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1 227 protocols using toluene

1

Synthesis of CsPbBr3 Perovskite Nanocrystals

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The 8.6 nm NCs
were synthesized following the method reported in ref (51 (link)). In a 25 mL three-neck
flask, PbBr2 (55 mg, ABCR, 98%) was degassed three times,
suspended in 5 mL of ODE, and degassed again three times at room temperature.
The suspension was fast heated up to 180 °C, when the temperature
reached 120 °C; 0.5 mL of OA and oleylamine (0.5 mL, OLA, Strem,
97%, distilled) was injected. At 180 °C, preheated to about 100
°C cesium oleate solution in ODE (0.6 mL) was injected. The reaction
mixture was cooled immediately to room temperature with an ice bath.
The crude solution was centrifuged at 20 130 relative centrifugal
force (rcf) for 5 min. The supernatant was discarded, and the precipitate
was dispersed in hexane (0.3 mL, Sigma-Aldrich, anhydrous, 95%). The
solution was centrifuged again at 13 750 rcf for 3 min, and
the precipitate was discarded. Then, OLA/OA ligands were exchanged
by didodecyldimethylammonium bromide (DDAB) treatment. Then, 0.3 mL
of hexane, toluene (0.6 mL, Sigma-Aldrich, anhydrous, 99.8%), and
DDAB (0.14 mL, 0.05 M in toluene, Sigma-Aldrich, 98%) were added to
the supernatant and stirred for 1 h, followed by destabilization with
ethyl acetate (1.8 mL, Sigma-Aldrich, 99.9%), centrifuging at 20 130
rcf for 3 min and redispersion in 0.6 mL of toluene. Synthesis of
5.3 nm CsPbBr3 NCs was adopted from ref (50 (link)) followed by DDAB treatment.
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2

Covalent Bioactive Compound Immobilization

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For covalent binding of bioactive compounds, Ti and TiNbHf samples were coated with amino groups by silanization. The surface of the material was activated by a 5 min oxygen plasma treatment (TePla 100-E). Activated samples were immersed into a 0.08 M solution of aminopropyl-triethoxysilane (APTES, Sigma-Aldrich) in toluene (Sigma-Aldrich) at 70 ºC for 1 h under agitation. After silanization, samples were sonicated in toluene for 5 minutes and washed with toluene (3x), acetone (1x), isopropanol (3x), distilled water (3x), ethanol (3x) and acetone (3x) (all chemicals from Sigma-Aldrich). Subsequently, aminosilanized samples were immersed into a 7.5 mM solution of N-succinimidyl-3-maleimidopropionate in DMF for 1h under agitation at room temperature. The cross-linked samples were rinsed in DMF (3x), acetone (1x), distilled water (10x), ethanol (3x), acetone (3x) and dried with nitrogen.
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3

Quantitative Tracer Analysis in HPLC

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Acetophenone and toluene were used as tracer analytes, both purchased from Sigma-Aldrich (Steinheim, Germany). Both test components were dissolved in a premixed mixture of either 50/50 or 30/70 (v/v) ACN/H2O in concentrations of 0.0125 mg/ml (12.5 ppm), 0.025 mg/ml (25 ppm), 0.05 mg/ml (50 ppm) or 0.075 mg/ml (75 ppm). The same premixed mixture (without any tracer) was also directly fed to the peripheral part of the column.
Acetonitrile (supra-gradient grade) was purchased from Biosolve (Valkenswaard, The Netherlands) and HPLC grade water (H2O) was prepared in the laboratory using a Milli-Q gradient water purification system (Millipore, Bedford, MA, USA).
The linear behavior of signal intensities versus injected tracer concentration on both VWD-and DADdetectors was validated up to continuous injections of 75 ppm of both Acetophenone and toluene tracers.
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4

Synthesis of Pyridine-Chromium Complexes

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The reagents were purchased from Sigma-Aldrich: 2-pyridinecarboxylic acid (2-pic), 99% purity), chromium(III) nitrate hexahydrate (99% purity), lithium carbonate (99% purity), toluene (99% purity), modified methylaluminoxane (MMAO-12, 7 wt% aluminum in toluene), 2-chloro-2-propen-1-ol (90%), and from Stanlab - nitric acid (65%).
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5

