A total of 25 g Citric acid monohydrate (>99.5%, Fluka, Munich, Germany) were completely dissolved in 500 mL of ultrapure water to which 6.0 g of iron powder (>99%, Sigma-Aldrich, St. Louis, MO, USA) were added. The solution was boiled and stirred under magnetic stirring (Sigma-Aldrich, St. Louis, MO, USA) until all iron powder disappeared and consequently appeared the ferrous citrate complex (Fe(II)C). Then the mixture was cooled at room temperature and the precipitate grey/pearly complex was filtered under vacuum with a paper filter and washed with water; finally, the obtained solid was freeze dried.
Iron powder
Manufactured by Merck Group
Sourced in United States
Iron powder is a fine, granular material composed of iron particles. It serves as a raw material for various industrial and manufacturing processes. The core function of iron powder is to provide a source of elemental iron that can be used in a variety of applications.
Automatically generated - may contain errors
Lab products found in correlation
Sylgard 184, by Dow (2 mentions)
Cetyltrimethylammonium bromide, by Merck Group (1 mentions)
Sodium hydroxide (naoh), by Thermo Fisher Scientific (1 mentions)
Hydrogen peroxide solution, by Merck Group (1 mentions)
Sodium sulfide, by Merck Group (1 mentions)
Multi element standard solution, by Merck Group (1 mentions)
Ultrapure water system, by Merck Group (1 mentions)
Hydrochloric acid solution, by Avantor (1 mentions)
Silver standard solution, by Chem-Lab (1 mentions)
Phosphorus oxychloride, by Merck Group (1 mentions)
2 pyridinecarboxaldehyde, by Thermo Fisher Scientific (1 mentions)
1 methylpiperazine, by Merck Group (1 mentions)
2 2 bipyridine, by Merck Group (1 mentions)
Cary 50 scan spectrophotometer, by Agilent Technologies (1 mentions)
Mcpba, by Merck Group (1 mentions)
Pyrrolidine, by Merck Group (1 mentions)
2 nitrobenzaldehyde, by Merck Group (1 mentions)
Lc ms 8030 tandem mass spectrometer, by Shimadzu (1 mentions)
Triton x 100, by Merck Group (1 mentions)
Hydrogen peroxide, by Merck Group (1 mentions)
13 protocols using iron powder
1
Synthesis of Ferrous Citrate Complex
2
Fabrication of Magnetic Microstructured PDMS MacroStamp
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Magnetic microstructured PDMS MacroStampTM (25 mm × 75 mm, Figure 2 ) were obtained by molding PDMS (Sylgard® 184, Dow Corning, Seneffe, Belgium) on a silicon-etched mold generated by UV photolithography and reactive ion etching (RIE) with a targeted etch depth of 160 µm. The mold is silanized using octodecyltrichlorosilane (OTS) to facilitate the MacroStampTM unmolding [29 (link)]. PDMS prepolymer solution (10:1 base to curing agent ratio) was then poured on the silicon mold and partially cured at 60 °C for 15 min. Then, a mix of PDMS prepolymer solution and iron powder (Sigma Aldrich (Saint Quentin Fallavier, France), hydrogen reduced, 50 µm diameter, 50/50, w/w) is prepared by successively mixing (2 min) and degassing (5 min) the resulting magnetic PDMS prepolymer solution. These steps were repeated twice and the magnetic PDMS was then molded on the first partially-cured PDMS layer. The two layers were then reticulated at 60 °C for 4 h. The resulting MacroStampTM containing 64 microstructured (50 circular patterns, 160 µM diameter at 300 µM pitch) millimetric pillars (Figure 2 ) were then removed from the mold. Each MacroStampTM was cleaned before and after its use by immersion in 96% ethanol (5 min).
