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9 protocols using propylene oxide

1

Synthesis and Characterization of Metal-Dye Complexes

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The chemicals in this study
were used as received and without any further purification. Aluminum
nitrate nonahydrate Al(NO3)3·9H2O was provided by BDH. Nickel nitrate hexahydrate Ni(NO3)2·6H2O and ethanol absolute were purchased
from Sigma-Aldrich. Propylene oxide (noted PO; CH3CHCH2O), orange II (noted OII, C16H11N2NaO4S), methyl orange (noted MO, C14H14N3NaO3S), Congo Red (noted CR,
C32H22N6Na2O6S2), methylene blue (noted MB, C16H18ClN3xH2O), rhodamine
B (noted rhB, C28H31ClN2O3), and rhodamine 6G (noted rh6G, C28H31N2O3Cl) were provided by Acros. Acetone was purchased
from Scharlau Chemie S.A. Double distilled water was obtained from
our laboratory.
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2

Synthesis of γ-Al2O3 Xerogel from AlCl3

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To ensure all samples originated from the exact same batch, a large batch of γ-Al2O3 was prepared, similar to the previously reported method [13 (link)]. To this end, 156 g of AlCl3·6H2O (Fluka) were dissolved in 137 mL of distilled water and 200 mL ethanol (Bioenergie Icking GmbH). After complete dissolution, 10.2 g of oxalic acid (dihydrate, Merck) were added and dissolved. Without delay, the reaction mixture was placed in a flask surrounded by an ice bath and cooled down to 4 °C, then 140 mL of propylene oxide (Acros Organics) were added, all at once, under vigorous stirring. The ice bath was removed after 6.5 min, and the reaction mixture was stirred at room temperature for another 6.5 min. The obtained sol was poured into a beaker, sealed and placed in an oven at 40 °C for gelation. To ensure a uniform heat transfer, the beaker resided in a water bath. After 24 h, solvent exchange to pure ethanol was carried out under static conditions for 3 days. The opaque white gel was then transferred to a drying cabinet pre-heated at 70 °C, with the lid removed. Drying was terminated after 7 days. Ultimately, the obtained xerogel was pre-calcined at 650 °C for 6 h, with a heating rate of 3 K min−1. Characterization of the starting material was carried out as described in Section 3.1.
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3

Electron Microscopy of Arterial Samples

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After fixation of arterial samples in 2.5% glutaraldehyde (TED PELLA, CA, USA) in PBS (pH 7.2), specimens were post-fixed in 1% osmium tetroxide (Heraeus, Hanau, Germany), dehydrated in graded ethanol and propylene oxide (Acros Organics, USA), and then embedded in Epoxy resin (mix with Nadic Methyl Anhydride (NMA) and Dodecenyl Succinic Anhydride (DDSA) and DMP-30, all reagents from Polysciences (PA, USA). Serial ultrathin sections were cut using an LKB-III ultratome (LEICA, Wetzlar, Germany). Ultrathin sections were stained with uranyl acetate (TED PELLA, CA, USA) and lead citrate (TED PELLA, CA, USA) and were examined with the aid of a Hitachi H7600 electron microscope (Hitachi, Japan) at an accelerating voltage of 100 kV.
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4

Hafnium Tetrachloride Synthesis Protocols

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Hafnium(IV) tetrachloride (98%) was used as the Hafnium source. Acetone, acetonitrile, hexanes, methanol, and pentane were all HPLC Plus (>99.9%). Hydrochloric acid (35.0–37.0%), sulfuric acid (95.0–98.0%), Sodium chloride (>99%) and deuterated water (D2O) were used as purchased from Sigma-Aldrich. N-Methyl formamide (99%) and sodium hydroxide pellets (98%) were purchased from Alfa Aesar. Poly(ethylene oxide) (MW 100 000) was purchased from Polysciences Inc. Propylene oxide (99.5%) and Trifluoroacetic acid (99.5%) were purchased from Acros Organics. Perfluorooctanoic acid (>98%) was purchased from TCI America. Ultrapure water (≥18.2 MΩ∙cm) used for synthesis and adsorption kinetics experiments was obtained from a Thermo Scientific Barnstead E-Pure Ultrapure water purification system.
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5

