboxamide-type ligands, edpaH and mdpaH,
were prepared by the literature procedure.23 (link) Na(edpa) and Na(mdpa) were prepared by a modified literature method.24 (link) TaCl3(NtBu)(pyridine)2 was obtained by modifying the reported
methods.32 (link)1H NMR and 13C NMR spectra were recorded on a Bruker DPX 500 MHz FT-NMR spectrometer.
All samples for NMR measurements were contained in sealed NMR tubes
and referenced using benzene-d6 as the
standard. Infrared (IR) spectra were collected in the 4000–400
cm–1 range with a SHIMADZU IRSpirit FT-IR spectrophotometer
in a 4 nm KBr window. The samples were prepared in a glovebox. Elemental
analysis (EA) was performed using a Thermo Scientific Flash 2000 CHNS
analyzer. Thermogravimetric analysis (TGA) was performed under a N2 atmosphere at a scan rate of 10 °C min–1 using a Thermo plus EVO II TG8120 series thermogravimetry and differential
thermal analysis instrument from Rigaku.
under a dry, oxygen-free nitrogen or argon atmosphere using standard
Schlenk techniques or in a glovebox. All solvents were purified by
the Innovative Technology PS-MD-4 solvent purification system. All
reagents were purchased from Sigma-Aldrich and/or Acros. A series
of N-alkoxy carboxamide-type ligands, edpaH and mdpaH,
were prepared by the literature procedure.23 (link) Na(edpa) and Na(mdpa) were prepared by a modified literature method.24 (link) TaCl3(NtBu)(pyridine)2 was obtained by modifying the reported
methods.32 (link)1H NMR and 13C NMR spectra were recorded on a Bruker DPX 500 MHz FT-NMR spectrometer.
All samples for NMR measurements were contained in sealed NMR tubes
and referenced using benzene-d6 as the
standard. Infrared (IR) spectra were collected in the 4000–400
cm–1 range with a SHIMADZU IRSpirit FT-IR spectrophotometer
in a 4 nm KBr window. The samples were prepared in a glovebox. Elemental
analysis (EA) was performed using a Thermo Scientific Flash 2000 CHNS
analyzer. Thermogravimetric analysis (TGA) was performed under a N2 atmosphere at a scan rate of 10 °C min–1 using a Thermo plus EVO II TG8120 series thermogravimetry and differential
thermal analysis instrument from Rigaku.
4
Synthesis and Spectroscopic Characterization of Organometallic Complexes
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All reactions were carried out under
dry, oxygen-free N2 atmosphere using standard Schlenk techniques.
The starting materials were purchased from Sigma-Aldrich Chemicals.
Rhenium carbonyl, dibutyldisulfide, dibenzyldisulfide, p-tolyldisulfide, and diphenyldiselenide were used as received. The
bridging ligands N,N′-bis(4-pyridinecarboxamide)-1,2-ethane, N,N′-bis(4-(4-pyridylcarboxamide)phenyl)methane,
and diferrocenedisulfide were synthesized as reported in the literature.17 ,7b Mesitylene and other solvents were purified and dried using the
literature procedure prior to use.18 IR
spectra were taken on a Thermo Nicolet iS10 Fourier transform infrared
spectrometer. 1H and 13C NMR were recorded on
an Avance Bruker 400 MHz spectrometer. Electronic absorption spectra
were recorded on a Shimadzu UV-2450 UV–vis spectrophotometer.
Emission spectra were recorded on a Fluoromax-4 spectrofluorometer.
Elemental analyses were performed using a Thermo Scientific Flash
2000 CHNS analyzer. Compounds1–8 were dried thoroughly
under high vacuum condition for several hours, prior to the submission
of samples for 1H and 13C NMR spectral characterization
and elemental analyses.
dry, oxygen-free N2 atmosphere using standard Schlenk techniques.
The starting materials were purchased from Sigma-Aldrich Chemicals.
