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8 protocols using nicolet nexus 670 spectrometer

1

Characterization of Nanoparticle Morphology

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A transmission electron microscope (TEM, Jeol JEM-2100F, Tokyo, Japan), operating at 200 kV, was used to characterize the morphology and size of the CDs, MNPs, AuNPs and Fe3O4@Au nanocomposites. Samples for TEM were dropped on holey carbon-coated 400 mesh copper grids. A zeta potential analyzer (Brookhaven Omni, Austin, TX., USA) was used to measure the zeta potential. The morphology of nanoporous alumina membranes was observed by a scanning electron microscope (SEM, Hitachi SU8010, Tokyo, Japan), and the dry samples were coated with gold for 50 s. X-ray diffraction (XRD) patterns were collected on a PANalytical X’Pert PRO powder diffractometer (Almelo, The Netherlands) operated at 40 kV and 40 mA using Cu–Kα radiation. FTIR spectra were obtained with a Thermo Nicolet Nexus 670 spectrometer (Madison, WI. USA) employing KBr optics in the 4000–400 cm−1 region with a resolution of 2.0 cm−1.
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2

Physicochemical Characterization of Nanoparticles

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Fourier transform infrared (FT-IR) spectra were recorded on a Nicolet Nexus 670 spectrometer (Thermo Fisher, Waltham, MA) by using powdered NPs (1 mg) dispersed in KBr (100 mg). Scans were recorded over 3500–1125 cm−1 with the resolution of 2 cm−1 and an average of 32 scans. 1H spectral measurements were performed on a Bruker DRX 400 nuclear magnetic resonance spectrometer (Bruker, Fällanden, Switzerland) using D2O or d6-DMSO as solvent. The mean hydrodynamic particle size and the polydispersity index (PDI) were measured by dynamic light scattering (DLS, 90 Plus Particle Size Analyzer, Brookhaven Instruments, Holtsville, NY). Zeta potential (ZP) was measured by the same instrument equipped with a ZP analyzer as previously described (Song et al., 2017 (link)). The particle size, PDI, and ZP were measured in triplicate. Particle morphology was characterized with a scanning electron microscope (SEM) (FEI Nova TM Nano SEM, FEI, Hillsboro, OR) and transmission electron microscopy (TEM) (JEOL 2010F, Tokyo, Japan) operating at 200 kV using an aqueous solution of the sample (3 mg/mL) dropped onto a carbon-coated copper grid and air dried before TEM analysis.
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3

FT-IR Analysis of Materials

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Thermo Nicolet Nexus 670 Spectrometer was used for FT-IR analysis. Potassium bromide was used as beam splitter, the infra red (IR) with the wavelength of 4000 cm-1 to 400 cm-1, was used as a radiation source at mid IR region (Majzner et al., 2013[20 (link)]). DTGS potassium bromide with resolution of 4 cm-1 was used as a detector.
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4

Synthesis and Characterization of Glutamic Acid Derivatives

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Naphthalene dianhydride, L-glutamic acid, D-glutamic acid, glycine, dry DMF, EDC, Et3N and DIPEA were purchased from Sigma-Aldrich, Bengaluru, Karnataka, India and were used as received. Ethanol (AR grade 99.9%) was purchased from S.D. fine chemicals Limited (SDFCL), India. Robinson-Britton buffer was prepared by using standard protocol (Annali di Chimica, 1974, 64, 409–412). There action solvents were degassed for 10–15 min using nitrogen gas. The reactions were carried out under nitrogen atmosphere. Silica-gel chromatography technique was used to purify the synthesised compounds. 1H and 13C NMR spectroscopy spectra were measured on Bruker Avance-500 MHz and 125 MHz spectrometer at 27 °C. Tetramethylsilane was used as an internal standard. All experiments were performed in deuterated chloroform (CDCl3), CDCl3+ deuterated TFA and DMSO-d6 wherever required. Electron spray ionization method was employed to ionize the samples with a spray voltage. Mass spectrometry measurements were performed using Fourier transform based high resolution mass spectrometry. IR-Spectra were recorded using Thermo Nicolet Nexus 670 spectrometer in the form of non-hygroscopic KBr pellets.
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5

