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29 protocols using flash 2000 chns o analyzer

1

Synthesis and Characterization of Schiff Base

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All chemicals were obtained from the Aldrich (Saint Louis, MO, USA), TEDIA (Fairfield, OH, USA), and Merck (Rahway, NJ, USA) companies. The melting point of the synthesized Schiff base was determined by employing an electrothermal melting point SMP 10 apparatus. The FTIR spectrum was detected using an FTIR Bruker-ATR (Leipzig, Germany). A Bruker Avance III −500 MHz was used to record the 1H and 13C NMR spectra in DMSO solvent. The mass spectra were recorded on a Brucker apex-IV. The UV–visible spectrum of the Schiff base–DMSO solution was recorded in the range from 200 to 900 nm using a SPECORD PLUS by Analytik Jena AG. GCMS ISQ models from Thermo Scientific were used for direct inlet mass spectrometry, and the FLASH 2000 CHNS/O analyzer was used to determine the elemental contents of the synthesized compounds.
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2

Synthesis and Characterization of Novel Compounds

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Starting materials, reagents and solvents were purchased from Sigma−Aldrich (USA), Alfa−Aesar, Loba Chemie Organics, Fisher scientific or Sigma−Aldrich and were used without further purification. Column chromatography was conducted on silica 60 (35–70 microns). Melting points were recorded on a Stuart SMP10 melting point apparatus. IR spectra (KBr) were recorded on a Perkin−Elmer spectrophotometer.1H-NMR spectra were recorded on a Bruker 400 MHz spectrometer in δ scale (ppm), using DMSO as solvent at special unit facility, Faculty of Pharmacy, Ain−shams University. EI−MS spectra were recorded by Triple Quadrupole LC/Ms/Ms mass spectrometer API 200 (AB Sciex Instrument) at the regional center of mycology and biotechnology et al.−Azhar University, Egypt. Elemental analyses were determined at the same center utilizing FLASH 2000 CHNS/O analyzer, Thermo Scientific. Compounds (1, 2, 3, 4, 5, 6a−c, 6e, 6g, 6h, 7a−c, 7e, 7g and 7h) were prepared according to the reported procedures [12 –20 ].
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3

Synthesis and Characterization of Sulfonyl Compounds

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All chemicals were purchased off the analytical grade. 4-bromomethylbenzenesulfonyl chloride, 1,3-diaminopropane, 4-nitrobenzene-sulfonyl chloride, and Et3N from Sigma-Aldrich (USA). All solvents from Tedia (USA). Tris, FeCl3, AlCl3, and K2CO3 from Merck (Germany). Uranyl nitrate from BDH (England) and the uranium nitrate standard solution (1000 μg/mL U in 2%–5% aqueous HNO3) from AccuStandard, (USA).
1H-NMR and 13C-NMR were done on a 400 MHz Bruker instrument using DMSO as a solvent. The infrared spectra were recorded on a Tensor II FT-IR spectrometer with an ATR attachment from Bruker. UV-Vis spectra were recorded using a SPECORD 200 PLUS spectrophotometer, Analytik-Jena (Germany). Elemental analysis was performed using a FLASH 2000 CHNS/O Analyzer, Thermo-Scientific (USA). Thermal gravimetric analysis (TGA) was observed at a rate of 10 °C/min up to 900 °C under N2 in alumina crucibles using a Netzsch TG 209F1 instrument. The sample mass range was 4.74–13.55 mg.
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4

Elemental Composition Analysis Protocol

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The elemental composition was determined using a Thermo ScientificTM FLASH 2000 CHNS/O Analyzer (Waltham, MA, USA) mounted with a thermal conductivity detector. The samples were prepared in crucibles made of tin (CHNS analysis) or silver (O analysis) and weighed with an accuracy of 0.000001 g. The composition of specific elements was determined using the calibration curve. L-cysteine, L-methionine, and sulphanilamide were used as standards in CHNS mode, while acetanilide and benzoic acid were used for calibration in O-mode, respectively.
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5

Characterization of Chemical Compounds

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NMR spectra was obtained using Bruker-400 MHz NMR spectrometer (1H at 400 MHz and 13C{1H} at 100 MHz). Spectrometer chemical shifts were reported relative to the internal standard tetramethylsilane (δ 0.00 ppm) and referenced to the residual proton and carbon signals at 7.24 and 77.0 ppm respectively of CDCl3. Infrared spectra were obtained neat using a Perkin Elmer Spectrum BX II fitted with an ATR probe. Melting points were obtained using a Gallenkamp Digital Melting-point Apparatus 5A 6797. Elemental analysis was performed on a Thermos Scientific FLASH 2000 CHNS-O Analyzer. Mass spectrometry was performed using Waters Synapt G2 mass spectrometer with both ESI positive and cone voltage 15 V. XRD spectra were obtained from a Bruker APEX-II CCD Diffractometer. Analytical thin layer chromatography (TLC) was performed on silica gel coated aluminium plates (0.2 mm). Developed plates were visualized with UV light or under iodine staining. Silica gel column chromatography was performed using silica gel 60 (70–230 mesh).
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6

