1 H-NMR spectra were recorded on a JEOL ECX-400 (400 MHz) or JEOL ECS-400 (400 MHz) in CDCl 3 with tetramethylsilane (δ = 0.00) as internal standard. Chemical shifts are reported in part per million (ppm), and signal are expressed as singlet (s), doublet (d) , triplet (t), quartet (q), multiplet (m), and broad (br). 13 C-NMR spectra were recorded on a JEOL ECX-400 (100MHz) in CDCl 3 (δ = 77.00) with tetramethylsilane as an internal standard (δ = 0.0). Chemical shifts are reported in part per million (ppm). HPLC analysis was directly performed with chiral stationary phase column, Chiralpak AD-H or Chiralcel OD-H purchased from DAICEL Co., Ltd. High resolution mass spectra (HRMS) were recorded on a JEOL JMS 700TZ mass spectrometer at the Center for Instrumental Analysis, Hokkaido University. Optical rotations were measured on a HORIBA SEPA-300 digital polarimeter. Kanto Chemical silica gel 60N (particle size 0.063-0.210 mm) was used for flash column chromatography. RuCl and RuCl 2 (nbd)(MeCN) 2 17 were prepared by the literature procedure. BIPAM ligand (Me-BIPAM) were prepared according to our previous procedure. 18 Me-BIPAM was commercially available from Wako Pure Chemical Industries, Ltd. Phthalide was purchased from commercial source and substituted phthalides were synthesized according to known literature. 19
Ecx 400
Manufactured by JEOL
Sourced in Japan
The ECX-400 is a nuclear magnetic resonance (NMR) spectrometer produced by JEOL. It is a compact and versatile instrument designed for the analysis of chemical samples. The ECX-400 features a 400 MHz superconducting magnet and provides high-resolution NMR data for a wide range of applications in chemistry, materials science, and life sciences.
Automatically generated - may contain errors
Lab products found in correlation
Al 400, by JEOL (2 mentions)
Ecx 500, by JEOL (2 mentions)
Avance 700, by Bruker (2 mentions)
Eca 600, by JEOL (2 mentions)
Masshunter workstation software version b 02, by Agilent Technologies (2 mentions)
Agilent 6220 esi tof ms instrument, by Agilent Technologies (2 mentions)
Ecp 500, by JEOL (2 mentions)
Avance 3 700, by Bruker (2 mentions)
Geigerflex radiib, by Malvern Panalytical (2 mentions)
Ecs 400, by JEOL (2 mentions)
Drx500, by JEOL (1 mentions)
Esca 3200 photoelectron spectrometer, by Shimadzu (1 mentions)
Jem 2100, by JEOL (1 mentions)
Miniflex 2, by Rigaku (1 mentions)
Irspirit spectrometer, by Shimadzu (1 mentions)
Qatr s, by Shimadzu (1 mentions)
Q trap 2000, by Thermo Fisher Scientific (1 mentions)
Alpha ftir spectrometer, by Bruker (1 mentions)
Q50 tg, by TA Instruments (1 mentions)
Spectrum 100 spectrometer, by PerkinElmer (1 mentions)
28 protocols using ecx 400
1
NMR Spectroscopy and HPLC Analysis Protocol
2
NMR and Mass Spectrometry Analysis
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1H (500 or 400 MHz) and 13C (125 or 100 MHz) nuclear magnetic resonance (NMR) spectra were recorded on a Bruker-DRX500, JEOL ECX-400 or JEOL AL-400 spectrometer. Fast atom bombardment mass spectrometry (FAB-MS) and electrospray ionization time-of-flight spectrometry were conducted using a JEOL JMS-700 MStation and Micromass LCT Premier XE mass spectrometer, respectively.
3
NMR Analysis of Chemical Compounds
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The nuclear magnetic resonance (NMR) analyses were performed by using the Jeol-ECX400 instrument operating at 400 MHz for proton NMR while 100 MHz for carbon NMR. The chemical shifts of the splitting patterns were compared to the tetramethylsilane (TMS standard at 0). The TMS (0.03%) was present within the chloroform-d or DMSO-d6. The chemical reactions were performed in a small 2 mL reaction vessel. The precoated silica gel aluminum plates were used for the routine thin layer chromatography analysis. The chemicals and standard drugs used in this research were purchased from the local supplier of Sigma-Aldrich. All the solvents used were of analytical grades.
4
Characterization of Ag Nanoparticles on TiO2
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The morphologies and sizes of Ag NPs of Agx/TiO2 were characterised via transmission electron microscope (TEM) images (JEOL JEM 2100) operating at 200 kV. All specimens for TEM were prepared by dropping a diluted suspension of Agx/TiO2 on a collodion membrane-coated Cu grid. The number-averaged particle sizes, dav, were calculated by measuring the long-axis lengths of more than 100 particles. The powder X-ray diffraction (XRD) patterns were obtained on an X-ray diffractometer (Rigaku MiniFlex II) equipped with a Cu Kα X-ray source (30 kV, 15 mA). 109Ag nuclear magnetic resonance (NMR) spectra of the Ag(i )–alkyldiamine complexes in aqueous solutions were measured with an NMR spectrometer (JEOL ECX-400), where an aqueous solution of AgNO3 was used as a reference for calibrating chemical shifts (δ). The concentrations of Ag ions in aqueous media and the Ag contents of Agx/TiO2 were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES, SII Nanotechnology, SPS 3500-DD). X-ray photoelectron spectroscopy (XPS) was carried out using a Shimadzu ESCA-3200 photoelectron spectrometer equipped with a Mg Kα X-ray source (hν = 1253.6 eV, 10 kV, 30 mA). The binding energy of the Ag NPs of Agx/TiO2 was calibrated by setting the C 1s peak to 284.8 eV.