Comprehensive Nanomaterial Characterization Protocols

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Transmission electron microscopy (TEM) was performed on a JEM 1200EX instrument (JOEL, Tokyo, Japan). Scanning electron microscopy (SEM) was undertaken with a Nova Nano microscope (FEI, Hillsboro, OR, USA). Fourier transform infrared (FT-IR) spectroscopy was performed with a Nicolet Nexus 670 spectrometer (Thermo Fisher, Waltham, MA, USA), and UV-vis spectra on a UV-3600 spectrophotometer (Shimadzu, Tokyo, Japan). Dynamic light scattering (DLS) and polydispersity index (PDI) data were collected on a BI-200SM instrument (Brookhaven Instruments, Holtsville, NY, USA). X-ray diffraction (XRD) patterns were measured using a D8 Advance X-ray powder diffractometer supplied with Cu Kα radiation (40 kV, 40 mA;
Bruker, Billerica, MA, USA). N2 adsorption/desorption isotherms were determined on a Tristar 3000 analyzer (Micromeritics, Atlanta, GA, USA), and the resultant data applied to measure the surface area and pore size of the obtained nanoparticles. X-ray photoelectron spectroscopy (XPS)
was conducted with the aid of an Escalab 250Xi (ThermoFisher, Waltham, MA, USA).
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6

Analytical Characterization of Compounds

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Nuclear magnetic resonance (NMR) detection: Bruker AV500 MHz spectrometer (Germany); high-resolution mass spectrometric (HR-MS) detection: Thermo Scientific LTQ Orbitrap XL mass spectrometer (New York, NY, USA); thin-layer chromatography (TLC) detection: silica gel GF-254 plates (Qingdao Haiyang Corporation, China); silica gel: 300–400 mesh (Qingdao Haiyang Corporation, China); elemental analysis: Vario EL element analyzer; ultraviolet detection: UV-2450 ultraviolet visible spectrophotometer; melting point detection: X-5 micro melting point apparatus (Beijing, China); infrared detection: Thermo Nicolet Nexus 670 spectrometer (New York, NY, USA). Yields were calculated based on the last step of the reaction. All of the chemicals and solvents that were used were of analytical or high-performance liquid chromatography grade.
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7

Advanced Materials Characterization

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A JEM 1200EX instrument (JEOL, Tokyo, Japan) was employed to collect transmission electron microscopy (TEM) images. IR spectra were obtained on a Nicolet Nexus 670 spectrometer (Thermo Fisher, Waltham, MA, USA), and UV-vis spectra on a UV-3600 spectrophotometer (Shimadzu, Tokyo, Japan). Dynamic light scattering (DLS) data were obtained with the aid of a Brookhaven Instruments BI-200 SM instrument (Holtsville, NY, USA). A Tristar 3000 analyzer (Micromeritics, Atlanta, GA, USA) was employed to collect N2 adsorption/desorption isotherms.
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8

Characterization of Nanostructured Materials

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Transmission electron microscopy (TEM) measurements were conducted on a JEOL-1010 microscope operated at 100 kV. Scanning electron microscopy (SEM) images were taken with a JEOL-7800F field emission electron microscopy. The N2sorption experiments were performed at 77 K on a Micromeritics Tristar 3000 system with micropore analysis. Prior to the measurement, the samples were degassed at 180 °C for 8 h. The Brunauer-Emmett-Teller (BET) specific surface areas were calculated using adsorption data at a relative pressure (P/P0) range of 0.05-0.25. The total pore volumes were estimated from the amount of nitrogen adsorbed at the maximum P/P0 point. Xray photoelectron spectroscopy (XPS) data was acquired using a Kratos Axis ULTRA X-ray Photoelectron Spectrometer. The atomic ratios were calculated using the Casa XPS version 2.3.14 software and a Shirley baseline with Kratos library Relative Sensitivity Factors. Peak fitting of the high-resolution data was also carried out using the same software. Fourier transform infrared (FTIR) spectra were recorded on a Thermo Nicolet NEXUS 670 spectrometer.
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