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19 protocols using hydriodic acid

1

Synthesis and Characterization of Methylammonium Lead Iodide Perovskite

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MAI was synthesised via the chemical reaction of 27 ml methylamine solution (CH3NH2, 40 wt.% in methanol, TCI) with 30 ml of hydriodic acid (HI 57 wt.% in water, Aldrich) in an ice bath for 2 h. The methylamine solution was added first into the round-bottom flask and then HI was dropwise added in during stirring. MAI precipitates were collected after the solution was transformed into a rotary evaporator and heated at 50 °C for 1 h. The white precipitates were washed three times with diethyl ether and finally dried in vacuum for 24 h. The PbI2 solution was prepared by dissolving 1 mole PbI2 in 1 ml DMF solvent and stirred at 70 °C and then 20 μl of DIO was added into the solution to promote the dissolution of PbI2. The PbI2 solution became clear after continuously stirring at 70 °C for overnight. Thereafter, 1.0 wt.% MAI solution was then produced by adding MAI in 2-propanol and stirred for 10 min at 50 °C. The PTB7 and PCBM solution were respectively prepared by dissolving 4 mg and 30 mg of PCBM in 1 ml of chlorobenzene. 2 mg of BCP was dissolved in 1 ml of methanol to form the BCP solution. The Al4083 PEDOT:PSS solution was used as received from Ossila (1.3 to 1.7 wt.% water solution).
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2

Synthesis and Characterization of Thiazolium Iodides

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All the following chemicals were brought from Sigma-Aldrich and used as received unless stated otherwise: bismuth(III) iodide ( powder, 99%), thiazole (97%), aminothiazole (≥98.0%), hydriodic acid (55%), water (distilled), dimethyl-formamide (≥99.0%), dimethylsulfoxide (≥99.0%) and ethanol (analytical grade). 1 H NMR was carried out in deuterated oxide (D 2 O) for thiazloium iodide and 2-aminothiazolium iodide on a Bruker Advance Pro500 spectrometer and referenced externally to SiMe 4 .
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3

Synthesis of MAPbI3 Perovskite Solution

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Methylamine (35 mL, 40% in water, TCI) and hydriodic acid (50 mL, 57 wt% in water, Aldrich) were reacted in a 250 mL round-bottom flask at 0 °C for 2 h under magnetic stirring. The precipitate was recovered by evaporation at 50 °C for 1 h. The product was then dissolved in ethanol (anhydrous 99.9%, Samchun pure chemical co., ltd.) recrystallized from diethyl ether (99.0%, Samchun pure chemical co., ltd.) and finally dried at room temperature in a vacuum oven for 24 h. 1 M of MAPbI3 perovskite solution was prepared by mixing the synthesized MAI powder (0.318 g) and PbI2 (0.924 g, 99%, Aldrich) in a mixture of γ-butyrolactone (1.4 mL, Aldrich) and dimethyl sulfoxide (0.6 mL, Aldrich) at 60 °C for 30 min.
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4

Synthesis of (PEA)2PbI4 Perovskite

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PEAI
was synthesized by mixing phenethylamine (Sigma-Aldrich) with hydriodic
acid (HI Sigma-Aldrich) in a 1:1 molar ratio at 0 °C with constant
stirring for 4 h. The solvent was then evaporated at 60 °C and
washed by cold diethyl for several times. At last, resultant was dried
at 70 °C for 12 h. For synthesis of (PEA)2PbI4 perovskite, 0.5 g of lead oxide powder (PbO Sigma-Aldrich)
was dissolved in a mixture solution of 3 mL of HI and 0.5 mL of hypophosphorous
acid (H3PO2 Sigma-Aldrich). Then the solution
was heated to 140 °C with stirring. After that, 2.5 mmol of PEAI
solution was added into the solution. At last, the stirring was stopped,
and the solution was naturally cooled down to room temperature for
crystallization.
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5