5
Spectroscopic and Thermal Analysis Methods
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1H NMR spectra were measured on a JEOL (Tokyo, Japan) ECX-400 (400 MHz) spectrometer using tetramethylsilane as an internal standard. The 13C NMR spectrum was measured on a JEOL (Tokyo, Japan) ECX-500 (125 MHz) spectrometer using d6-DMSO as an internal standard. d6-DMSO (Kanto Chemical) was used as the solvent. Fourier-transfer infrared (IR) spectra were measured on a Shimadzu (Kyoto, Japan) IRSpirit spectrometer equipped with a Shimadzu QATR-S attenuated total reflection accessory with a diamond disk with a step of 1 cm–1. Differential scanning calorimetry (DSC) measurements were performed on a Seiko (Tokyo, Japan) DSC-220 instrument under a nitrogen atmosphere (10 °C min−1, N2, second heating scan).
6
Analysis of Purified Hydrolysed Lipids
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The purified hydrolysed lipids were analysed by mass spectrometry using a Q-Trap 2000 (Applied Biosystems, Foster City, USA) which operated at ion-spray ionisation (ESI-MS). The purified lipid hGDNT was diluted to 0.1 μg/mL prior to measurement. IR spectrum of hGDNT was recorded by an ALPHA FT-IR spectrometer (Bruker Corp., Massachusetts, USA). 5 mg of hGDNT was used to obtain the transmission spectrum. For 1H-NMR studies, hydrolysed lipids were dissolved at 2.5 mg/mL in CDCl3 and analysed with a JEOL ECX-400 with an autotune sample head. HPTLC plates were used to identify the lipids PLFE and hGDNT using the mobile phases CHCl3 : MeOH : H2O (22.5 : 50 : 22.5 v/v) and CHCl3 : MeOH (90 : 10 v/v), respectively. Lipids were spotted using a MeOH/sulfuric acid spray reagent.
7
Characterization of Coordination Complexes
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Reagents and solvents were purchased from Sigma-Aldrich, Fluorochem, Alpha or TCL and used without further purification. C3S3 reaction was performed using agate mortar and pestle. 1H and 13C Nuclear Magnetic Resonance (NMR) spectra of 5 were recorded on a Jeol ECX400 at a frequency of 400 and 100 MHz, respectively. PXRD of the Werner complexes, clathrates and the reversible phase transformation in SAMM-5-Co-NCS·NB to SAMM-5-Co-NCS were acquired on Empyrean diffractometer (PAN-analytical, Philips) using CuKα (λ = 1.54178 Å) source. PXRD data of 5 , (SAMM-5-Co-NCS and SAMM-5-Ni-NCS after soaking in OX) and (SAMM-5-Co-NCS after removal and soaking in 1,2-DCB) were acquired on Proto AXRD Benchtop Powder Diffractometer. TGA curves were performed on a TA Instrument Q50 TG under flow of N2 with heating rate of 10 °C min−1. The balance purge was 40 mL min−1 and the sample purge was 60 mL min−1 of N2. Differential scanning calorimetry (DSC) analyses were carried out on a TA Instrument DSC Q20 under a sample purge of 50 mL min−1 of N2 with the heating rate of 10 °C min−1 for all compounds. Fourier Transform Infrared (FTIR) spectra of 5 , Werner complexes and clathrates were collected on a PerkinElmer Spectrum 100 spectrometer with ATR accessory.
8
Characterization of Nanomaterial Composites
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1H NMR spectra
were recorded on a JEOL (Tokyo, Japan) ECX-400 instrument using tetramethylsilane
as an internal standard (400 MHz). FTIR spectra were recorded on a
JASCO (Tokyo, Japan) FTIR-460 plus spectrometer. Hydrodynamic diameter
and ζ potential were analyzed using DLS on a Malvern Instruments
(Malvern, U.K.) Zetasizer Nano ZS. EDX spectra were recorded on a
JEOL (Tokyo, Japan) JSM-6510A analytical scanning electron microscope.
SEM measurements were conducted on a Hitachi (Tokyo, Japan) SU8000
microscope at an accelerating voltage of 30 kV. TEM measurements were
conducted on a JEOL (Tokyo, Japan) TEM-2100F field emission scanning
electron microscope. The XRD patterns were measured on a Rigaku (Tokyo,
Japan) Ultima IV RINT D/max-kA diffractometer with Cu Kα radiation
(λ = 1.54178 Å) under ambient conditions. TGA was carried
out on a Seiko Instruments (Tokyo, Japan) TG/DTA 6200 (EXSTER6000)
at a heating rate of 10 °C min–1 under N2. The magnetic properties of the composites were analyzed
on a Riken Denshi (Tokyo, Japan) BHV-30 series vibrating sample magnetometer
under ambient conditions. The optical absorbance was measured on an
AS ONE (Osaka, Japan) ASV11D UV–visible spectrophotometer.
