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5 protocols using potassium indigotrisulfonate

1

Electrochemical Biosensor Reagents Synthesis

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Potassium cyanide, sodium nitrite, ethylenediaminetetraacetic acid disodium salt (EDTA), anthroquinone-2-sulfonic acid sodium salt monohydrate, methyl viologen hydrate and safranine-O were purchased from Acros Organics. Anthroquinone-1,5-disulfonic acid disodium salt hydrate, hexaammineruthenium(III) chloride, potassium indigo trisulfonate, potassium indigo tetrasulfonate and indigo carmine were purchased from Sigma-Aldrich. Sodium chloride and 2-[4-(2-hydroxyethyl)-piperazin-1-yl]ethanesulfonic acid (HEPES) sodium salt were from Fisher Scientific. The mediator Diquat (6,7-dihydrodipyrido[1,2-a:2′,1′-c]pyrazinediium dibromide, Table 1) was synthesized using the method described by Homer and Tomlinson(20 ).
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2

Synthesis of Cerium Phosphate Nanomaterials

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Cerium(III) nitrate hexahydrate (Ce(NO3)3 × 6H2O, Sigma-Aldrich, ACS Reagent, 99.99%), sodium hydroxide (NaOH, POCH, ACS reagent), ammonium phosphate dibasic ((NH4)2HPO4, Sigma-Aldrich, ACS reagent, ≥ 98%), potassium bromide (KBr, Sigma-Aldrich, FT-IR grade, ≥ 99%), hydrochloric acid (HCl, Chempur, 38%), perchloric acid (HClO4, Fisher Chemicals 60%) potassium indigotrisulfonate (Sigma Aldrich > 60%), tert-butyl alcohol (TBA, Sigma-Aldrich, ≥ 99.5%), benzoic acid (BA, Sigma-Aldrich ≥ 99.5%). All chemicals were used without further purification. Deionized water was used during synthesis. In ozonation and adsorption experiments high purity (Merck-Millipore) water was used.
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3

Measuring Ozone Concentrations by Meter and Indigo

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Ozone concentrations were determined by both an ozone meter (OZ 2000G), and the indigo method. The ozone meter was used to determine the concentration of ozone in the chamber, and the indigo method to make sure that the ozone reached the same concentration in conditions with and without ion capture. In the case of the ozone meter, the air sampler was placed at the bottom of the chamber and the air was sampled every 15 min for 2 h. For the indigo method, 12.5 μM of potassium indigotrisulfonate (Sigma, Inc., St Louis, MO, USA) solution was exposed in a 60Φ dish with stirring. Decolorization of the blue potassium indigotrisulfonate solution by dissolved ozone was measured with a SpectraMax M2 multi-microplate reader (Molecular Devices) at 600 nm.
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4

Kinetics of Micropollutant Ozonation

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Nineteen environmentally-relevant micropollutants with differing physical-chemical properties (molecular weight, hydrophobicity, pK a , structures, reactivity with ozone; see Tables S2-S4 compounds, second-order rate constants for their reaction with ozone were experimentally determined as described in Text S1 and Fig. S1. The rate constants are compiled in SI, Table S4.
A stock solution was prepared by dissolving the 19 parent compounds (each at 1 mg L -1 ) in ultrapure water overnight. To enhance the solubility of the majority of the compounds, the pH was adjusted to 7
with 1 M NaOH and the solution was heated to 40 °C.
Potassium indigo trisulfonate, sodium bromide and hydrogen peroxide (35% (w/w) in H 2 O) were obtained from Sigma-Aldrich (Buchs, Switzerland).
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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.
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