Mechanochemical Synthesis of CsPbBr3 Nanocrystals

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Bulk CsPbBr3 (0.02 g,
0.035 mmol, prepared as described
above) was loaded into a zirconia bowl with 25 zirconia balls (4 mm
and 5 mm) and with OAmBr (0.01 g, 0.03 mmol, prepared as described
above), and 0.4 mL of mesitylene (98%, Sigma-Aldrich). Another tested
ligand system was a mixture of OA (0.05 mL, Sigma-Aldrich, 90%) and
OLA (0.05 mL, Strem, 95%). Other tested solvents were octadecene (Sigma-Aldrich,
90%), Dowtherm A (diphyl, eutectic mixture of 26% diphenyl + 73.5%
dipheniloxide), toluene (Sigma-Aldrich, 99.5%), hexane (>95%, Sigma-Aldrich),
and chloroform (HPLC grade, Fisher Chemicals). The bowl was mounted
on a planetary ball mill (Fritsch, Pulverisette 7, classic line),
and the speed was set to 500 rpm. The time was varied from 30 min
to 24 h. After the milling, a bright green suspension was obtained,
which was diluted with toluene (2 mL) and used as-obtained or precipitated
one time with acetonitrile (0.5 mL, 99.8%, Aldrich). The precipitate
was redispersed in 2 mL of toluene.
Alternatively, CsBr (0.011
g, 0.05 mmol, Aldrich, 99.9%) and PbBr2 (0.018 g, 0.05
mmol) were loaded into a zirconia bowl with 25 zirconia balls (4 mm
and 5 mm) and with 1.6 mL of mesitylene and 0.01 g of OAmBr (0.03
mmol). The subsequent milling lasted 2 h at 500 rpm. The bright green
crude solution was diluted with 2 mL of toluene.
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6

Synthesis of Stereoregular Polydienes

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Manipulations of air- and/or moisture-sensitive materials were carried out under an inert atmosphere using a dual vacuum/nitrogen line and standard Schlenk-line techniques. Toluene (≥99.7% pure, Aldrich, Milano, Italy) and heptane (≥99% pure, Aldrich) were refluxed over Na for about 8 h and then distilled and stored over molecular sieves under nitrogen. o-Xylene (Aldrich, anhydrous grade), p-Toluenesulfonylhydrazide (TSH, Aldrich), deuterated solvent for NMR measurements (C2D2Cl4) (Cambridge Isotope Laboratories, Inc., Tewksbury, MA, USA), diethylaluminum chloride (AlEt2Cl) (97% pure Fluka-Aldrich, Milano, Italy), triisobutylaluminum (Al(iBu)3) (98% pure, Aldrich), methylaluminoxane (MAO) (10 wt% solution in Toluene, Aldrich) and Nd(OCOC7H15)3 (Strem Chemicals, Bischheim, France) were used as received. (E)-1,3-pentadiene (96% pure, Fluka) and isoprene (98%, Aldrich,) were refluxed over calcium hydride for about 4 h, then distilled trap-to-trap, and stored under nitrogen. Isotactic cis-1,4-poly(E-1,3-pentadiene) and cis-1,4 poly(isoprene) were synthesized with the catalyst AlEt2Cl/(NdOCOC7H15)/AliBu3 as described in reference 21 and 32/33, respectively; syndiotactic cis-1,4 poly(E-1,3-pentadiene) was synthesized with the catalyst CoCl2(PtBu2Me)2/MAO as described in [34 (link)].
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7

