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10 protocols using universal atr

1

FTIR Spectroscopy of Microsamples

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The FTIR spectra were obtained using a Spectrum Two FT-IR spectrometer equipped with a Universal ATR with a diamond crystal (PerkinElmer, Waltham, MA, USA). The data were collected over the 4000–500 cm−1 spectral range. Typically, a few microliters were used on the diamond, and the measurements were repeated three times for each sample.
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2

Characterization of βCD-B Complex

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The formation of the βCD–B complex was confirmed by a PerkinElmer Spectrum Two FTIR spectrometer equipped with a universal ATR (PerkinElmer, Waltham, MA, USA). Three replicates of ATR–FTIR spectra were obtained for every sample in the spectral range of 4000 to 400 cm−1 at a resolution of 4 cm−1. All the spectra were baseline-corrected interactively using Spectrum® Quant software (PerkinElmer, Waltham, MA, USA).
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3

Characterization of Date Fruit Melanin

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The method of Hou et al.38 (link) was followed for preliminary identification of extracted melanin. Solubility of date fruit melanin (10 mg) was tested in acetic acid, acetone, chloroform, distilled water, Dimethyl sulfoxide (DMSO), ethanol, ethyl acetate, methanol, 1 M hydrochloric acid, 1 M sodium hydroxide/sodium carbonate (20 mL each) after shaking and letting stand for 3 h. The pigment was also precipitated with 1% FeCl322 (link). The color of the melanin samples was measured as l*, a*, and b* color values using Hunter Lab colorimeter (Hunter Lab Inc., Reston, VA, USA). Melanin samples (0.5 g) were dissolved in NaOH (0.01 M 100 mL) to get 0.5% melanin solution, and after 5 min of sonication, its UV–visible spectra were scanned from the range of 200–700 nm using a BioTek EPOCH 2 Microplate spectrophotometer (Agilent, Santa Clara, USA)39 (link). Attenuated total reflectance spectroscopy (ATR-FTIR) was performed using Spectrum Two IR coupled with Universal ATR (Perkin-Elmer inc., Norwalk, CT, USA). Date fruit melanin was placed on the ATR diamond crystal plate and scanned in the spectral range from 4000 cm−1 to 400 cm−1 at room temperature.
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4

Spectroscopic Analysis of Organic Compounds

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Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Fourier 300 spectrometer and a Bruker Fourier 400 spectrometer (Bruker, Billerica, MA, USA). Melting points were determined on a Stuart Scientific SMP10 AC/DC input, 230 V (Merck, Darmstadt, Germany). Optical rotations were measured on an Anton Paar MC100 polarimeter (in CHCl3 solution) (Anton Paar, Graz, Austria). Attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FT-IR) spectra were collected on a Perkin-Elmer Spectrum Two FT-IR spectrophotometer with Universal ATR (Perkin-Elmer, Shelton, CT, USA). LC-HRMS was performed on a Dionex Ultimate 3000 UHPLC+ system equipped with a multiple-wavelength detector, using an imChem Surf C18 TriF 100 A 3 µm 100 × 2.1 mm column, a linear solvent gradient from 20 to 30% aqueous ACN over 10 min, 0.2 mL of min−1, and UV detection at 250 nm, connected to a Thermo Scientific Q-Exactive hybrid quadrupole-Orbitrap mass spectrometer (Thermo Scientific, Waltham, MA, USA). All solvents were distilled from commercial-grade sources. Pyridine (Merck, Darmstadt, Germany) and all benzoyl and anhydride reagents were used without any previous purification.
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5

