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24 protocols using spectrum 400 spectrometer

1

Physicochemical Characterization of Lasalocid-Carrier Dispersions

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SDs of lasalocid with carriers of PVP K30 (Sigma-Aldrich, St Louis, MO, USA), PEG 4000 (BDH, London, UK), Pluronic® F68 (Sigma-Aldrich), or Soluplus® (BASF, Ludwigshafen, Germany) were prepared at different ratios (lasalocid:carrier 3:1, 5:1, or 9:1) by a conventional solvent evaporation method. Briefly, lasalocid and carriers were dissolved in a minimum volume of methanol, and the solvent was removed under vacuum in a Rotavapor at 50°C and 30 rpm for 5 hours, until all trace of methanol was removed. The solid products were then crushed out by a spatula and milled in a blender.
The DSC curves of pure lasalocid and each dispersion system were recorded on a TA Thermal Advantage™ DSC thermal analyzer (New Castle, DE, USA). Thermal behavior was studied by heating the samples (2–4 mg) in a sealed aluminum crucible, using an empty crucible as reference, over the temperature range 15–400°C at a rate of 10°C/minute.
FT-IR spectra were measured on a PerkinElmer Spectrum 400 spectrometer equipped with an attenuated total reflectance (ATR, top-plate type) accessory (PerkinElmer, Waltham, MA, USA). A ~0.05 g sample was mounted onto crystal using air as a background reference before each scan. The samples were scanned over the range of 400–4,000 cm−1 at a resolution of 2 cm−1.
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2

Characterization of Functionalized Magnetic Nanochains

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The RB-nanochain-COOH structure was assessed by transmission electron microscopy (TEM). A drop of RB-nanochains-COOH suspension was deposited on a copper grid coated with a perforated, transparent carbon foil. The suspension was dried prior to TEM observations performed with a transmission electron microscope (Jeol, JEM, 2100, Akishima, Japan), operating at 200 kV. Magnetic properties of the RB-nanochains-COOH were measured at room temperature by vibrational sample magnetometry (VSM) (Lake Shore 7307 VSM). The zeta-potential measurements as a function of the pH of the RB-nanochains, RB-nanochains-NH2, and RB-nanochains-COOH suspensions (volume 15 mL) at final nanochains concentration of 0.2 mg/mL were monitored in an aqueous solution containing KCl (final concentration 10 mM). Zeta-potential measurements were performed on Zeta PALS, Brookhaven Instruments Corporation. FTIR-ATR analysis of the powders of the freeze-dried samples (RB-nanochains-NH2, and RB-nanochains-COOH; 15–20 mg each) was performed on Perkin Elmer, Spectrum 400 Spectrometer. The quantitative analysis of primary amines of the RB-nanochains-NH2 was determined by Keiser test, where accurately weighed 10 mg of the freeze-dried RB-nanochains-NH2 was applied in the reaction with ninhydrin while following the manufacturer’s protocol specified in the Kaiser kit.
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3

FTIR Analysis of Soybean Phospholipids

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FTIR analysis of OS extract, soybean phospholipids and OS liposomes was carried out using Spectrum 400 spectrometer (Perkin Elmer, USA). The IR spectra were recorded in the range of 4000 – 400 cm−1 (n = 3).
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4

Spectroscopic and Magnetic Characterization

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UV–visible–NIR
spectra were measured in KBr pellets on a PerkinElmer Lambda 1050
spectrometer in the 250–2500 nm range. Fourier transform infrared
spectra were obtained in KBr pellets with a PerkinElmer Spectrum 400
spectrometer (400–7800 cm–1). EPR spectra
were recorded for sealed polycrystalline samples of 6 in the 4–295 K temperature range with a JEOL JES-TE 200 X-band
ESR spectrometer equipped with a JEOL ES-CT470 cryostat. A Quantum
Design MPMS-XL SQUID magnetometer was used to measure static magnetic
susceptibility of 15 at 100 mT magnetic
field in cooling and heating conditions in the 300–1.9 K range.
A sample holder contribution and core temperature-independent diamagnetic
susceptibility (χd) were subtracted from the experimental
values. The χd values were estimated by the extrapolation
of the data in the high-temperature range (150–300 K for 13 and 240–300 K for 4, 20–300 K for 5) by fitting the data with the
following expression: χM = C/(TΘ) + χd, where C is the Curie constant and Θ is the Weiss temperature. Effective magnetic moments (μeff) were calculated with the formula: μeff = (8·χM·T)1/2.
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5

Characterization of Functionalized Halloysite Nanotubes

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FTIR-ATR spectra were obtained with a Perkin Elmer SPECTRUM 400 spectrometer (Waltham, MA, USA) using a ZnSe trapezoidal shaped ATR element. Sample spectrum and background were acquired with the coated ATR element and the clean ATR element, respectively. The spectra were acquired with a resolution of 4 cm−1 and 16 scans. An FEI Nova NanoSEM 200 scanning electron microscope (SEM) (Hillsboro, OR, USA), with an acceleration voltage of 15 kV, and secondary electron detector under vacuum, was used to characterize the morphology of the untreated and functionalized HNTs. The Energy-dispersive X-ray spectroscopy (EDS) elemental analysis was performed using an INCA X-Sight (Abingdon, UK). XRD analysis was performed by an Empyrean PANalytical diffractometer (Boulder, CO, USA) with an X’Cellerator detector in a continuous mode scanning with a start angle of 30.000°, and end angle of 100.000°, a step size of 0.02, and time per step of 1 s. An X-ray tube copper wavelength (λ) of 1.5405 was used, at a voltage of 45 kV, and current of 40 mA. Decomposition temperatures of samples were determined by thermogravimetrical analysis (TGA) with a TA Instruments SDT Q600 (New Castle, DE, USA). All samples were heated al 10 °C/min from room temperature (25 °C) to 850 °C under 100 mL/min nitrogen purge.
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6