Rhenium carbonyl, dibutyldisulfide, dibenzyldisulfide, p-tolyldisulfide, and diphenyldiselenide were used as received. The
bridging ligands N,N′-bis(4-pyridinecarboxamide)-1,2-ethane, N,N′-bis(4-(4-pyridylcarboxamide)phenyl)methane,
and diferrocenedisulfide were synthesized as reported in the literature.17 ,7b Mesitylene and other solvents were purified and dried using the
literature procedure prior to use.18 IR
spectra were taken on a Thermo Nicolet iS10 Fourier transform infrared
spectrometer. 1H and 13C NMR were recorded on
an Avance Bruker 400 MHz spectrometer. Electronic absorption spectra
were recorded on a Shimadzu UV-2450 UV–vis spectrophotometer.
Emission spectra were recorded on a Fluoromax-4 spectrofluorometer.
Elemental analyses were performed using a Thermo Scientific Flash
2000 CHNS analyzer. Compounds
under high vacuum condition for several hours, prior to the submission
of samples for 1H and 13C NMR spectral characterization
and elemental analyses.
5
Synthesis and Characterization of Pyridyl Ligands
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All reactions were carried out under
an oxygen-free, N2 atmosphere using standard Schlenk line
techniques. The starting materials were purchased from Alfa-Aesar
and Sigma-Aldrich Chemicals. Mn2(CO)10, trimethylamine-N-oxide, isonicotinoyl chloride hydrochloride, 1,2-ethanediol,
1,2-dihydroxybenzene, diethylene glycol, 1,2-ethylene diamine, 1,4-phenylenediamine, p-benzoquinone, n-butylamine, and phenethylamine
were used as received. The aminoquinone ligands (bbbq and bpbq) and
ditopic pyridyl ligands (etdp, pcadgd, pdi, bpce, and pdia) were synthesized
as reported in the literature.17 (link) Dichloromethane,
ethanol, methanol, tetrahydrofuran, and other solvents were dried
using standard methods and freshly distilled prior to use.18 IR spectra were recorded on a Nicolet iS10 Fourier
transform infrared spectrometer. Electronic absorption spectra were
obtained on a Shimadzu UV-2450 spectrophotometer. Emission spectra
were recorded on a Fluoromax-4 spectrofluorometer. Solvents used for
UV–vis and emission titration experiments were of spectral
grade. 1H NMR spectra were recorded on a Bruker Avance
400 MHz NMR spectrometer with tetramethylsilane as the internal reference.
Elemental analyses were performed using a Thermo Scientific Flash
2000 CHNS analyzer. ESI-mass spectra were taken on an Agilent 6530B
Q-TOF mass spectrometer.
an oxygen-free, N2 atmosphere using standard Schlenk line
techniques. The starting materials were purchased from Alfa-Aesar
and Sigma-Aldrich Chemicals. Mn2(CO)10, trimethylamine-N-oxide, isonicotinoyl chloride hydrochloride, 1,2-ethanediol,
1,2-dihydroxybenzene, diethylene glycol, 1,2-ethylene diamine, 1,4-phenylenediamine, p-benzoquinone, n-butylamine, and phenethylamine
were used as received. The aminoquinone ligands (bbbq and bpbq) and
ditopic pyridyl ligands (etdp, pcadgd, pdi, bpce, and pdia) were synthesized
as reported in the literature.17 (link) Dichloromethane,
ethanol, methanol, tetrahydrofuran, and other solvents were dried
using standard methods and freshly distilled prior to use.18 IR spectra were recorded on a Nicolet iS10 Fourier
transform infrared spectrometer. Electronic absorption spectra were
obtained on a Shimadzu UV-2450 spectrophotometer. Emission spectra
were recorded on a Fluoromax-4 spectrofluorometer. Solvents used for
UV–vis and emission titration experiments were of spectral
grade. 1H NMR spectra were recorded on a Bruker Avance
400 MHz NMR spectrometer with tetramethylsilane as the internal reference.
Elemental analyses were performed using a Thermo Scientific Flash
2000 CHNS analyzer. ESI-mass spectra were taken on an Agilent 6530B
Q-TOF mass spectrometer.
