Reagents were used from manufacturer without additional purification: phosphoric acid, fumed silica, titanium isoproproxide and KOH Pellets were purchased from Sigma Aldrich. Sodium hydroxide (98%), nitric acids (70% optima) and trace metal grade hydrochloric acid were purchased from Fisher. La, Ce, Lu ICP standards were purchased form Fluka in 1000 mg/L concentrations. ICP single elemental certified standards of: Th, Ag, Ba, Rh, Ce, and La were purchased from SPEX Certiprep. All solutions were prepared using Milli-Q water and all experiments were conducted at room temperature. All the chemicals used were of analytical reagent grade. Buffers were prepared from previously prepared 0.5 N Sodium Acetate buffer and adjusted with 8 N HCl or 10 M NaOH. Initial and equilibrium pH readings were obtained using a Denver Instruments UB-10 pH/mV meter calibrated at pH 2.0, 4.0 and 7.0. Since Ba chemically behaves similarly to Ra and La is chemically similar to 225Ac for some studies Ba and La can be used as surrogates. 225Ac radiotracer was supplied by Oak Ridge National Laboratory as a dried sample, and the sample was dissolved in 0.1 M HCl solution prior to use. 223Ra and 227Th were present in some 225Ac samples as a result of the decay of 227Ac.
Koh pellets
Manufactured by Merck Group
Sourced in Germany
KOH pellets are a laboratory chemical compound commonly used as a desiccant and pH adjuster. They are solid, white, and hygroscopic in nature. KOH pellets have a variety of applications in scientific research and analysis.
Automatically generated - may contain errors
Lab products found in correlation
Sodium hydroxide (naoh), by Thermo Fisher Scientific (1 mentions)
Fumed silica, by Merck Group (1 mentions)
Trace metal grade hydrochloric acid, by Thermo Fisher Scientific (1 mentions)
Phosphoric acid, by Merck Group (1 mentions)
Smz25, by Nikon (1 mentions)
Gf c glass microfibre filters, by Cytiva (1 mentions)
Glass coverslip, by Corning (1 mentions)
Carbon black, by Merck Group (1 mentions)
Sodium sulfide hydrate, by Merck Group (1 mentions)
Niobium nitrate, by Merck Group (1 mentions)
Hydrochloric acid (hcl), by Merck Group (1 mentions)
Silver nitrate, by Merck Group (1 mentions)
Sp 150 potentiostat, by Bio-Logic (1 mentions)
Pyrrolidine, by Thermo Fisher Scientific (1 mentions)
Piperidine, by Thermo Fisher Scientific (1 mentions)
4 4 azobis 4 cyanovaleric acid acva, by Merck Group (1 mentions)
Acryloyl chloride, by Merck Group (1 mentions)
Anhydrous dichloromethane dcm, by Thermo Fisher Scientific (1 mentions)
N n dimethylacrylamide dma, by Merck Group (1 mentions)
Brockmann 1, by Merck Group (1 mentions)
13 protocols using koh pellets
1
Radionuclide Separation and Purification
2
Microplastics Extraction and Characterization
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Prior to carrying out the microplastics extraction and characterization, the digestive system of each specimen was rinsed with pre-filtered (0.22 μm) deionized water and centrifuged to eliminate alcohol used to store them. Subsequently each pellet was incubated with 10% of KOH (w/v) solution prepared using KOH pellets (Sigma-Aldrich, Saint-Quentin-Fallavier, France) and double-distilled water. Then they were placed on an agitation plate (IKA RT15, Staufen, Germany) set at 300 rpm and 60 ± 1 °C for 24 h. After digestion, all samples were filtered on 90 mm diameter GF/C glass microfibre filters (Whatman, Velizy-Villacoublay, France) using a vacuum system. Filters were then placed in closed Petri dishes until subsequent analysis. For the first characterisation, filters were observed under a stereomicroscope (Nikon SMZ25, Tokyo, Japan), allowing the identification of plastic particles. Items with characteristics similar to plastic polymers were characterized by size (< 100 µm; 100–500 µm; ˃500 µm) and colour. Filtered fragments and fibres were then rinsed in distilled water and mounted on double-sided adhesive carbon tabs on aluminium SEM stubs for successive SEM/EDX analyses.