3
Metal Recovery from Photovoltaic Waste
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Cetyltrimethylammonium bromide, CTAB (≥98%), sodium chloride (a.r.), hydrogen peroxide solution (30 wt%) and sodium sulfide (a.r.) were purchased from Merck KGaA (Darmstadt, Germany). Multi element standard solution (100 mg L−1 in 2–5% HNO3) and iron powder (<44 mm, 97%) were obtained from Sigma-Aldrich (Overijse, Belgium). Hydrochloric acid solution (37 wt%) was purchased from VWR (Fontenay-sous-Bois, France). Tetrafluoroboric acid solution (50% w/w), ethanol (EtOH, 99.8+%, absolute) and sodium hydroxide (pearls, a.r.) were obtained from Fisher Scientific (ThermoFisher Scientific, Loughborough, United Kingdom). Nitric acid solution (65 wt%) and silver standard solution (1000 mg L−1 in 2–5% HNO3) were purchased from Chem-Lab NV (Zedelgem, Belgium). Water was always of ultrapure quality, deionized to a resistivity of 18.2 MΩ cm with a Millipore ultrapure water system. All chemicals were used as received without any further purification. The photovoltaic panel residue was produced in the PVP recycling installation of Groupe Comet (Belgium).
4
Synthesis and Purification of Heterocyclic Compounds
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2-Aminobenzylamine,
phosphorus oxychloride, 1-methylpiperazine, and iron powder were purchased
from Sigma-Aldrich (St. Louis, MO), while isatin, 5-nitroisatin, and
2-pyridinecarboxaldehyde were purchased from Acros (Geel, Belgium).
All chemicals, as well as the synthesized precursors, were used without
further purification. 2-Amino-5-nitrobenzylamine hydrochloride was
synthesized according to a procedure published elsewhere.46 The free amine was obtained by the dissolution
of the hydrochloride in a minimal amount of water, addition of 4 equiv
of aqueous ammonia, and collection of the formed precipitate by filtration.
Ethanol was dried over molecular sieves (3 Å), and tetrahydrofuran
(THF) was dried by using a standard procedure (Na/benzophenone).47
phosphorus oxychloride, 1-methylpiperazine, and iron powder were purchased
from Sigma-Aldrich (St. Louis, MO), while isatin, 5-nitroisatin, and
2-pyridinecarboxaldehyde were purchased from Acros (Geel, Belgium).
All chemicals, as well as the synthesized precursors, were used without
further purification. 2-Amino-5-nitrobenzylamine hydrochloride was
synthesized according to a procedure published elsewhere.46 The free amine was obtained by the dissolution
of the hydrochloride in a minimal amount of water, addition of 4 equiv
of aqueous ammonia, and collection of the formed precipitate by filtration.
Ethanol was dried over molecular sieves (3 Å), and tetrahydrofuran
(THF) was dried by using a standard procedure (Na/benzophenone).47
5
Fabrication of Magnetic PDMS Stamps
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Magnetic PDMS stamps were structured with a variety of feature sizes (from 10 to 150 μm) and forms (squares, lines, spots and triangles). SU-8 resist master molds required for the fabrication of micro-structured PDMS stamps were fabricated by photolithography. After UV exposure of the resist layer (SU-8 3050, thickness of 25 μm), the master mold was developed in SU-8 developer for 9 minutes and rinsed using isopropanol. Then a PerFluorodecylTrichloroSilane (PFTS) coating was performed by spray pyrolysis deposition (SPD) to confer anti-adhesive properties to the mold surface [19 ]. Similar to the fabrication of the microfluidic devices, structured magnetic PDMS stamps were obtained in two steps. A thin layer of degassed PDMS solution (mixture of PDMS prepolymer and curing agent in 10:1 weight ratio) was poured onto the master mold and cured for 1 hour at 65°C. Magnetic PDMS solution (50/50, w/w) of iron powder (Sigma Aldrich, hydrogen reduced, 50 μm diameter) mixed with PDMS solution, was degassed and casted on top of the first layer and cured for 12 hours at 65°C. Finally, the structured PDMS stamps were removed from the mold.
6
Fabrication of Magnetic PDMS Composites
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PDMS Sylgard 184 was supplied in a two-component kit containing a pre-polymer (silicone elastomer base) and a crosslinker (184 silicone elastomer curing agent) in a ratio of 10:1 by weight (Dow Corning Corporation, Midland, MI, USA). Iron powder (size 5–9 µm; CAS no. 7439-89-6) was purchased from Sigma-Aldrich (St. Louis, MO, USA).
7
PDMS Magnetic Composite Fabrication
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PDMS Sylgard 184 is supplied as a two-part kit consisting of pre-polymer (silicone elastomer base) and cross-linker (184 silicone elastomer curing agent) components (Dow Corning Corporation, Midland, MI, USA) and iron powder (size 5–9 μm) with CAS no. 7439-89-6 was purchased from Sigma-Aldrich (St. Louis, MO, USA).