Elemental Composition Analysis Protocol

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The determination of elemental composition was carried out on Thermo Scientific™ FLASH 2000 CHNS/O Analyzer (Waltham, MA, USA). 2,5-Bis(5-(tert-butyl)-2-benzo-oxazol-2-yl)thiophene, l-cysteine, l-methionine, and sulphanilamide were used as standards in CHNS-mode and acetanilide and benzoic acid were used for calibration in O-mode respectively. The samples were prepared in a tin (CHNS analysis) or silver (O analysis) crucibles and were weighed with an accuracy of ±0.000001 g.
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7

Synthesis and Characterization of Iridium(III) Complexes

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All reactions were carried out in air unless otherwise stated. All solvents used were reagent grade, purchased from Sigma-Aldrich, and dried under nitrogen before use. 1-Phenyl-1H-tetrazole-5-thiol, chlorodiphenylphosphine, chlorobis(3,5-dimethylphenyl)phosphine, bis(3,5-di(trifluoromethyl)phenyl)chloro phosphine, and sodium methoxide were purchased from Sigma-Aldrich and used without further purification. Iridium(III) chloride was purchased from Heraeus South Africa and used as received. [Ir(C5Me5)Cl2]2 (White et al., 1992 ) was synthesized according to literature procedures. NMR spectra were recorded on a Bruker 400-MHz NMR spectrometer (1H at 400 MHz, 13C{1H} at 100 MHz, and 13P{1H} NMR 161.99 MHz). Spectrometer chemical shifts were reported relative to the internal standard tetramethylsilane (δ 0.00 ppm) and referenced to the residual proton and carbon signals at 7.24 and 77.0 ppm, respectively, of CDCl3. Infrared spectra were obtained neat using a Perkin Elmer Spectrum BX II fitted with an ATR probe. Melting points were obtained using a Gallenkamp Digital Melting-point Apparatus 5A 6797. Elemental analysis was performed on a Thermos Scientific FLASH 2000 CHNS-O Analyzer. Mass spectrometry was performed using Waters Synapt G2 mass spectrometer with both ESI positive and Cone Voltage 15 V. XRD spectra were obtained from a Bruker APEX-II CCD Diffractometer.
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8

Synthesis and Characterization of Eu(III) Complexes

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The compounds EuCl3·6H2O (99.9%, Aldrich) and 4,4,5,5,6,6,6-heptafluoro-1-(2-thienyl)-1,3-hexanedione (hth) (Apollo Scientific), and the co-ligands dpso (97%, Aldrich), dpsoCH3 (97%, Aldrich), dpsoCl (97%, Aldrich), and tppo (>98%, Fluka) were used without further purification. The NMR spectra of the complexes, in CDCl3 (99.8%, Cambridge Isotope Labs) at 25 °C, were recorded on a Varian Mercury 400 MHz and on an Agilent DD2 500 MHz equipped with the OneNMR probe NMR spectrometers. The infrared spectra were recorded using a VERTEX 70v Bruker FT-IR spectrometer, examining powder samples in anhydrous KBr via diffuse reflection spectroscopy. Elemental analyses were carried out using a Thermo Scientific™ FLASH 2000 CHNS/O Analyzer at the Department of Chemical, Pharmaceutical and Agricultural Sciences, University of Ferrara.
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9

Oyster Mushroom Protein and Amino Acid Composition

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As the edible fungi P. ostreatus M2140 (oyster mushroom) was included in second experiment, total protein and amino acid composition of fungal biomass produced was also determined. Total amount of protein was analysed by the Dumas method [13 (link)], using a Thermo Scientific™ FLASH 2000 CHNS/O Analyzer and a conversion factor of 4.38 for total nitrogen [14 (link)]. Amino acid composition (alanine, arginine, aspartic acid, cysteine, glutamic acid, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tyrosine and valine) was determined at a certified laboratory (Eurofins Food & Agro Testing Sweden AB, Linköping, Sweden) by ion exchange chromatography according to the method by Llames and Fontaine [15 ].
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10

Elemental Analysis of Organic Compounds

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The elemental analysis CHNS/O was performed by using a Thermo Scientific™ FLASH 2000 CHNS/O Analyzer (Waltham, MA, USA). Compounds were weighed to an accuracy of ±0.000001 g in tin crucibles (2–3 mg) for analysis in CHNS mode, and in silver crucibles (1–2 mg) in oxygen mode, respectively. 2,5-(Bis(5-tert-butyl-2-benzo-oxazol-2-yl) thiophene (BBOT), sulfanilamide, L-cysteine, and L-methionine were used as standards to calibrate the device in CHNS mode. In oxygen mode, acetanilide and benzoic acid were used.
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