3
Cleaning Glass Coverslips for Research
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Glass coverslips purchased from Corning (18 × 18 mm, No. 1.5, catalog #: 2850-18) were used for the study. They were cleaned using KOH pellets (Sigma Aldrich, catalog #: P5958) dissolved in absolute ethanol (Fisher Scientific, catalog #: BP2818) as follows. Saturated KOH solution was prepared by mixing 90 g of KOH in 350 ml of absolute ethanol. This mixture was stirred using a magnetic stirrer in a 1 L beaker until the solution turned dark orange in color (~4 hrs). Home built Teflon baskets were used to hold the glass cover slips along their periphery for treatment in the saturated KOH solution for 3 min while immersed in a sonicator (Branson 5510). Coverslips were then rinsed with deionized water (18.2 MΩ*cm) using a squirt bottle and transferred into a beaker to be sonicated in distilled deionized water for an additional 3 min twice, with rinsing in-between. Coverslips were then rinsed with 95% ethanol, dried using ultra high purity nitrogen gas, and stored in a desiccator. Over several days surfaces can lose their hydrophilicity40 . Thus, immediately before use, surfaces were plasma cleaned to render them hydrophilic as described below.
4
Synthesis of NbOx-AC Hybrid Electrode
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The subsequent materials were bought from Sigma Aldrich: carbon black (CB), niobium nitrate (Nb(NO3)5), KOH pellets, silver nitrate (AgNO3), hydrochloric acid (HCl), activated carbon, sodium sulfide hydrate (Na2S·9H2O) and niobium nitrate (Nb(NO3)5). The chemicals were bought in their purest form and weren't further purified before use. Deionized water (DIW) was used to make solutions, wash samples, and prepare electrolytes. The reference electrodes (Hg/HgO), nickel foam, and platinum wire were imported from Japan.
5
Electrochemical Analysis of NiFe Films
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The OER tests were operated in a three-electrode cell with a NiFe film as the working electrode (WE), a platinum foil counter electrode, and a Hg/HgO (1.0 M KOH) reference electrode. The schematic diagram of working electrode preparation shows in Supplementary Fig. 1 . Au was deposited on the NiFe films where contact with the Pt electrode holder. Then, the film as a working electrode was attached to a Pt electrode holder. Subsequently, the back and sides of the electrode were covered with a non-conductive, chemically resistant epoxy (Omegabond 101). An effective electrode surface (0.2 cm × 0.2 cm; area: 0.04 cm2) was exposed to 1.0 M KOH during electrochemical measurements. The electrochemical measurements were carried out by a Biologic SP-150 potentiostat. The KOH electrolyte with a concentration of 1.0 M was prepared using deionized water (>18 MΩ cm) and KOH pellets (99.99% purity, Sigma-Aldrich). Oxygen was bubbled to ensure O2/OH− equilibrium at 1.23 V vs. RHE. All potentials were converted to RHE scale with iR correction according to the equation: E (vs. RHE) = E (vs. Hg/HgO) + 0.059 × pH + 0.098-iR, where i is the current and R is the electrolyte resistance, determined by high-frequency AC impedance (~15 Ω for 1.0 M KOH). All electrochemical data were normalized using film surface area (Supplementary Table 2 ).
6
RDE Electrochemical Experiments in Alkaline Electrolyte
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RDE electrochemical experiments were performed in a three-compartment glass cell with a rotating disk electrode (RDE, 5 mm in diameter of GC, Pine Instrument) and a potentiostat (Gamry) at room temperature. A Pt-mesh and a Hydroflex reversible hydrogen electrode (RHE, Gaskatel) were used as counter electrode and reference electrode, respectively. The electrolytes were prepared with KOH pellets (semiconductor grade, 99.99% trace metals basis, Aldrich) and MilliQ water, and were further purified75 (link),76 (link). The catalyst was deposited on the GC by drop casting from an ink based on isopropanol/water solution with Nafion as a binder. The catalyst loading was 0.1 mg cm−2. The detailed protocol is provided in Supplementary Methods .
DEMS measurements were performed using dual thin-layer electrochemical flow cell (seeSupplementary Methods for details) with nitrogen-saturated electrolyte 0.1 M KOH.