8
Bipyridine Synthesis and Characterization
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tert-Butylamine was purchased from Acros Organics. 2,2′-Bipyridine, mCPBA, 6-bromo-2,2′-Bipyridine, (S)-BINAP, iron powder, PhCF3, and KOtBu
were purchased from Sigma-Aldrich. p-Toluenesulfonic
acid anhydride was purchased from VWR. Pd(dba)2, TFA, and
MTBE were purchased from Fisher Scientific. All chemicals were used
as received without further purification. The concentration of mCPBA
was determined via titration with sodium thiosulfate before use. (S)-BINAP, iron powder, PhCF3, and KOtBu were stored under argon.
2,2′-Bipyridine mono-N-oxide, 6-amino-2,2′-Bipyridine, and N,N-bis(2,2′-bipyrid-6-yl)amine were synthesized according to
literature procedures.63 (link)−65 (link) Solvents were degassed according to standard freeze–pump–thaw
protocols.
UV–vis spectra were recorded on a Varian Cary
50 Scan spectrophotometer.
Mass spectra were measured on a Thermo Scientific MSQ Plus ESI spectrometer.
Elemental analyses were performed by Mikroanalytisches Laboratorium
Kolbe in Germany.
were purchased from Sigma-Aldrich. p-Toluenesulfonic
acid anhydride was purchased from VWR. Pd(dba)2, TFA, and
MTBE were purchased from Fisher Scientific. All chemicals were used
as received without further purification. The concentration of mCPBA
was determined via titration with sodium thiosulfate before use. (S)-BINAP, iron powder, PhCF3, and KOtBu were stored under argon.
2,2′-Bipyridine mono-N-oxide, 6-amino-2,2′-Bipyridine, and N,N-bis(2,2′-bipyrid-6-yl)amine were synthesized according to
literature procedures.63 (link)−65 (link) Solvents were degassed according to standard freeze–pump–thaw
protocols.
UV–vis spectra were recorded on a Varian Cary
50 Scan spectrophotometer.
Mass spectra were measured on a Thermo Scientific MSQ Plus ESI spectrometer.
Elemental analyses were performed by Mikroanalytisches Laboratorium
Kolbe in Germany.
9
Synthesis and Characterization of 2-Nitrobenzaldehyde Compound
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2-Nitrobenzaldehyde, iron powder, pyrrolidine etc were procured from Sigma-Aldrich (USA) and used as received. The FT-IR spectra of the compound was recorded on Agilent FT-IR spectrometer in KBr discs (4000–400 cm−1). 1H, 13C NMR spectra were recorded on a Bruker Spectrospin DPX-400 NMR spectrometer at 400.13 and 100.47 respectively using TMS as an internal standard. Mass analysis was carried out using Nexera UHPLC at 130 MPa with SIL-30 AC Nexera autosampler coupled to an LC-MS 8030 tandem mass spectrometer manufactured by Shimadzu Corporation, Kyoto, Japan. The software SADABS was used for absorption correction and SHELXTL for space group, structure determination and refinements. All non-hydrogen atoms were refined anisotropically. All the computations have been carried out at DFT/B3LYP/6-31G (d,p) level of theory using GAUSSIAN 09 software.
10
Fabrication of Anisotropic Janus Particles
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Corn starch granules (MFG 2006779) were purchased from Argo (Oakbrook, IL), and used to prepare starch/water mediums by mixing with DI-water at various concentrations of 5–25 wt% and gelatinizing the granules at 95 °C for 1 h. Amylase enzyme (SKU: 5BHBZZ7100B) was purchased from BSG (Shakopee, MN). Field’s Metal blocks (SKU: LMP144) were purchased from RotoMetals (San Leandro, CA) and used as-is. Two-part silicone resin EcoFlex 00-30 and one-part RTV silicone resin Semicosil 964 were purchased from Smooth-On (Macungie, PA) and Wacker (Adrian, MI), respectively. Iron powder (<10 μm) (SKU: 267953) and silver-coated ferrite particles (~25 μm) (SM25P20) were purchased from Sigma Aldrich (St. Louis, MO) and Potters Industries, LLC respectively, and used as fillers of anisotropic particles. Hydrogen peroxide and Triton X-100 (SKU: X100) were purchased from Sigma Aldrich (St. Louis, MO) and used as reaction medium and surfactant for propelling Janus particles.
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