Copper sulfates (CuSO4, 99%), silver nitrate (AgNO3, 99%), ammonium sulfate(99%, ethylenediamine(NH2CH2CH2NH2, 99.5%), potassium hydroxide (KOH, 90%) potassium bicarbonate(KHCO3, 99.7%), sulfuric acid(H2SO4, 99.99%), Iridium (III) chloride hydrate (IrCl3·xH2O, 99.9%), 5-Amino-1,3,4-thiadiazole-2-thiol(C2H3N3S2,95%), 3-amino-1,2,4-triazole-5-thiol(C2H4N4S,99%), cysteamine(C2H7NS,99%) and 1-Propanethiol (C3H8S, 99%) were purchased from Sigma Aldrich. Nafion 117 and anion exchange membrane (Fumapem FAA-3-50), gas diffusion layer (Freudenberg, H23C6), and titanium mesh were obtained from Fuel Cell Store. All chemicals were used as received. All aqueous solutions were prepared using deionized water with a resistivity of 18.2 MΩ cm−1.
Iridium 3 chloride hydrate
Manufactured by Merck Group
Sourced in Germany
Iridium (III) chloride hydrate is an inorganic compound with the chemical formula IrCl3·xH2O. It is a dark green, crystalline solid that is used as a precursor in the synthesis of other iridium-containing compounds. The exact number of water molecules (x) in the hydrate can vary.
Automatically generated - may contain errors
Lab products found in correlation
Potassium hydroxide, by Merck Group (2 mentions)
Methanol, by Merck Group (2 mentions)
Potassium bicarbonate, by Merck Group (1 mentions)
Ammonium sulfate, by Merck Group (1 mentions)
1 propanethiol, by Merck Group (1 mentions)
Nafion 117, by Fuel Cell Store (1 mentions)
Sulfuric acid, by Merck Group (1 mentions)
Silver nitrate, by Merck Group (1 mentions)
Ethylenediamine, by Merck Group (1 mentions)
Cysteamine, by Merck Group (1 mentions)
Lithium hydroxide, by Merck Group (1 mentions)
Polyvinylpyrrolidone, by Merck Group (1 mentions)
Sodium hydroxide (naoh), by Merck Group (1 mentions)
Rhodium 3 chloride hydrate, by Merck Group (1 mentions)
1 2 3 4 5 pentamethylcyclopentadiene, by Merck Group (1 mentions)
Sdt q600, by TA Instruments (1 mentions)
Iridium 4 oxide, by Merck Group (1 mentions)
Sodium phosphate dibasic, by Merck Group (1 mentions)
L cysteine, by Merck Group (1 mentions)
Isopropanol, by Merck Group (1 mentions)
6 protocols using iridium 3 chloride hydrate
1
Electrochemical Synthesis of Metal-Organic Compounds
2
Iridium Compound Synthesis and Purification
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Iridium(III) chloride hydrate (IrCl3·nH2O, reagent grade), sodium nitrate (NaNO3, ReagentPlus, ≥99.0%), lithium hydroxide (LiOH, reagent grade, 98%), and iridium(IV) oxide (IrO2-CR, 99.9%) were purchased from Sigma-Aldrich. DI water was supplied by the Milli-Q Benchtop laboratory water purification systems (Sigma-Aldrich).
3
Synthesis of Iridium Nanoparticles with PVP
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Iridium (III) chloride hydrate (IrCl3·3H2O; Mw = 298.58 gmol−1, anhydrous basis, 99.9% trace metal basis) and polyvinylpyrrolidone (PVP; average Mw = 1,300,000 gmol−1) were purchased from Sigma-Aldrich Chemie GmbH, Tauflirchen, Germany. Sodium hydroxide (NaOH; Mw = 40.00 gmol−1) and methanol (MeOH; analytical grade) were purchased from Sigma-Aldrich Chemie GmbH, Tauflirchen, Germany and Sharlau Chemicals (Barcelona, Spain), respectively. All chemicals were used as received from the manufacturer without further purification. The Millex®-HP 13 mm filter unit (PES 0.45 μm membrane) that was employed in solution filtration was purchased from Sigma-Aldrich Chemie GmbH, Tauflirchen, Germany.
