Olive stone was used as raw material to prepare the catalyst support. Olive stone, an abundant and low-cost biomass waste from the olive oil industry, was supplied by Sociedad Cooperativa Andaluza Olivarera y Frutera San Isidro, Periana (Málaga), Spain. The olive stone was initially impregnated with phosphoric acid (H3PO4, 85% w/w, Panreac, Castellar del Vallés, Spain) at a mass ratio 2/1 (H3PO4/olive stone). After that, it was dried overnight, at 60 °C, in an oven. The mixture was introduced in a tubular furnace under a 150 cm3/min N2 (99.999%, Linde, Barcelona, Spain) flow and the temperature was raised at a heating rate of 10 °C/min to 800 °C, at which the sample remained for 2 h. Then, the sample was washed with distilled water, at 60 °C, until a constant pH was reached in the residual water, and sieved, between 100 and 300 μm. The chemically activated carbon obtained (ACP) was, subsequently, impregnated by the incipient wetness method with zirconium (IV) oxynitrate hydrate (N2O7Zr·xH2O, 99%, Sigma Aldrich, St. Louis, MO, USA). The amount of salt used was calculated to obtain a zirconium mass loading of 5.25%. The impregnated sample was then dried at 120 °C overnight and heated at 250 °C for 2 h, in a muffle furnace. A more detailed description of the catalyst preparation process can be found elsewhere [30 (link)].
H3po4
Manufactured by ITW Reagents
Sourced in Spain
H3PO4 is a chemical compound commonly known as phosphoric acid. It is a clear, colorless, odorless liquid that is widely used in various laboratory applications. The primary function of H3PO4 is to serve as a chemical reagent and buffer solution for pH adjustment and control in analytical and experimental procedures.
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Lab products found in correlation
Acetonitrile, by ITW Reagents (2 mentions)
Nah2po4, by ITW Reagents (2 mentions)
Na2hpo4, by ITW Reagents (2 mentions)
Jsm 7001f, by JEOL (1 mentions)
D8 advance twin, by Bruker (1 mentions)
Fecl3 6h2o, by ITW Reagents (1 mentions)
Zncl2, by ITW Reagents (1 mentions)
Scharlau, by Scharlab (1 mentions)
Hplc grade acetonitrile, by Scharlab (1 mentions)
Hydrochloric acid (hcl), by Merck Group (1 mentions)
Sodium hydroxide (naoh), by Merck Group (1 mentions)
Zirconium 4 oxynitrate hydrate, by Merck Group (1 mentions)
Acetamiprid, by Merck Group (1 mentions)
Filtration system, by Merck Group (1 mentions)
Potassium indigotrisulfonate, by Merck Group (1 mentions)
Sulfamethoxazole, by Merck Group (1 mentions)
Methiocarb, by Merck Group (1 mentions)
Tert butanol, by ITW Reagents (1 mentions)
Milli q water, by Merck Group (1 mentions)
Phenol, by Merck Group (1 mentions)
6 protocols using h3po4
1
Olive Stone-Derived Activated Carbon Catalyst
2
Synthesis and Characterization of nHA Nanoparticles
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The procedure followed to synthetize nHA is fully described by Z. Zhao et al. [45 (link)] Briefly, a solution of 0.2 M H3PO4 (purity 85 wt %, Panreac) was added dropwise into 100 mL of 0.334 M Ca(OH)2 (purity 96 wt%, Fluka) at a constant rate of 1 mL/min. When the pH reached 8 the reaction was stopped, and the suspension was left stirring 20–30 min. The following day, the suspension was rinsed with MilliQ water, centrifuged and lyophilized to obtain hydroxyapatite-nanoparticle powder.