FTIR-ATR Analysis of Seaweed Polysaccharides

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The Fourier Transform Infrared Spectroscopy—Attenuated Total Reflection (FTIR-ATR) examination is a methodology of infrared spectroscopy that is frequently used to investigate and characterize carbohydrates found in seaweeds (among other chemicals) and is based on the procedure outlined by Pereira, Gheda and Ribeiro-Claro (2013) [30 (link)].
The dried polysaccharide samples from the previous polysaccharide extraction phases were powdered using a commercial mill and subjected to direct examination without further preparation for FTIR-ATR analysis. This technique requires only a dried milled (<1 mm) sample to be evaluated.
FTIR-ATR spectra were recorded on an Perkin Elmer Spectrum 400 spectrometer (Waltham, MA, USA), with no need for sample preparation, since these assays only required dried samples [31 (link)]. All spectra are the average of two independent measurements from 650 to 1500 cm−1 with 128 scans, each at a resolution of 2 cm−1.
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7

Synthesis and Characterization of Fe-Pt Nanoparticles

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For the synthesis of the Fe–Pt NPs, a hemispherical heating mantle (model WiseTherm WHM 12112 from Witeg Labortechnik GmbH) connected to a temperature controller (J-KEM, model 310) with a J-type Teflon thermocouple was used. The samples were characterized using a (scanning) transmission electron microscope (TEM Jeol JEM-2010F) equipped with energy-dispersive X-ray spectroscopy (EDXS). Low-temperature magnetic measurements were performed on a Quantum Design MPMS-XL-5 SQUID magnetometer. With the thermogravimetric analyses (TG analyser NETZSCH STA 449 C/6/G Jupiter) the amount of organic matter in the sample was determined to be 30%. The magnetization values are reported for the mass of Fe–Pt in the sample after the subtraction of the organic content. Fourier-transform infrared spectroscopy (FTIR) measurements were performed using a Spectrum 400 spectrometer (Perkin Elmer, USA). The spectra were recorded on dried samples in the wavenumber range 4000–650 cm−1.
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8

Bentonite Modification and Characterization

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First, 10 g of dry
bentonite powder was put into the pressure chamber and compacted using
1000 psi for 30 min to prepare the bentonite wafer. Then, the bentonite
wafers were soaked in water and water–inhibitor solutions for
24 h. The wet bentonite was taken out of the solutions and dried in
an oven at 80 °C temperatures for approximately 16 h. After that,
the dried bentonite was crushed into fine powder by pestle and mortar.
The IR spectral of the powder bentonite modified with inhibitors was
measured by a PerkinElmer Spectrum 400 spectrometer. The experiment
was carried out at room temperature between 4000 and 400 cm–1.
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9

Physicochemical Characterization of Complexes

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The metal contents of the complexes were measured by inductively coupled plasma optical emission spectrometry (ICP-OES) at 25 ± 0.1°C using an Agilent 5110. The size and morphology of the complexes were characterized by transmission electron microscopy (TEM) using an FEI Tecnai G2 F20. The size distribution was determined by measuring at least 50 microspheres from TEM images followed by statistical treatment. The microstructures of the samples were observed by scanning electron microscopy (SEM) with a SEU8010. The zeta potentials of the complexes were measured using a Zetasizer nano. Samples were mixed in absolute ethanol with a concentration of 0.1% (w/v) and immediately transferred into the quartz cuvette for determination. Fourier transform infrared (FTIR) spectra were recorded in the range of 400–4,000 cm−1 using a Perkin-Elmer Spectrum 400 spectrometer. The powder samples were dried and ground with potassium bromide in a volume ratio of 1:100. The elemental composition and chemical status of the electrodes were analyzed by X-ray photoelectron spectroscopy (XPS, EscaLab 250, Thermo Fisher Scientific) with a monochromatic Al Kα as the excitation source. The energy calibration was made against the C 1s peak. Thermogravimetric (TG) analyses were performed with a NETZSCH STA 449F3 at the heating rate of 10°C·min−1 from 30 to 500°C in a dynamic nitrogen atmosphere.
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10

Analytical Characterization of Organic Compounds

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All chemicals are commercially available and used as received. The elemental analyses for C, H, and N were carried out on a Thermo Finnigan Flash EA 1112 (Thermo Scientific, Hudson, NH, USA). The infrared spectra were obtained on a Perkin-Elmer Spectrum 400 spectrometer with samples as KBr pellets in the region 4000–400 cm-1. The UV-vis spectra were obtained using a Shimadzu UV-vis-NIR 1600 spectrophotometer. 1H-NMR spectra were recorded on a JEOL FT-NMR lambda 400 MHz spectrometer. The solvent was DMSO-d6. The chemical shifts were reported in ppm using the residual protonated solvent as the reference.
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