Perovskite Solar Cell Fabrication

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Lead oxide (PbO), methylamine hydrochloride (MACl), hydriodic acid (HI, 57 weight % in H2O), hypophosphorous acid (H3PO2, 50% in H2O), butylamine (BA, 99%), C60-Fullerene, PTAA, and N,N-dimethylformamide (DMF, anhydrous) were purchased from Sigma-Aldrich and used without further purification. Tektronix Keithley 2400 SMU was used for data collection. The silicon reference device (FDS 1010 Si Photodiode) was purchased from Thorlabs.
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6

Determination of Aromatic Amines

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Aromatic amines and reference substances with a purity of >97 % were purchased from Sigma-Aldrich, Steinheim, Germany and Alfa-Aesar, Karlsruhe, Germany. The reagents used for hydrolysis and derivatization, namely concentrated hydrochloric acid (37 %), hydriodic acid (55 %, unstabilized, A.C.S.), sodium nitrite (≥97 %), sodium sulphite (≥98 %), alizarinsulfonic acid (98 %), and amidosulfonic acid (99, 3 %) were all products of Sigma-Aldrich. Sodium hydroxide (99 %) was from VWR, Darmstadt, Germany, and sodium acetate (≥99 %) from Applichem, Darmstadt, Germany. Analytical grade methanol was purchased from KMF Laborchemie, Lohmar, Germany, and the ultra-filtered water used was a product of PureLab Ultra (ELGA LabWater, Celle, Germany).
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7

Synthesis of Tin(II) Halides and Antimony Trichloride

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Tin(ii) bromide, tin(ii) iodide, antimony trichloride, N,N′-dimethylethylenediamine (99%), 1-butyl-1-methylpyrrolidinium chloride, γ-butyrolactone (GBL, ≥99%), hydrobromic acid (48 wt% in H2O) and hydriodic acid (55%) were purchased from Sigma-Aldrich. Dichloromethane (DCM, 99.9%), dimethylformamide (DMF, 99.8%), toluene (anhydrous, 99.8%) and ethyl ether (stabilized with ∼1 ppm BHT) were purchased from VWR. Acetone (HPLC grade) was purchased from EMD Millipore. All reagents and solvents were used without further purification unless otherwise stated.
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8

Synthesis of F-PEAI Organic Semiconductor

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4-fluorophenethylammonium iodide (F-PEAI, purity > 99%) purchased from Xi’an Polymer Light Technology Corp. Lead(II) oxide (PbO, purity > 99.999%), Hydriodic acid (HI, 57 wt.% in water), Hypophosphorous acid solution (H3PO2, 50 wt.% in water), and Hexane (purity > 95%) purchased from Sigma–Aldrich. All materials are used as received.
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9

Synthesis of Hybrid Perovskite Materials

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Lead oxide (PbO, 99%), Methylammonium chloride (CH3NH3Cl, 99%), 2-(1-Cyclohexenyl)ethylamine (C6H9C2H4NH2+, ≥ 98%), Hydriodic acid (HI, 57 wt % in H2O), hypophosphorous acid (H3PO2, 50 wt.% in H2O), N,N-dimethylformamide (DMF, anhydrous, 99.8%), were used as received from Sigma-Aldrich.
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10

Evaluation of Plastic Evidence Bags

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Three types of plastic evidence bags were provided by the NSW Police Force: LDPE bags sourced from two different manufacturers (denoted LDPE 1 and LDPE 2) and PVC bags sourced from a third manufacturer (manufacturers names as well as polymers compositions are confidential). The three types of bags are sealable bags with adhesive closure.
Thirteen reagents regularly encountered in clandestine laboratories were examined at the request of the NSW Police based on the frequency of collection of such reagents: acetic acid (≥99.7%), acetone (≥99.9%), acetonitrile (≥99.9%), ethyl acetate (99.8%), formic acid (≥97%), hydrogen peroxide (30% in H2O), hydrochloric acid (37%), hydriodic acid (57% in H2O), hydrogen bromide (48% in H2O), methylamine (40% in H2O), methanol (99.8%), nitroethane (≥98%) and phosphoric acid (85% in H2O) (supplied by Sigma-Aldrich).
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