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116 protocols using anhydrous toluene

1

Synthesis and Characterization of Polymeric Nanoparticles

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Moisture and air-sensitive materials were manipulated under nitrogen using Schlenk techniques. The chemicals anhydrous toluene (99.8%), hexane (≥95%), stannous octoate (92.5–100.0%) (SnOct2), methanol (99.8%), dimethylformamide (≥99.8%) (DMF), chloroform (≥99.5%), tetrahydrofuran (≥99.9%) (THF), Nile Red (≥97.0%) (NR), quercetin (≥95%) (Q), and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (≥97.5%) (MTT) were acquired from Merck and used as received. The ε-caprolactone (97%) (ε-CL), acquired from Merck, was distilled in vacuo from CaH2 prior to use. Polyethylene glycol (PEG-2000 MW), acquired from Merck, was dried in vacuo over phosphorus pentoxide (P2O5) for 72 h.
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2

Silica-Based Drug Delivery System

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Tetraethyl orthosilicate (TEOS) (≥99.0%), hydrochloric acid (purum p.a. ≥32.0%), Pluronic P-123, (3-aminopropyl) triethoxysilane (APTES) (99%), sodium dodecyl sulfate (≥99.0%), anhydrous toluene (99.8%), and sulindac (≥98.0%) were supplied by Merck Life Science Sp.z.o.o., an affiliate of Merck KGaA, Darmstadt, Germany (Poznań, Poland). Chloroform (p.a. ≥98.5%), sodium chloride (pure p.a.), dipotassium phosphate (pure p.a.), and sodium hydroxide 0.1 mol/L (0.1 N) were purchased from Avantor Performance Materials Poland (Gliwice, Poland).
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3

Octadecyltrichlorosilane Surface Modification

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Precut polished silicon wafers
Si(111) were purchased from Ted Pella, Inc. (Redding, CA). Octadecyltrichlorosilane
(OTS) was obtained from Acros Organics, Thermo Fisher Scientific (New
Jersey). Silicon tetrachloride and 2,3,7,8,12,13,17,18-octaethylporphyrin
(OEP) were obtained from TCI America (Portland, OR). Size-sorted silica
spheres (500 nm) were obtained from Thermo Scientific (Fremont, CA).
Chloroform (high-performance liquid chromatography grade) was acquired
from Fisher Scientific (Lenexa, KS). Concentrated sulfuric acid (98.0%)
(J.T. Baker, Fisher Scientific) and hydrogen peroxide (30%) (British
Drug Houses, VWR) were used to prepare piranha solution. Ethanol was
purchased from Deacon Labs (Prussia, PA) and used as received. Anhydrous
toluene was purchased from Merck Millipore (Billerica, MA).
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4

Surface Modification of DHA Particles

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DHA particles were surface-modified using trimethoxy(propyl)silane
(TMPS) (Sigma-Aldrich). For this, the particles (100 mg) were kept
in a vacuum chamber at 60 °C for 24 h before being ultrasonically
dispersed in 5.0 mL of anhydrous toluene (Merck) for 30 min. The resultant
solution/dispersion was refluxed at 110 °C for 24 h while being
vigorously stirred after the addition of TMPS (4.0 mL). Following
the grafting procedure, the modified DHA (dubbed MDHA) was separated
from the dispersing solvent by centrifugation at 3900 rpm for 10 min,
thoroughly rinsed with ether to remove the physically attached silane
molecules, and dried at 60 °C for 16 h. To chemically confirm
the surface modification, we carried out FTIR analysis. Moreover,
grafting density of TMPS to particles was determined according to
the method described in the literature.31 (link) The colloidal stability of unmodified and surface modified particles
was also investigated by using sedimentation experiments. The powder
was dispersed in chloroform (Fluka) at a particle loading of 1 mg/mL
using a water bath sonicator, and the suspensions were allowed to
stand for 48 h, while the particle sedimentation behavior was recorded
at various time intervals.
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5

Cardanol-based Epoxy Resin Synthesis and Characterization

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Cardanol-based epoxy (GX-2551, Figure 1), termed EC, was
provided by Cardolite Corporation (USA). EC was characterized by a
viscosity at 25 °C of 102 cP, while the epoxy equivalent weight
was 170 g/g equiv epoxy. Pripol 1006, dimer acid hydrogenated was
provided by Croda Coatings & Polymers (acid value 196 mg KOH/g).
Benzene-1,4-diboronic acid, 1-thioglycerol (97%), ethanol (EtOH, 96%),
and anhydrous toluene (99.8%) were purchased from Merck and used as
received unless otherwise stated. The cross-linker, namely, [2,2′-(1,4-phenylene)-bis[4-mercaptan-1,3,2-dioxaborolane]
(DBEDT), was prepared by following the procedure previously reported.31 (link)
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6