4
Synthesis and Characterization of Organometallic Complexes
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Rhodium(III) chloride hydrate
(RhCl3·xH2O), iridium(III)
chloride hydrate (IrCl3·xH2O), and 1,2,3,4,5-pentamethylcyclopentadiene (Cp*) were purchased
from Sigma-Aldrich and used without further purification. The dimers
(Cp*IrIIICl2)2 and (Cp*RhIIICl2)2 were synthesized according to the published
procedures,16 and their purity was confirmed
by Fourier transform infrared (FTIR) and 1H and 13C NMR spectroscopy. The polyanion precursors Na12[Bi2W22O74(OH)2]·44H2O and K12[Sb2W22O74(OH)2]·27H2O were prepared according to
the published procedures.17 (link) FTIR spectra
were recorded on a Nicolet-Avatar 370 FTIR spectrophotometer using
KBr pellets. Elemental analyses were done at ExxonMobil Chemicals
Europe Inc., European Technology Center. Thermogravimetric analyses
(TGAs) were performed on a SDT Q600 from TA Instruments under the
flow of N2 gas. The NMR spectra were recorded on a JEOL
ECS 400 MHz spectrometer, using 5 mm tubes for 13C and
10 mm tubes for 183W NMR, with resonance frequencies of
100.71 and 16.69 MHz for 13C and 183W, respectively.
The chemical shifts are reported with respect to the references Si(CH3)4 for 13C and 1 M aqueous Na2WO4 for 183W.
(RhCl3·xH2O), iridium(III)
chloride hydrate (IrCl3·xH2O), and 1,2,3,4,5-pentamethylcyclopentadiene (Cp*) were purchased
from Sigma-Aldrich and used without further purification. The dimers
(Cp*IrIIICl2)2 and (Cp*RhIIICl2)2 were synthesized according to the published
procedures,16 and their purity was confirmed
by Fourier transform infrared (FTIR) and 1H and 13C NMR spectroscopy. The polyanion precursors Na12[Bi2W22O74(OH)2]·44H2O and K12[Sb2W22O74(OH)2]·27H2O were prepared according to
the published procedures.17 (link) FTIR spectra
were recorded on a Nicolet-Avatar 370 FTIR spectrophotometer using
KBr pellets. Elemental analyses were done at ExxonMobil Chemicals
Europe Inc., European Technology Center. Thermogravimetric analyses
(TGAs) were performed on a SDT Q600 from TA Instruments under the
flow of N2 gas. The NMR spectra were recorded on a JEOL
ECS 400 MHz spectrometer, using 5 mm tubes for 13C and
10 mm tubes for 183W NMR, with resonance frequencies of
100.71 and 16.69 MHz for 13C and 183W, respectively.
The chemical shifts are reported with respect to the references Si(CH3)4 for 13C and 1 M aqueous Na2WO4 for 183W.
5
Melamine-Cysteine Electrocatalyst Synthesis
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Melamine (99%, CAS no. 108-78-1), l -cysteine (≥98%, CAS no. 52-90-4), iridium(III) chloride hydrate (99.9% trace metals basis, CAS no. 14996-61-3), sodium phosphate dibasic (≥99.0%, CAS no. 7558-79-4), sodium phosphate monobasic (≥99.0%, CAS no. 7558-80-7), perchloric acid (70%, CAS no. 7601-90-3), potassium hydroxide (pellets, 99.99% trace metals basis, CAS no. 1310-58-3), methanol (≥99.9%, CAS no. 67-56-1), platinum on Vulcan XC72 powder (20 wt.% loading), iridium on Vulcan XC72 powder (20 wt.% loading), iridium(IV) oxide (99.9% trace metals basis, CAS no. 12030-49-8), isopropanol (99.5%, CAS No. 67-63-0) and nafion 117 solution (~5% in a mixture of lower aliphatic alcohols and water) were purchased from Sigma-Aldrich and used without further purification.
6
Synthesis and Characterization of Iridium(III) Complexes
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Iridium (III) chloride hydrate, 2-phenyl pyridine and 2-ethoxyethanol (Sigma-Aldrich), 1phenyl-3-methyl-2-pyrazoline-5-one (Merck) were used as received. The organic solvents and other reagents were used after purification using the standard protocols. 43, 44 All the reactions were carried out in nitrogen atmosphere with the Schlenk line. The nuclear magnetic resonance (NMR) spectra were collected using a Bruker 400 MHz Spectrometer (Fig. S7-S9). Deuterated dimethyl sulfoxide (DMSO-d 6 ) was used as solvent for the measurement and calibration for the residual peak of the deuterated solvent (δ 2.52 for 1 H NMR). The high resolution mass spectra (HR-MS) of the complexes were taken with the Shimadzu LCMS-2010 Spectrometer (Fig. S10).
The FT-IR Spectra were taken with the Infrared Spectrophotometer MB-3000 (Fig. S11).
The FT-IR Spectra were taken with the Infrared Spectrophotometer MB-3000 (Fig. S11).
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