Spectroscopic Analysis of Organic Compounds

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Optical rotation was measured on a Rudolph Research Analytical AUTOPOL III automatic polarimeter. UV spectra were collected on a NanoDrop Spectrophotometer (Thermo Fisher Scientific, Inc., Waltham, MA, USA). NMR data was collected on a JEOL ECA-600 spectrometer (JEOL USA, Peabody, MA, USA) operating at 600 MHz for 1H, and 150.9 for 13C. The edited gHSQC spectrum was optimized for 140 Hz and the gHMBC spectrum optimized for 8 Hz. Chemical shifts were referenced to solvent, e.g., CD3OD, δH observed at 3.31 ppm and δC observed at 49.1 ppm. High-resolution mass spectrometry for 1 was performed on a JEOL AccuTOF-DART 4G (JEOL USA, Peabody, MA, USA) using the ESI source for ionization and detected in positive ion mode. High-resolution mass spectrometry for 2 was performed on a Thermo Fisher Orbitrap (Thermo Fisher Scientific, San Jose, CA, USA) using the ESI source for ionization and detected in positive ion mode. IR data was collected on a Perkin Elmer Spectrum 100 with Universal ATR (Perkin Elmer, Waltham, MA, USA).
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6

FT-IR Analysis of Microsamples

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FT-IR spectra were determined by the spectrum Two FT-IR spectrometer with a Universal ATR with a diamond crystal (PerkinElmer, Waltham, MA, USA). The experiment was set up for all available spectral ranges (500–4000 cm−1). Typically, a microgram of the sample was put on the diamond crystal in the ATR system with a controlled force gauge. The measurements were conducted three times for each fraction sample.
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7

Characterization of Nanohydroxyapatite using FTIR and XRD

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Fourier transform infrared spectroscopy analysis. The functional group present in the prepared nHAp were identified using FTIR (Perkin Elmer Universal ATR). An initial background check was carried out before scanning. Thereafter, a few quantities of the nHAp were dropped in the sample holder and scanned at a resolution of 4 cm -1 . The range of scan was 400 to 4500 cm -1 .
X-ray diffraction analysis. The crystallinity of the prepared nHAp was studied using X-ray diffraction (XRD). The XRD patterns were documented using a diffractometer (D8 Advance BRUKER AXS instrument Germany instrument; Cu-Ka radiation (lKa1 = 1.5406 Å). The operating condition includes a pass time of 0.5 s, a voltage of 40 Kv, and current of 40 mA. The range of analysis was 0 to 90 (2θ).
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8

FTIR Spectra of Organic Compounds

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The FTIR spectra were obtained using a Spectrum Two FT-IR Spectrometer equipped with a Universal ATR with a diamond crystal (PerkinElmer, Waltham, MA, USA). The data were collected over a spectral range of 400–500 cm−1.
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9

Infrared Spectroscopy of Samples

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The FTIR spectra were obtained using a Spectrum Two FT-IR spectrometer equipped with a Universal ATR with a diamond crystal (PerkinElmer, Waltham, MA, USA). The data were collected over a spectral range of 4000–500 cm−1. The measurements were repeated three times for each sample.
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10

Thermal and Structural Analysis of POM Nanosuspension

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ATR-FT-IR spectra were acquired with a Perkin Elmer Spectrum One FT-IR (Perkin Elmer, Waltham, MA, USA), equipped with a Perkin Elmer Universal ATR sampling accessory consisting of a diamond crystal. Analyses were performed in a spectral region between 4000 and 650 cm - and analysed by transmittance technique with 28 scansions and 4 cm - resolution.
Differential Scanning Calorimetry analyses were performed to characterize the thermal behavior of POM and corresponding nanosuspension using a Perkin Elmer DSC 6 Waltham, MA, USA. All experiments were conducted at a heating rate of 10 • C/min up to 350 • C in a nitrogen atmosphere purging nitrogen at a flow rate of 20 mL/min. Samples (2-3 mg) were hermetically sealed in an aluminum pan and a control empty pan subjected to the same heating conditions was used as reference.
The XRPD analyses were performed with a Rigaku MiniFlex diffractometer by using a CuKα radiation detector (λ = 1.54056 Å) as source of X-rays. The voltage and current were of 30 kV and 15 mA, respectively. Measurements were undertaken at scan angular speed of 2 • C/min, and a scan step time of 2.00 s in the range from 3 • to 60 • C. The diffractograms are expressed as peak intensity versus 2θ.
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