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6 protocols using copper 2 perchlorate hexahydrate

1

Synthesis and Characterization of Copper(II) Chalcone Complexes

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All of the reagents used, namely 3-hydroxybenzaldehyde (3-HBA; ≥99%), 2-pyridinecarboxaldehyde (2-PCA; 99%), 2′,4′-dihydroxy-2-methoxychalcone (DH-2-MC; 97%), 2′,4′-dihydroxy-3-methoxychalcone (DH-3-MC; 97%), and copper(II) perchlorate hexahydrate (98%), were obtained from Sigma Aldrich (St. Louis, MO, USA). All of the solvents were of purity grade p.a. and were used without any purification. Methanol (MeOH) and hydrochloric acid (HCl) were purchased from Stanlab (Lublin, Poland), dichloromethane (DCM) from Eurochem BGD (Tarnów, Poland), and ethyl alcohol absolute (EtOH) from POCH (Gliwice, Poland).
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2

Synthesis and Characterization of Metal Complexes

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Chemicals were purchased from commercial sources and used without further purification, unless otherwise noted. Tetraethyl orthosilicate, cetyltrimethylammonium bromide, sodium aluminate, sodium hydroxide, aqueous solutions of hydrogen peroxide (30 wt%) and perchloric acid (60%) were purchased from Wako Pure Chemical Industries. Tris(2-pyridylmethyl)amine and oxo[5,10,15,20-tetra(4-pyridyl)porphyrinato]titanium(iv) (Ti–TPyP) were supplied from Tokyo Chemical Industry. Copper(ii) perchlorate hexahydrate was supplied by Sigma-Aldrich. Acetone and acetonitrile were purchased from Nacalai tesque as a spectral grade and used as received. Ultra-pure water was provided by a water purification system, Millipore Direct-Q3 UV, wherein the electronic conductance was 18.2 MΩ cm. Benzene was purchased from Wako Pure Chemical Industries and purified by washing with sulphuric acid and water following distillation. [Cu(tmpa)(CH3CN)](ClO4)2, [Cu(tepa)(ClO4)]ClO4, [CuII2(N5)(H2O)2](NO3)4 and Al-MCM-41 were synthesised by literature methods.53a ,61 (link)–64
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3

Fabrication and Sensing of Metal Ions

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All reagents used for device fabrication and sensing were utilized without further pre-treatment. ARS, a commercially available river sample with trace elements in river water (Elevated Level, NMIJ CRM 7202-c, Supplementary Table S1), and iron(III) nitrate enneahydrate (Fe3+) were obtained from FUJIFILM Wako Pure Chemical Co., Ltd. The target metal ions including cobalt(II) perchlorate hexahydrate (Co2+), calcium perchlorate tetrahydrate (Ca2+), lead(II) perchlorate trihydrate (Pb2+), cadmium perchlorate hydrate (Cd2+), nickel(II) perchlorate hexahydrate (Ni2+), copper(II) perchlorate hexahydrate (Cu2+), magnesium perchlorate hexahydrate (Mg2+), aluminum perchlorate non-ahydrate (Al3+), mercury(II) perchlorate hydrate (Hg2+), and zinc perchlorate hexahydrate (Zn2+) were purchased from Sigma-Aldrich. The building blocks of the chemosensors purchased from Tokyo Chemical Industry Co., Ltd. were 3-NPBA, BPR, PR, and PV. A buffer material purchased from DOJINDO was 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES). All aqueous solutions were prepared using Milli-Q water (18.2 Ω cm).
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4

Synthesis and Characterization of Liquid Crystals

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11-Mercaptoundecanoic acid (MUA), aluminum (III) perchlorate nonahydrate,
aluminum (III) nitrate nonahydrate, copper (II) perchlorate hexahydrate, and
copper (II) chloride dehydrate salts were purchased from Sigma Aldrich
(Milwaukee, WI). Aluminum (III) acetylacetonate was purchased from Alfa-Aesar
(Ward Hill, MA). 5CB was purchased from EMD Chemicals (Gibbstown, NJ). Titanium
(99.999%) and gold (99.999%) were purchased from Advanced
Materials (Spring Valley, NY). Methanol and Fischer’s Finest glass
slides were purchased from Fischer Scientific (Pittsburgh, PA). Absolute ethanol
(anhydrous, 200 proof) was purchased from Pharmco-AAPER (Brookfield, CT). All
chemicals and solvents were of analytical reagent grade and were used as
received without any further purification. All deionized water used in the study
possessed a resistivity of at least 18.2 MΩ cm.
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5

Synthesis of Copper(II) Coordination Complexes

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The chemicals for synthesis of the complexes were purchased from Sigma-Aldrich (Darmstadt, Germany) (copper(II) perchlorate hexahydrate (≥99.99% trace metals basis), 2,2′-bipyridine (bpy, 99%), 1,10-phenanthroline (phen, 99%), 1-phenyl-1,3-butanedione (99%) and 3-amino-4H-1,2,4-triazole (96%)) and Merck (Darmstadt, Germany) (dibenzo-18-crown-6-ether, potassium superoxide) as reagent grade and were used as received, without further purification. The 5-phenyl-7-methyl-1,2,4-triazolo[1,5-a]pyrimidine (pmtp) was synthesized by a method reported in the literature [30 (link)].
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6

Synthesis of Copper(II) Complexes with Heterocyclic Ligands

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The chemicals for the synthesis of the complexes were purchased from Sigma-Aldrich (Darmstadt, Germany) (copper(II) perchlorate hexahydrate (≥99.99% trace metals basis), 2,2′-biyridine (bpy, 99%), 1,10-phenantroline (phen, 99%), 2,3-pentanedione (97%) and 3-amino-4H-1,2,4-triazole (96%)) and Merck (Darmstadt, Germany; dibenzo-18-crown-6-ether, potassium superoxide) at reagent grade and were used as received, without further purification. The 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine (dmtp) was synthesized by [1+1} condensation of 3-amino-4H-1,2,4-triazole and 2,3-pentanedione.
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