6
Elemental Analysis of Plant Samples
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Elemental analysis was performed according to Maillard et al. [81 (link)] in the PLATIN’ (Plateau d’Isotopie de Normandie) core facility. Elements were quantified by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS, Thermo Scientific, Element 2TM) with prior microwave acid sample digestion (Multiwave ECO, Anton Paar, les Ulis, France) (800 µL of concentrated HNO3, 200 µL of H2O2, and 1 mL of Milli-Q water for 40 mg DW). For the determination by high resolution inductively coupled plasma mass spectrometry (HR ICP-MS) all the samples were spiked with two internal-standard solutions of gallium and rhodium for final concentrations of 10 and 2 µg L−1, respectively, diluted to 50 mL with Milli-Q water to obtain solutions containing 2.0% (v/v) of nitric acid, then filtered at 0.45 µm using a teflon filtration system (Filtermate, Courtage Analyses Services, Mont-Saint-Aignan, France). Quantification of each element was performed using external standard calibration curves.
Analysis of N was performed using an elemental FLASH 2000 CHNS analyzer (Thermo Scientific, Waltham, MA, USA) according to manufacturer’s instructions from 2.5 mg of homogenized and lyophilized plant material.
Analysis of N was performed using an elemental FLASH 2000 CHNS analyzer (Thermo Scientific, Waltham, MA, USA) according to manufacturer’s instructions from 2.5 mg of homogenized and lyophilized plant material.
7
Spectroscopic Characterization of Compounds
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Solvents and fine chemicals
were obtained from commercial sources and utilized with no additional
purification. A Fisher melting apparatus was used to determine melting
points that are uncorrected. A JEOL a 500 MHz NMR spectrometer at
the Faculty of Science, Mansoura University, was used to record the 1H NMR (500 MHz) and 13C NMR (125 MHz) spectra using
DMSO-d6, D2O, and CDCl3 as solvents. On the other hand, a Bruker 400 MHz NMR spectrometer
at the Faculty of Science, Zagazig University, was used to record
the 1H NMR (400 MHz) and 13C NMR (100 MHz) spectra
using DMSO-d6 as a solvent. Chemical shifts
(δ) are given in ppm, and coupling constants (J) are reported in Hz. Elemental analyses were performed at the Regional
Center for Mycology & Biotechnology, Al-Azhar University, on a
Thermo Fisher Flash 2000 CHNS analyzer. The progress of the reactions
was checked by (TLC), and short-length UV irradiation was used for
visualization.
were obtained from commercial sources and utilized with no additional
purification. A Fisher melting apparatus was used to determine melting
points that are uncorrected. A JEOL a 500 MHz NMR spectrometer at
the Faculty of Science, Mansoura University, was used to record the 1H NMR (500 MHz) and 13C NMR (125 MHz) spectra using
DMSO-d6, D2O, and CDCl3 as solvents. On the other hand, a Bruker 400 MHz NMR spectrometer
at the Faculty of Science, Zagazig University, was used to record
the 1H NMR (400 MHz) and 13C NMR (100 MHz) spectra
using DMSO-d6 as a solvent. Chemical shifts
(δ) are given in ppm, and coupling constants (J) are reported in Hz. Elemental analyses were performed at the Regional
Center for Mycology & Biotechnology, Al-Azhar University, on a
Thermo Fisher Flash 2000 CHNS analyzer. The progress of the reactions
was checked by (TLC), and short-length UV irradiation was used for
visualization.
8
Comprehensive Analytical Characterization
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All the chemicals and solvents were purchased with the highest purity grade available and used without further purification unless otherwise specified; pH measurements were carried out using a calibrated pH-meter (Mettler-Toledo). Liquid chromatography/mass spectrometry (LC/MS) was performed on an Agilent 6300 Ion Trap LC/MS System equipped with an electrospray ionization (ESI) interface. Elemental analysis was performed on a Thermo Scientific™ FLASH 2000 CHNS Analyzer.
