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32 protocols using spectrum bx ft ir spectrometer

1

Synthesis and Characterization of Novel Compounds

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Reagents were purchased from Sigma-Aldrich (St. Louis, MO, USA). The reaction course and purity of the synthesized compounds were monitored by TLC using aluminum plates pre-coated with silica gel 60 F254 (MerckKGaA, Darmstadt, Germany). Melting points were determined on a MEL-TEMP (Electrothermal, Bibby Scientific Company, Burlington, NJ, USA) melting point apparatus and are uncorrected. IR spectra (ν, cm−1) were recorded on a Perkin–Elmer Spectrum BX FT-IR spectrometer (PerkinElmer, Inc., Waltham, Massachusetts, United States) using KBr pellets. The 1H and 13C-NMR spectra were recorded in DMSO-d6 on a Bruker Avance III (400 MHz, 101 MHz) spectrometer. Chemical shifts (δ) are reported in parts per million (ppm) calibrated from TMS (0 ppm) as an internal standard for 1H NMR, and DMSO-d6 (39.43 ppm) for 13C NMR. Elemental analyses (C, H, N) were performed on an Elemental Analyzer CE-440 (Exeter Analytical, Inc., North Chelmsford, MA, USA). Compounds 2-23 and 25-42 synthesis methods, identification data and NMR spectra can be found in Supplementary Materials file. The peak shapes are denoted as follows: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad.
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2

FTIR Spectroscopy Analysis Protocol

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FTIR spectroscopy was assessed with a Perkin-Elmer Spectrum BX FTIR™ spectrometer from 1200 cm−1 to 400 cm−1 with a resolution of 4 cm−1 and 128 co-added scans. The data acquisition was performed at room temperature (approximately 25 °C) and with 37% of humidity.
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3

Characterization of Organic Compounds by NMR and MS

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All chemicals were purchased from commercial suppliers and were used as received unless otherwise stated. Proton Nuclear Magnetic Resonance NMR (1H NMR) spectra and carbon nuclear magnetic resonance (13C NMR) spectra were recorded on a Varian Unity Plus 400, Varian MR400, Varian vnmrs 500, Varian Inova 500, Varian Mercury 500, and Varian vnmrs 700 spectrometers. Chemical shifts for protons are reported in parts per million and are references to the NMR solvent peak (CDCl3: δ 7.26). Chemical shifts for carbons are reported in parts per million and are referenced to the carbon resonances of the NMR solvent (CDCl3: δ 77.23). Data are represented as follows: chemical shift, multiplicity (br = broad, s = singlet, d = doublet, t = triplet, q = quartet, dq = doublet of quartet, ddq = doublet of doublet of quartet, p = pentet, dd = doublet of doublet, ddd = doublet of doublet of doublet, hept = heptet, m = multiplet), coupling constants in Hertz (Hz) and integration. Mass spectroscopic (MS) data was recorded at the Mass Spectrometry Facility at the Department of Chemistry of the University of Michigan in Ann Arbor, MI on an Agilent Q-TOF HPLC-MS with ESI high resolution mass spectrometer. Infrared (IR) spectra were obtained using either an Avatar 360 FT-IR or Perkin Elmer Spectrum BX FT-IR spectrometer. IR data are represented as frequency of absorption (cm−1).
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4

FTIR Spectroscopy Analysis Protocol

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FTIR spectroscopy was assessed with a Perkin-Elmer Spectrum BX FTIR™ spectrometer from 1200 cm−1 to 400 cm−1 with a resolution of 4 cm−1 and 128 co-added scans. The data acquisition was performed at room temperature (approximately 25 °C) and with 37% of humidity.
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5

FTIR Analysis of Gel Samples

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In order to record the FTIR spectra of gels and samples of dried gels in an oven, up to constant weight at 30 °C, a Spectrum BX FTIR spectrometer (PerkinElmer, Sunnyvale, CA, USA) provided with an Attenuated Total Reflectance (ATR PIKE MIRacleTM, Madison, WI, USA) with a diamond crystal plate was used. The resolution was 2 cm−1 in the range of 4000–800 cm−1.
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6

Photophysical Characterization of Luminescent Materials

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All reagents and solvents were obtained commercially and used without further purification. The FT-IR spectra were recorded from KBr pellets in range 400–4000 cm–1 on a Perkin-Elmer Spectrum BX FT-IR spectrometer. Elemental analysis was performed on a Vario EL-II elemental analyzer. XRPD data were recorded in a Bruker D8 ADVANCE X-ray powder diffractometer (Cu, λ = 1.5418 Å).
Steady-state photoluminescence spectra and lifetime measurements were measured from 300 K down to 5 K by a single-photon counting spectrometer using an Edinburgh FLS920 spectrometer equipped with a continuous Xe-900 xenon lamp, and a μF900 microsecond flash lamp. The corrections of excitation and emission for the detector response were performed ranging from 200 to 900 nm. Temperature-dependent measurements were carried out in a JANIS SHI-4S-1 cold head cooled with HC-4A compression engine. The data were analyzed by iterative convolution of the luminescence decay profile with the instrument response function using the software package provided by Edinburgh Instruments. Lifetime data were fitted with triple-exponential-decay functions. The quantum yields were measured by use of an integrating sphere with Edinburgh Instrument FLS920 spectrometer.
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7