Water was deionized on a Nomura Micro Science (Kanagawa, Japan) MINIPURE
TW-300RU.
were recorded on a JEOL (Tokyo, Japan) ECX-400 instrument using tetramethylsilane
as an internal standard (400 MHz). FTIR spectra were recorded on a
JASCO (Tokyo, Japan) FTIR-460 plus spectrometer. Hydrodynamic diameter
and ζ potential were analyzed using DLS on a Malvern Instruments
(Malvern, U.K.) Zetasizer Nano ZS. EDX spectra were recorded on a
JEOL (Tokyo, Japan) JSM-6510A analytical scanning electron microscope.
SEM measurements were conducted on a Hitachi (Tokyo, Japan) SU8000
microscope at an accelerating voltage of 30 kV. TEM measurements were
conducted on a JEOL (Tokyo, Japan) TEM-2100F field emission scanning
electron microscope. The XRD patterns were measured on a Rigaku (Tokyo,
Japan) Ultima IV RINT D/max-kA diffractometer with Cu Kα radiation
(λ = 1.54178 Å) under ambient conditions. TGA was carried
out on a Seiko Instruments (Tokyo, Japan) TG/DTA 6200 (EXSTER6000)
at a heating rate of 10 °C min–1 under N2. The magnetic properties of the composites were analyzed
on a Riken Denshi (Tokyo, Japan) BHV-30 series vibrating sample magnetometer
under ambient conditions. The optical absorbance was measured on an
AS ONE (Osaka, Japan) ASV11D UV–visible spectrophotometer.
Water was deionized on a Nomura Micro Science (Kanagawa, Japan) MINIPURE
TW-300RU.
9
Characterization of Ga-based Complexes
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Chemicals were purchased from commercial sources (like Sigma‐Aldrich, TCI, AlfaAesar, ABCR and Fluka). Indolenine precursors and the protected DOTA chelator were synthesized according to published procedures. 1H, 13C and 71Ga NMR spectra in solution were measured with the spectrometers ECX 400 (400 MHz) and ECP 500 (500 MHz) from JEOL and Avance 500 (500 MHz) and Avance 700 (700 MHz) from Bruker. Mass spectra were measured on a 6210 ESI‐TOF and 6230 ESI‐TOF from Agilent. UV/VIS spectra were recorded using a PerkinElmer LAMBDA 950 UV/Vis/NIR spectrometer and fluorescence spectra recorded using a JASCO FP‐6500 spectrometer. NP automated column chromatography was done on a CombiFlash Rf (Teledyne ISCO) using prepacked silica columns (30 μm). Purification of compounds using size exclusion chromatography was done on a Sephadex column (NAP‐25, Sephadex G‐25 DNA) with water as eluent.
10
Comprehensive Polymer Characterization
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1H NMR spectra
were recorded on a JEOL (Tokyo, Japan) ECX-400 (400 MHz) and ECX-500
(500 MHz) spectrometer. FTIR spectra were recorded on a JASCO (Tokyo,
Japan) FT/IR-460Plus spectrometer. Samples were molded as KBr disks
using KBr dried under reduced pressure with heating above 200 °C
before use. XRD patterns were recorded on a Rigaku (Tokyo, Japan)
RINT RAPID diffractometer with Cu Kα irradiation. The degree
of crystallization was calculated from the intensities of the diffraction
of the 200 lattice at 2θ = 22.6° and the diffraction at
2θ = 18.5°.31 (link) Thermogravimetric
analysis was conducted using Seiko Instruments (Chiba, Japan) EXSTAR
6000 TG/DTA 6200 instrument under a nitrogen atmosphere. Scanning
electron microscopy measurements were conducted on a Hitachi (Tokyo,
Japan) SU8000 microscope at an accelerating voltage of 30 kV.
were recorded on a JEOL (Tokyo, Japan) ECX-400 (400 MHz) and ECX-500
(500 MHz) spectrometer. FTIR spectra were recorded on a JASCO (Tokyo,
Japan) FT/IR-460Plus spectrometer. Samples were molded as KBr disks
using KBr dried under reduced pressure with heating above 200 °C
before use. XRD patterns were recorded on a Rigaku (Tokyo, Japan)
RINT RAPID diffractometer with Cu Kα irradiation. The degree
of crystallization was calculated from the intensities of the diffraction
of the 200 lattice at 2θ = 22.6° and the diffraction at
2θ = 18.5°.31 (link) Thermogravimetric
analysis was conducted using Seiko Instruments (Chiba, Japan) EXSTAR
6000 TG/DTA 6200 instrument under a nitrogen atmosphere. Scanning
electron microscopy measurements were conducted on a Hitachi (Tokyo,
Japan) SU8000 microscope at an accelerating voltage of 30 kV.
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