Silanization of Dental Implants

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Dental implants with titanium grade 4, size 3.75 by 6 mm, external hexagon platform (P-I Brånemark, São Paulo, Brazil) were hydroxylated in a solution of H2SO4/30%H2O2 (dilution ratio 1:1) for 1 h prior to being silanized by dipping in a 10% APTES (Sigma-Aldrich Corp., St. Louis, MO, USA) in boiling anhydrous toluene (Merck SA, Rio de Janeiro, Brazil) for 4 h under reflux [8 (link),19 (link)]. It is critical to use an anhydrous solvent to control the increase the aminosilane polymerization that occurs on the surface [29 (link)]. Besides, the hydrogen bonds can be disturbed with high temperatures which then can reduce the number of infirm bonded silane molecules [30 (link)].
The titanium implants were subsequently cleaned in toluene and acetone (Merck SA/ Brazil, Rio de Janeiro, Brazil) during 10 min each in an ultrasonic bath to remove unbonded molecules. The implants were dried overnight at 110 °C in a vacuum oven to condensate the hydrogen-bonded silanols into siloxane bonds [29 (link)]. The control group only received titanium screws treated with acid (Ti) to present the same surface topography as the test group. All implants were sterilized with 25 kGy gamma radiation before use (CBE Embrarad, SP, Brazil).
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7

Amoxicillin Adsorption on Magnetic Silica Nanoparticles

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All the reagents used in this work were of analytical grade. All solutions were prepared in ultrapure water (18 MΩ at 25°C) obtained from Milli-Q Direct-0.3 (Millipore). Ethyl acetate, triethyleneglycol (TREG), acetylacetonate [Fe(acac)3, 97%], ethanol absolute, ammonia solution (23-28% v/v), anhydrous toluene, tetraethyl orthosilicate (TEOS), and methanol (HPLC grade), sodium phosphate (monobasic and dibasic) purchased from Merck. Meanwhile, 3-methylpropyltrimethoxysilane (MPS), acrylamide (AAm), amoxicillin, potassium persulfate (KPS), N, N′-methylenebisacrylamide (MBAA), graphite, and mineral oil were acquired from Sigma–Aldrich. Ultrapure water (UP, 18.2 MΩ cm at 298 K) was used for all the experiments and was obtained from a Purelab Classic water purification system. The stock solution of amoxicillin (10 μmol L−1) was prepared in 0.1 mol L−1 sodium hydroxide solution.
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8

Synthesis of Ti-Grafted S-1 Zeolite

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The SSP on S-1 surface was based on literature reports [21 (link)]. Typically, 1.0 g of pre-dried S-1 zeolite powder was added into a reactor under an anhydrous condition. Subsequently, 5 mL of titanium(IV) butoxide (97%, Aldrich, Shanghai, China) in a mixture of 10 mL of anhydrous toluene (99.8%, Aldrich, Shanghai, China) and 10 mL of anhydrous methanol (99.8%, Aldrich, Shanghai, China) was added into the reactor through a syringe. After 30 min, the precipitate was separated and washed with anhydrous methanol to remove the unreacted titanium(IV) butoxide. After that, an excess amount of water was mixed with the resulting sample to hydrolyze the monolayer of titanium oxide. Finally, the sample was washed with anhydrous methanol several times and dried at 40 °C in a vacuum oven.
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9

Synthesis of Semiconductor Nanocrystals

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Anhydrous MeOH, anhydrous toluene, anhydrous dichloromethane, pentane, trans-3,6-endomethylene-1,2,3,6-tetrahydrophthaloylchloride (97 %), 3-mercaptopropionic acid (99+ %), and hexamethyldisilathiane ((TMS)2S) were purchased from Aldrich and used without further purification. TOPO (90 % purity) was purchased from Alfa Aesar. Tri-n-butyl phosphine (TBP, 99 %), bis(tricyclohexylphosphine)benzylidene ruthenium(IV) dichloride, and dimethylcadmium (Cd(CH3)2, 97 %) were purchased from Strem Chemicals. Selenium (Se, 99.999 % purity) 100-mesh powder and diethylzinc (Et2Zn, 1.0 M solution in heptane) were purchased from Aldrich. Both Cd(CH3)2 and Et2Zn were filtered through an array of 0.2–0.1–0.05 μm pore size filters prior to use. 7-octenyl dimethyl chlorosilane was purchased from Gelest. Norbornenylethylisobutyl-POSS® (norbornoPOSS) was procured from Hybrid Plastics. Rhodamine 590, for QY measurements, was purchased from Exciton.
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10

Polymer Thin Film Preparation

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Cylinder-forming polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) BCP with a molar mass (Mn) of PS and PMMA of 46 and 21 kg/mol, respectively, was purchased along with polydispersity (PDI; Mw/Mn of 1.09) and hydroxy-terminated polystyrene (PS-OH) (Mn: 33.5 kg/mol and PDI: 1.08) from Polymer Source, Inc. (Dorval, QC, Canada). Anhydrous toluene sourced from Aldrich (St. Louis, MO, USA) was used to solvate the block copolymer and PS-OH. The resulting polymer solution was heated to 60 °C for 1 h, and then allowed to cool to room temperature.
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