Comprehensive Analytical Characterization

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Infrared (IR) spectra were recorded with a Perkin-Elmer spectrum BX FTIR spectrometer. Ultraviolet (UV) spectra were obtained using a Shimadzu UV-2600 UV–vis spectrophotometer in MeOH. ECD spectra were recorded on a JASCO J-815 polarimeter. 1H and 13C nuclear magnetic resonance (1H and 13C NMR) spectra were recorded on 300 and 500 MHz Bruker FTNMR Ultra ShieldTM spectrometers. Specific rotations were measured with a JASCO P-2000 polarimeter. ESI-TOF mass spectra were obtained using a TOF/Q-TOF Mass spectrometer. Thin-layer chromatography (TLC) and preparative TLC were performed on silica gel 60 GF254 (Merck). Column chromatography (CC) was conducted on silica gel (Merck) type 100 (70–230 mesh ASTM) and type 60 (230–400 mesh ASTM), Sephadex LH-20, or reversed-phase C18 silica gel.
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8

Synthesis and Characterization of Novel Compounds

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Reagents and solvents were purchased from Sigma-Aldrich (St. Louis, MO, USA) and used without further purification. The reaction course and purity of the synthesized compounds were monitored with TLC using aluminum plates pre-coated with Silica gel at F254 nm (Merck KGaA, Darmstadt, Germany). Melting points were determined with a B-540 melting point analyzer (Büchi Corporation, New Castle, DE, USA) and were uncorrected. NMR spectra were recorded with a Brucker Avance III (400, 101 MHz) spectrometer. Chemical shifts were reported in (δ) ppm relative to tetramethylsilane (TMS) with the residual solvent as an internal reference ([D6]DMSO, δ = 2.50 ppm for 1H and δ = 39.5 ppm for 13C). The data are reported as follows: chemical shift, multiplicity, coupling constant [Hz], integration, and assignment. The IR spectra (ν, cm−1) were recorded with a Perkin–Elmer Spectrum BX FT–IR spectrometer using KBr pellets. Mass spectra were obtained with a Bruker maXis UHRTOF mass spectrometer with ESI ionization.
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9

Multimodal Imaging of Bacterial Biofilms

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The proper assessment of the existence, the quality and topography of the BFF used the following imaging techniques: OCT, SEM and FTIR. The OCT measurements were performed by an OCTG-1300 Handheld Scanner (THORLABS GmbH, Luebeck, Germany) equipped with an OCTH-LK30 lens kit (THORLABS GmbH, Luebeck, Germany). The images were further processed using Adobe Photoshop to emphasize the biofilm by coloring in a different shade for each strain.
The SEM images were obtained using a JEOL/JSM 5600-LV (JEOL Ltd., Tokyo, Japan). For this technique samples were washed with absolute ethanol and were further carbon layered with plasma sputtering equipment.
In order to record the FTIR spectra of the bacterial biofilms formed on the surface of the PLA printed plates, a Spectrum BX FTIR spectrometer (PerkinElmer, Sunnyvale, CA, USA) provided with an Attenuated Total Reflectance (ATR PIKE MIRacleTM, Madison, WI, USA) with a diamond crystal plate was used. The resolution was 4 cm−1 in the range of 4000–800 cm−1. For this characterization step, no sample preparation was necessary. Using the attenuated total reflection (ATR) accessory alongside the traditional infrared spectroscopy allowed for a direct visualization of the characteristic spectra of the biofilms.
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10

Synthetic Characterization of Organic Compounds

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All commercially available chemicals of the appropriate purity were purchased from Merck (Kenilworth, NJ, U.S.A.) or Sigma ((St. Louis, MO, U.S.A.). The IR spectra were recorded on a Perkin Elmer Spectrum BX FT-IR spectrometer (Waltham, MA, U.S.A.). The 1H NMR and 13C NMR spectra were recorded using a BRUKER Avance III-300 MHz (Billerica, MA, U.S.A.) or an AGILENT DD2-500 MHz ((Santa Clara, CA, U.S.A.) spectrometer. Chemical shifts were reported in δ (ppm) and signals were given as follows: s, singlet; d, doublet; t, triplet; m, multiplet. Melting points (mp) were determined with a MEL-TEMPII apparatus, Laboratory Devices, Sigma-Aldrich (Milwaukee WI, U.S.A) and were uncorrected. The microanalyses were performed on a Perkin-Elmer 2400 CHN elemental analyser (Waltham, MA, U.S.A.). Thin-layer chromatography (TLC silica gel 60 F254 aluminium sheets, Merck (Kenilworth, NJ, U.S.A.) was used to follow the reactions and the spots were visualised under UV light.
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