Sodium-containing Macroporous Alumina Synthesis

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The macroporous sodium-containing alumina bulk material was synthesized via an epoxide-mediated sol-gel route as described by Carstens and Enke [26 (link)]. The synthesis procedure was slightly modified regarding the replacement of ethanol by methanol to enable the integration of sodium-ions in the system.
7.80 g AlCl3·6H2O (Alfa Aesar, 99%) and 0.00, 0.01 or 0.10 g polyethylene oxide with a molecular weight (M.W.) of 900,000 (Acros Organics) were dissolved in a mixture of 5.77 g deionized water and 7.90 g methanol (VWR Chemicals, 100.0%) at room temperature. The solution was placed in an ice bath and cooled down to 5 °C within 1 h. 1.414 g of 4 M NaOH (VWR chemicals) were added under constant stirring (500 rpm). Immediately, 7.00 mL propylene oxide (Acros Organics, 99.5%) was added. The ice bath was removed after three minutes. The reaction solution was stirred for another seven minutes at room temperature. The reaction vessel was then placed in a water bath at 40 °C to induce gelation, followed by aging for 24 h at 40 °C. After an ethanol exchange for five days and drying at 50 °C for seven days, the obtained xerogels were calcined at 1200 °C for 1 h with a heating rate of 10 K∙min−1 (IH 60/14, Nabertherm, Germany). For disc preparation (diameter: 20 mm, high: 3 mm), the calcinated xerogels were ground to a particle size <350 µm and pressed into a disc form.
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6

Ultrastructural Analysis of Skin Fibroblasts

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Primary human skin fibroblasts were fixed in PBS containing 4% paraformaldehyde and 2.5% glutaraldehyde for 24 h and rinsed in PBS. The samples were then subjected to 70-nm sectioning after gradual dehydration in ethanol solutions and propylene oxide (Acros Organics, Morris Plains, NJ, USA), and stained with epoxy resins using standard procedures. Images were acquired with a Hitachi electron microscope (Hitachi, Tokyo, Japan) equipped with a ES500W digital camera (GATAN, Pleasanton, CA, USA).
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7

Synthesis of Rare-Earth Doped Silica Nanoparticles

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The chemicals were used as received and without further purification. Tetraethoxysilane, titanium(iv) isopropoxide, dysprosium(iii) chloride hexahydrate, holmium(iii) chloride hexahydrate, neodymium(iii) chloride hexahydrate, erbium(iii) chloride hexahydrate, and samarium(iii) chloride hexahydrate were purchased from Sigma-Aldrich. Cobalt(ii) chloride hexahydrate was provided by AnalaR. Iron(iii) chloride hexahydrate was from Fluka. Curcumin (98% purity) and propylene oxide were purchased from Acros Organics. Methanol, hydrochloric acid (37%), and ammonium hydroxide were from Riedel-de-Haen, Panreac and Fischer Scientific, respectively. Double deionized water was prepared in our laboratory.
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8

Synthesis of Aluminum-based Compounds

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All reagents were used as received, without further purification or treatment. AlCl3·6H2O (99% purity) was purchased from Alfa Aesar. Propylene oxide was delivered by Acros Organics, citric acid (food quality) by purux, and all employed dicarboxylic acids by Merck. Solvents (ethanol and distilled water) were taken from domestic lines.
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9

Ultrastructural Analysis of Leptocephalus Larvae

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Before embedding in epoxy resin (EPON, Sigma-Aldrich, United States), the leptocephalus larvae were cut into three evenly sized parts, which were post-fixed in a mixture consisting of 3% potassium ferrocyanide (KFC, Sigma-Aldrich, United States) and 4% osmium (Carl Roth, Germany) for 1 h, and then bulkstained for 1.5 h with 1.5% uranyl acetate (VWR Chemicals, United States) in distilled water. The larvae were dehydrated in ethanol and propylene oxide (Acros Organics, Belgium), before embedding in EPON. , SL 11.17) showing the difference between the two areas of the digestive tract, the esophagus and the intestine, and the transition zone between these.
Transverse sections (1µm) were produced on a Leica Reichert Ultracut microtome (Leica Microsystems, Germany). Sections were produced of the mouth/pharynx and of the esophagus,
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