All the reaction intermediates were purified as specified in the following procedures and their purity (≥95%) was checked by a combination of LC/MS, NMR and elemental analysis.
Atom numbering of the NMR data refers toFigure 1 .
All the reaction intermediates were purified as specified in the following procedures and their purity (≥95%) was checked by a combination of LC/MS, NMR and elemental analysis.
Atom numbering of the NMR data refers to
9
Comprehensive Physicochemical Characterization
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All the chemicals and solvents were purchased with the highest purity grade available and used without further purification unless otherwise specified; pH measurements were carried out using a calibrated pH-meter (Hach).
UV–visible spectra were recorded using a JASKO V-570 UV/Vis/NIR spectrophotometer at 298 K in the 250–600 nm spectral range employing quartz cells (1 cm optical path). Elemental analysis was performed on a Thermo Scientific™ FLASH 2000 CHNS Analyzer. TG analyses were performed using a Seiko SSC 5200 in a temperature range between 25 °C and 1000 °C, with a heating rate of 1 °C/min. The morphology of the beads before and after soaking was examined by SEM using a JSM-6335F (JEOL) microscope operating at 20 kV. IR spectra were recorded in the 4000–400 cm−1 spectral range, using a FT-IR Jasco 4700 equipped with the ATR proONE.
UV–visible spectra were recorded using a JASKO V-570 UV/Vis/NIR spectrophotometer at 298 K in the 250–600 nm spectral range employing quartz cells (1 cm optical path). Elemental analysis was performed on a Thermo Scientific™ FLASH 2000 CHNS Analyzer. TG analyses were performed using a Seiko SSC 5200 in a temperature range between 25 °C and 1000 °C, with a heating rate of 1 °C/min. The morphology of the beads before and after soaking was examined by SEM using a JSM-6335F (JEOL) microscope operating at 20 kV. IR spectra were recorded in the 4000–400 cm−1 spectral range, using a FT-IR Jasco 4700 equipped with the ATR proONE.
10
Characterization of Porous PolyHIPE Materials
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Chemical structure was characterized
by Fourier transform infrared (FTIR) spectroscopy. FTIR spectra were
recorded on a PerkinElmer Spectrum One instrument (PerkinElmer, Inc.,
Waltham, MA, USA). Elemental analyses were performed to determine
the nitrogen content in the resulting polyHIPEs (Flash 2000 CHNS Analyzer,
Thermo Scientific). Porous structure of the dry polyHIPEs was studied
by scanning electron microscopy (SEM) (Carl Zeiss, SUPRA 35 VP microscope).
A piece of each sample was cryogenically fractured and mounted on
a carbon tab for better conductivity. A thin layer of gold was sputtered
on the sample’s surface prior to SEM analysis. The polyHIPE
densities (ρPH) were determined gravimetrically.
The polyHIPE skeletal (polymer wall) densities (ρP) was analyzed using a fully automated, high-precision helium pycnometer
(Micromeritics AccuPyc II 1340).
by Fourier transform infrared (FTIR) spectroscopy. FTIR spectra were
recorded on a PerkinElmer Spectrum One instrument (PerkinElmer, Inc.,
Waltham, MA, USA). Elemental analyses were performed to determine
the nitrogen content in the resulting polyHIPEs (Flash 2000 CHNS Analyzer,
Thermo Scientific). Porous structure of the dry polyHIPEs was studied
by scanning electron microscopy (SEM) (Carl Zeiss, SUPRA 35 VP microscope).
A piece of each sample was cryogenically fractured and mounted on
a carbon tab for better conductivity. A thin layer of gold was sputtered
on the sample’s surface prior to SEM analysis. The polyHIPE
densities (ρPH) were determined gravimetrically.
The polyHIPE skeletal (polymer wall) densities (ρP) was analyzed using a fully automated, high-precision helium pycnometer
(Micromeritics AccuPyc II 1340).
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