Synthesis of Colloidal Quantum Dots

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Cadmium oxide (CdO, 99.98%), selenium (Se, 99.999%, 200 mesh) and methanol (99.9%, anhydrous) were purchased from Alfa Aesar. Sulfur (S, 99.98%), tetrakis(acetonitrile)copper(I) hexafluorophosphate ([Cu(CH 3 CN) 4 ]PF 6 , 97%), toluene (99.8%, anhydrous), zinc chloride (ZnCl 2 , 99.999%), cadmium acetate dihydrate (Cd(OAc) 2 •2H 2 O, 98%), mercaptoacetic acid (MAA, 99%), 3-mercaptopropionic acid (MPA, 99%), 11-mercaptoundecanoic acid (MUA, 95%), methanol (99.8%), n-hexane (99%), potassium hydroxide (KOH, 85%), chloroform (99.8%), hydrochloric acid (HCl, 37%), oleic acid (90%), cadmium nitrate tetrahydrate (99%), sodium myristate (99%) and toluene (99.7%) were purchased from Sigma-Aldrich. Tri-n-octylphosphine (TOP, 97%) and Tri-n-octylphosphine oxide (TOPO, 99%) were purchased from ABCR. Octadecylphosphonic acid (ODPA, >99%) and hexylphosphonic acid (HPA, >99%) were purchased from PCI Synthesis. 1-Octadecene (ODE, 90%), oleylamine (OLAM, 80-90%) and 2-(dimethylamino)ethanethiol hydrochloride (DMAET•HCl, 95%) were purchased from Acros Organics. Ethanol (99.8%) was purchased from Roth. Rhodamine 6G was purchased from Lambda Physik.
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8

Preparation of PS-r-PMMA Blend Solutions

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A homogeneous 1% (by wt) solution of random copolymer PS-r-PMMA (Sigma Aldrich, average Mw 100 000–150 000, styrene 40 mol%) was prepared by dissolving the polymer in toluene. Likewise, the 1% solutions of PS (Sigma Aldrich, Mw = 192 000) and PMMA (Sigma Aldrich, Mw = 120 000) were prepared in toluene (Sigma Aldrich). In order to prepare a homogeneous blend of PS–PMMA, separate solutions of PS (1 wt%) and PMMA (1 wt%) in toluene were prepared and mixed thoroughly with PS : PMMA: 40 : 60 volume ratio.
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9

Synthesis of Colloidal Nanocrystals

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Styrene (≥ 99.0%), divinylbenzene (DVB, 80%), azobisisobutyronitrile (AIBN, 98%), tin(II) 2-ethylhexanoate (92.5–100%), ε-caprolactone (97%), poly(ethylene glycol) (PEG, MW 2,500), trioctylphosphine oxide (TOPO, 99%), 1-octadecene (ODE, 90%), toluene (≥ 99.7%), methanol (≥ 99.8%), isopropanol (≥ 99.8%), oleylamine (OLA, 70–80%), 1-octanethiol (98.5%) and acetone (≥ 99.5%) were obtained from Sigma Aldrich Co. Polyvinylpyrrolidone (PVP, MW 40,000), cadmium oxide (CdO, 99.998%), selenium powder (200 mesh, 99.999%) and oleic acid (OA, 90%) were purchased from Alfa Aesar. toluene, ethanol and n-heptane (all spectr. grade) as well as n-hexane (≥ 99%) were obtained from Merck KGaA. ethanol (abs., 99.9%) and dichloromethane (HPLC grade) were obtained from Chemsolute. Benzyldimethyloctadecylammonium chloride (OBDAC, 98.9%) was purchased from HPC Standards GmbH, Nile red (NR) from Fluka Analytical, n-octadecylphosphonic acid (ODPA, > 99%) from PCI Synthesis and tri-n-octylphosphine (TOP, 99.7%) as well as deuterated chloroform (99.8 atom%) from ABCR. All solvents used for the optical measurements were of spectroscopic grade and all chemicals were employed as received without further purification.
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10

Fabrication of Toluene-Based Organic Thin Films

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Microscope cover glasses (Marienfeld, borosilicate glass, 18 × 18 mm2) were immersed in an Aqua Regia (HCl/HNO3 3:1 in volume ratio) for 30 mins for cleaning, followed by 5-min sonication in DI water, and finally dried with N2.
Toluene solutions were purchased from two manufacturers; Sigma-Aldrich (ACS reagent, ≥99.5%) and Daejung (>99.5%). Few drops of Toluene on the cover glasses were evaporated on a hot plate at 86 °C. Para-terphenyl (Sigma-Aldrich, >99.5%) was dissolved in Toluene (Sigma-Aldrich) with a concentration of 1.2 mg/ml and then spin coated on cleaned cover glasses at 2000 rpm for 5 s.
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