The crystallinity and composition of the nanoparticles was assessed by X-Ray powder Diffraction (XRD) (D8 ADVANCE Twin, Bruker). Cu Kα radiation was used over a 2θ range of 20° – 50°. Scan step was set to 0.02, and a counting time of 2 s per point at 40 kV and 40 mA, and crystal morphology was assessed using a field emission Scanning Electron Microscopy (SEM, JEOL JSM-7001F). Prior to observation, the nHA were sputtered with carbon (EMITECH K950X Turbo Evaporator, Quorum Technologies Ltd., UK) to avoid charging effects.
The crystallinity and composition of the nanoparticles was assessed by X-Ray powder Diffraction (XRD) (D8 ADVANCE Twin, Bruker). Cu Kα radiation was used over a 2θ range of 20° – 50°. Scan step was set to 0.02, and a counting time of 2 s per point at 40 kV and 40 mA, and crystal morphology was assessed using a field emission Scanning Electron Microscopy (SEM, JEOL JSM-7001F). Prior to observation, the nHA were sputtered with carbon (EMITECH K950X Turbo Evaporator, Quorum Technologies Ltd., UK) to avoid charging effects.
3
Activated Carbons from Lignin Precursor
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Lignin (from LignoTech Ibérica S.A., Cantabria, Spain) was selected as the carbon precursor for activated carbons. FeCl3·6H2O (≥97%), ZnCl2 (97%), H3PO4 (85%) and KOH (85%), used as agents for the chemical activation of lignin, were all purchased from Panreac (Panreac Química S.L.U., Barcelona, Spain). Titanium tetrabutoxide (Ti(OBu)4; ≥97%) was supplied by Sigma Aldrich (Sigma-Aldrich Co., St. Louis, MO, USA). Ethanol (EtOH; 96%) was obtained from Panreac (Panreac Química S.L.U., Barcelona, Spain). HCl (≥37%) and NaOH (≥95%) were purchased from Sigma Aldrich (Sigma-Aldrich Co., St. Louis, MO, USA) and Scharlau (Scharlab S.L., Barcelona, Spain), respectively. Acetaminophen (ACE; ≥99%, from Sigma-Aldrich Co., St. Louis, MO, USA) was selected as the target emerging contaminant. Acetonitrile (HPLC grade, Scharlau, Scharlab S.L., Barcelona, Spain) and acetic acid (≥99%, Sigma Aldrich Sigma-Aldrich Co., St. Louis, MO, USA) were used as the mobile phase for liquid chromatography. Ultrapure water (Type I, 18.2 MΩ·cm) and deionized water (Type II) were used in this work.
4
Activated Carbon from Mango Pits
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Mango pits were cut into pieces with a size of 1-2 cm, washed with distilled water under stirring in ambient temperature for 3 h and then dried in an oven at 120 °C in air overnight. The dried pieces were ground in a planetary ball mill (PM100 model, Retsch) at 300 rpm for 30 min using a 125 mL grinding jar with 8 stainless steel balls (10 mm diameter). Then, the obtained powder was impregnated with a solution of H3PO4 (85 %, Panreac) in a mass ratio of 1:1 and subsequently heated in a hot plate under stirring at 85 °C for 3 h until a solid paste was obtained, which was dried at 120 °C in overnight.
The impregnated product was ground again in the planetary ball mill at 300 rpm for 30 min, heated at 10 °C min -1 in a tubular furnace (ST-11 model, Hobersal) to 700 °C and calcinated for 2 h under a N2 atmosphere (flow rate of 50 mL min -1 ). To remove the impurities, the sample was treated with a solution of 3 M HCl (37 %, Panreac) and heated in a hot plate under stirring at 80 °C for 3 h and then washed with distilled water until neutral pH was achieved. The resulting powder was dried in an oven in air at 120 °C for one day. The activated carbon obtained from mango pit is indicated in the work using the acronym MPAC.