DEMS measurements were performed using dual thin-layer electrochemical flow cell (see
7
Synthesis of 1233xf in Roth Autoclave
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Example 3
In a 250 ml Roth autoclave with deep pipe and gas outlet, 50 ml 123 (73 g, 0.48 mol) were mixed with 28 g KOH pellets from Aldrich and 30 ml deionized water together with 2 g TBAB (tetrabutylammoniumbomide, 0.006 mol) also from Aldrich and the autoclave was closed. The autoclave was heated to 80° C. Afterwards, 73 g (0.48 mol) liquid 123 (using a piston pump) and 30.29 g (0.6 mol) Chloromethane (over a Bronkhorst flow meter out of a gas cylinder) were fed together over the deep pipe into the autoclave and the pressure was kept at 4 bar abs. with a pressure valve installed at the gas outlet of the autoclave. The gas stream leaving the reactor tube was fed over a 1 m cooled pipe (+25° C.) of 1 cm diameter into a water scrubber to absorb still some present HCl (most of the HCl remained in the autoclave). A GC/GC-MS analysis of the gas steam leaving the scrubber contained no 123 but mainly 1233xf. The gas stream after the scrubber was again condensed into a stainless steel cylinder (fed inlet over a deep pipe) cooled to −78° C. with CO2/EtOH.
8
Synthesis and Purification of 1233xf
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Example 3
In a 250 ml Roth autoclave with deep pipe and gas outlet, 50 ml 123 (73 g, 0.48 mol) were mixed with 28 g KOH pellets from Aldrich and 30 ml deionized water together with 2 g TBAB (tetrabutylammoniumbomide, 0.006 mol) also from Aldrich and the autoclave was closed. The autoclave was heated to 80° C. Afterwards, 73 g (0.48 mol) liquid 123 (using a piston pump) and 30.29 g (0.6 mol) Chloromethane (over a Bronkhorst flow meter out of a gas cylinder) were fed together over the deep pipe into the autoclave and the pressure was kept at 4 bar abs. with a pressure valve installed at the gas outlet of the autoclave. The gas stream leaving the reactor tube was fed over a 1 m cooled pipe (+25° C.) of 1 cm diameter into a water scrubber to absorb still some present HCl (most of the HCl remained in the autoclave). A GC/GC-MS analysis of the gas steam leaving the scrubber contained no 123 but mainly 1233xf. The gas stream after the scrubber was again condensed into a stainless steel cylinder (fed inlet over a deep pipe) cooled to −78° C. with CO2/EtOH.
9
Synthesis of 1233xf via Autoclave
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Example 3
In a 250 ml Roth autoclave with deep pipe and gas outlet, 50 ml 123 (73 g, 0.48 mol) were mixed with 28 g KOH pellets from Aldrich and 30 ml deionized water together with 2 g TBAB (tetrabutylammoniumbomide, 0.006 mol) also from Aldrich and the autoclave was closed. The autoclave was heated to 80° C. Afterwards, 73 g (0.48 mol) liquid 123 (using a piston pump) and 30.29 g (0.6 mol) Chloromethane (over a Bronkhorst flow meter out of a gas cylinder) were fed together over the deep pipe into the autoclave and the pressure was kept at 4 bar abs. with a pressure valve installed at the gas outlet of the autoclave. The gas stream leaving the reactor tube was fed over a 1 m cooled pipe (+25° C.) of 1 cm diameter into a water scrubber to absorb still some present HCl (most of the HCl remained in the autoclave). A GC/GC-MS analysis of the gas steam leaving the scrubber contained no 123 but mainly 1233xf. The gas stream after the scrubber was again condensed into a stainless steel cylinder (fed inlet over a deep pipe) cooled to −78° C. with CO2/EtOH.
10
Continuous Synthesis of 1233xf from 123
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Example 3
In a 250 ml Roth autoclave with deep pipe and gas outlet, 50 ml 123 (73 g, 0.48 mol) were mixed with 28 g KOH pellets from Aldrich and 30 ml deionized water together with 2 g TBAB (tetrabutylammoniumbromide, 0.006 mol) also from Aldrich and the autoclave was closed. The autoclave was heated to 80° C. Afterwards, 73 g (0.48 mol) liquid 123 (using a piston pump) and 30.29 g (0.6 mol) Chloromethane (over a Bronkhorst flow meter out of a gas cylinder) were fed together over the deep pipe into the autoclave and the pressure was kept at 4 bar abs. with a pressure valve installed at the gas outlet of the autoclave. The gas stream leaving the reactor tube was fed over a 1 m cooled pipe (+25° C.) of 1 cm diameter into a water scrubber to absorb still some present HCl (most of the HCl remained in the autoclave). A GC/GC-MS analysis of the gas steam leaving the scrubber contained no 123 but mainly 1233xf. The gas stream after the scrubber was again condensed into a stainless steel cylinder (fed inlet over a deep pipe) cooled to −78° C. with CO2/EtOH.
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