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8 protocols using diamond crystal

1

FTIR Analysis of PLGA Residual MeCl

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The presence of residual MeCl in different samples was determined using a Nicolet X Summit Attenuated total reflection Fourier-Transform Infrared Spectroscope with a diamond crystal (ThermoFisher, Waltham, MA, USA) [25 (link)]. Two drops of MeCl were placed on the crystal and covered with a cap to minimize evaporation during analysis. Dry powders of unprocessed PLGA, 1:1 PLGA:MeCl, and optimized PLGA MPs were also placed on the crystal as a thin layer (1 µm) for analysis. FTIR spectra were analyzed using OMNIC® Specta software (ThermoFisher, Waltham, MA, USA).
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2

Investigating AmB-BSA Complex Stability

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Fourier transform infrared-attenuated total
reflectance (FTIR-ATR)
measurements were recorded on a Nicolet iS50 spectrometer using diamond
crystal (Thermo Scientific). The stability of the AmB–BSA complex
was tested at different intervals of incubation time at 37 °C.
5% of D2O was added into the solution phase of every sample
containing AmB, BSA, and AmB–BSA complex, then the samples
were partially dried with nitrogen gas by depositing the sample directly
onto a diamond reflector. A solvent correction was made based on the
D2O band beyond the principal bands used for analyses,
as tested and applied previously.15 (link) Typically,
10 scans were collected, Fourier transform, and averaged for each
measurement. Absorption spectra at a resolution of one data point
every 4 cm–1 were obtained in the region between
4000 and 400 cm–1. An increase in the absorption
spectra was monitored in the Amide I region. Spectral analyses were
performed with Grams software from Galactic Industries.
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3

FTIR Analysis of Wood Photodegradation

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FTIR spectra of the wood surface were recorded on a Nicolet iS10 FT-IR spectrometer (Thermo Fisher Scientific, Waltham, MA, USA) equipped with Smart iTR using an Attenuated Total Reflectance (ATR) sampling accessory with a diamond crystal (Thermo Fisher Scientific). The spectra were recorded in an absorbance mode (A) from 4000 to 650 cm−1 with a spectral resolution of 4 cm−1, and 32 scans were used. Measurements were made on four replicates per sample. The peak at 1030 cm−1 (assigned to CO stretching) was used to normalize the obtained infrared spectra. This band shows little changes during wood photodegradation in a xenotest chamber [17 (link)]. Calculations for changes due to aging were made using the ratio of absorbances A0/At, where A0 is the absorbance of the corresponding peak of the reference sample, and At is the absorbance of the peak at time t.
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4

ATR-IR Spectroscopy of Cellular Materials

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ATR-IR spectra were obtained using a Nicolet iS10 ATR-IR spectrometer with a diamond crystal (Thermo Fisher Scientific, United States). Samples were placed on the crystal and held steady by the specific crimping tool. The experimental set up involved acquisition of 32 scans in the range 500–4000 cm–1, both of sample and background, at a resolution of 4 cm–1 with the sampling depth is approximately 1.6 μm. Beside decellularized and polylysine-enriched samples, the ATR-IR spectrum of polylysine (Sigma-Aldrich, United States) was acquired as a reference.
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5

Analytical Techniques for Molecular Characterization

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Fourier transform
infrared (FTIR) spectroscopy was performed using a Smart iTR ATR sampling
accessory for a Nicolet iS10 spectrometer with a diamond crystal (Thermo
Scientific, Massachusetts). 1H and 13C NMR spectra
were obtained on Varian 300 and 75 MHz NMR spectrometers, respectively,
in tubes with 5 mm outside diameters. CDCl3 or DMSO-d6 containing tetramethylsilane served as a solvent
and shift reference. Thin layer chromatography (TLC) plates were purchased
from Merck (Silica gel matrix coated with a fluorescent indicator
on aluminum plates).
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6

Characterization of Functionalized Halloysite Nanotubes

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To determine the percentage of functionalization of the HNTs, a Q5000 thermal gravimetric analyzer (TGA) (TA Instruments Ltd., New Castle, DE, USA) was used. In a nitrogen atmosphere, the heating rate was 10 °C/min from 30 °C to 800 °C. The top surface morphology of the membranes was evaluated using scanning electron microscopy (SEM). All of the samples were coated by gold sputtering. Attenuated Total Reflection-Fourier Transform Infrared (ATR-FTIR) spectra of the membranes (TFC and TFN membranes) and NPs were obtained using a Nicolet 6700 FT-IR instrument with a diamond crystal (Thermo Fisher, Waltham, MA, USA). OMNIC ™ software was utilized to analyze the spectra. To investigate the TFC and TFN membranes’ hydrophilicity, a VCA Optima goniometer (AST Products, Inc., Billerica, MA, USA) was used. The morphology of the nanoparticle was characterized using a TEM (Philips CM30, Algonquin, IL, USA) instrument. The zeta potential of the surface of membranes was determined using a zeta analyzer (Zetasizer PSS0012-22, Malvern Instruments, Westborough, MA, USA).
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7

Characterization of Surface-Modified Magnetic Nanoparticles

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FTIR measurements were carried out in Attenuated Total Reflectance (ATR) mode using the Nicolet iS10 apparatus with an adapter equipped with a diamond crystal (Thermo Scientific). Measurements were carried out in the mid-infrared range (500–4000 cm−1) using: (i) solid samples of nanoparticle powders and (ii) surface modifiers in their pure form. Thermogravimetric analysis (TGA) was carried out using a TGA/DSC3+ thermogravimeter (Mettler Toledo) at a temperature increment 10 °C/min in a temperature window of 25–750 °C and air flow rate 60 mL/min. The total content of C, H, and N elements in modified MNPs was measured using a Vario EL III analyzer with a thermal conductivity detector (Elementar, Langenselbold, Germany) by the accurate weighting of the solid sample and its burning in oxygen at 1150 °C in a dynamic system. Fe, Au, and Si content in solid MNPs was established using the ICP-MS/MS technique, analogically to the methodology presented above (see Section 3.3.2; monitored isotopes: 28Si, 56Fe, 197Au at on-mass mode), but solid samples before digestion were accurately weighted. The oxygen content in the cores of surface-modified MNPs was estimated using the molar ratio of Fe/O in the synthesized bare MNPs as the rest types of the nanomaterials were formed based on such cores (with specific FeO/Fe2O3 ratio).
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8

FT-IR Analysis of Wood Surface

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Fourier transform-infrared spectroscopy (FT-IR) spectra of the wood surface were recorded on the Nicolet iS10 FT-IR spectrometer, equipped with Smart iTR using an attenuated total reflectance (ATR) sampling accessory attached to a diamond crystal (Thermo Fisher Scientific). The spectra were from 4000 to 650 cm -1 at a spectral resolution of 4 cm -1 , and 64 scans were used. Measurements were performed on four replicates per sample.
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