The impregnated product was ground again in the planetary ball mill at 300 rpm for 30 min, heated at 10 °C min -1 in a tubular furnace (ST-11 model, Hobersal) to 700 °C and calcinated for 2 h under a N2 atmosphere (flow rate of 50 mL min -1 ). To remove the impurities, the sample was treated with a solution of 3 M HCl (37 %, Panreac) and heated in a hot plate under stirring at 80 °C for 3 h and then washed with distilled water until neutral pH was achieved. The resulting powder was dried in an oven in air at 120 °C for one day. The activated carbon obtained from mango pit is indicated in the work using the acronym MPAC.
5
Stability of Acetamiprid in Ozonation Experiments
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Acetamiprid and p-chlorobenzoic acid analytical standards, as well as potassium indigotrisulfonate, were acquired from Sigma-Aldrich (Germany). Na2HPO4, NaH2PO4, H3PO4 and acetonitrile were purchased from Panreac (Spain), and were all analytical grade. Milli-Q water was produced by a filtration system (Millipore, USA). Pure oxygen ( ≥ 99.999%) was supplied by Abelló Linde (Spain).
In order to control the effects of side mechanisms like hydrolysis, adsorption or UV-Vis photolysis on ACMP disappearance during ozonation experiments, several control assays were performed. All runs were carried out in 250 mL closed glass beakers, with initial ACMP concentrations of 1 mg L -1 . For hydrolysis and adsorption experiments, the beaker was covered with aluminum foil in order to avoid the possible influence of ambient radiation. The pH in hydrolysis tests was adjusted to a value of 2 or 7 by adding adequate quantities of H3PO4 and Na2HPO4. For adsorption experiments, several plastic materials (different types of silicones, PVDF and PTFE) usually employed in laboratory were put in contact with the pesticide solution. In all experiments, the medium was under stirring conditions. Samples were withdrawn at 0, 1, 5 and 24 h, and analyzed by HPLC-DAD. Results showed that ACMP remained stable prior to oxidant addition.
In order to control the effects of side mechanisms like hydrolysis, adsorption or UV-Vis photolysis on ACMP disappearance during ozonation experiments, several control assays were performed. All runs were carried out in 250 mL closed glass beakers, with initial ACMP concentrations of 1 mg L -1 . For hydrolysis and adsorption experiments, the beaker was covered with aluminum foil in order to avoid the possible influence of ambient radiation. The pH in hydrolysis tests was adjusted to a value of 2 or 7 by adding adequate quantities of H3PO4 and Na2HPO4. For adsorption experiments, several plastic materials (different types of silicones, PVDF and PTFE) usually employed in laboratory were put in contact with the pesticide solution. In all experiments, the medium was under stirring conditions. Samples were withdrawn at 0, 1, 5 and 24 h, and analyzed by HPLC-DAD. Results showed that ACMP remained stable prior to oxidant addition.
6
Adsorption Mitigation for Methiocarb Analysis
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Methiocarb, sulfamethoxazole and phenol analytical standards were acquired from Sigma-Aldrich (Germany). NaH2PO4, Na2HPO4, H3PO4, tert-butanol and acetonitrile were purchased from Panreac (Spain), and were all analytical grade. Milli-Q water was produced by a filtration system (Millipore, USA). Finally, all the reagents employed during toxicity bioassays were purchased from Modern Water (UK).
As early commented, MC was suspected to be adsorbed to some non-polar materials, due to its hydrophobicity. In order to be sure about that, some preliminary experiments were performed. Results revealed important losses of MC when aqueous solutions of this chemical were put in contact with plastic elements (i.e. filters, tubing), whereas this was not observed when working with glassware. Therefore, glass was selected as material for handling MC solutions during experimentation.
As early commented, MC was suspected to be adsorbed to some non-polar materials, due to its hydrophobicity. In order to be sure about that, some preliminary experiments were performed. Results revealed important losses of MC when aqueous solutions of this chemical were put in contact with plastic elements (i.e. filters, tubing), whereas this was not observed when working with glassware. Therefore, glass was selected as material for handling MC solutions during experimentation.
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