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13 protocols using concentrated sulphuric acid

1

Chloramphenicol Synthesis and Characterization

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Chloramphenicol (Fig. 1) and zinc nitrate were supplied by Loba Chemie (India). Concentrated sulphuric acid (99.9%), potassium tetraoxomanganate (VII), hydrogen peroxide and ethanol were purchased from Merck (UK). All the chemicals used were of analytical reagent grade or the highest purity available and were used as received.

Structure of chloramphenicol (M.W. = 323.13 g/mol).

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2

Comprehensive Polyphenol Analysis Protocol

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Concentrated sulphuric acid, mix catalyst (96% sodium sulphate anhydrous, 3.5% cuprum sulphate sulphate, 0.5% selenium dioxide, sodium hydroxide (NaOH), sulphuric acid (H2SO4), boric acid, petroleum ether, n-hexane, iodine reagent, starch, potassium acetate, and potassium iodide were purchased from Merck (Kenilworth, New Jersey, USA). While, ethanol, methanol, acetone, acetic acid (C2H4O2), hydrochloric acid, 1 M phosphate buffer solution, alpha amylase from porcine pancreas, alpha glucosidase enzyme from Saccharomyces cerevisiae, PNPG (4-Nitrophenyl-α-d-glucopranoside), and acarbose were purchased and from Sigma (St. Louis, Missouri, USA). All the authentic standard (HPLC grade) from Sigma. The standards include ellagic acid, kaempferol, chlorogenic acid, apigenin, myricetin, p-coumaric acid, proto-catechuic acid, mangiferin, ethyl gallate, vanillic acid, trans-cinnamic acid, epicatechin, catechin, quercetin hydrate, gallic acid, quercetin, ascorbic acid, and catechin.
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3

Carbonized Rubber Wood Sawdust Synthesis

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The sand was collected from the nearby area of the Howrah River, Tripura, India. The sand was washed several times with deionized water and sieved for the desire particle size of 0.25–1 mm. The rubber wood sawdust was collected from rubber wood processing industry, Nagechera, Tripura, India, and it was utilized to prepare CCRWSD. Concentrated sulphuric acid (98%) and concentrated nitric acid (98%) were purchased from Merck India. The rubber wood sawdust (10 gm) was introduced to 11 mL (98% m/m) concentrated H2SO4 and stands for 10 minutes to make it carbonized. Then carbonized slurry was added to concentrated HNO3 (6.6 mL, 65% m/m). The slurry material was heated at 150°C for 24 hours. The CCRWSD was then thoroughly washed with deionized water to remove the acid and dried at oven. Finally screening was used to get the desired particle size (0.5–1 mm).
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4

Reagents for Chemical Analysis

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The reagents used for this study are phenolphthalein, methyl orange, manganous sulphate, sodium iodide, sodium azide, starch, sodium thio-sulphate, ferrous sulphate, hydrogen peroxide (30% v/v), sodium hydroxide, concentrated hydrochloric acid, silver sulphate, mercuric sulphate, potassium dichromate, concentrated sulphuric acid, ammonium ferrous sulphate (Merck, India).
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5

Synthesis of Niobium-doped Mesoporous Silica

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Tetraethylorthosilicate (TEOS) (Sigma-Aldrich, Germany 98%), Pluronic P123 (Sigma-Aldrich, Germany), niobium(v) chloride (Sigma-Aldrich, Germany), sodium thiosulphate (Sigma-Aldrich, Germany), concentrated sulphuric acid (Merck, Germany), 1-ethanol (Sigma-Aldrich, Germany), peracetic acid 32% (Sigma-Aldrich, Germany), and distilled water. All the chemicals and reagents were used as received without any further purification.
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6

Analytical Reagents for Environmental Assays

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Hexane, dichloromethane, cycloHexane and toluene (gas chromatography grade, respectively), concentrated sulphuric acid, (analytical grade), sodium sulphate (anhydrous for analysis) and silica gel (0.063-0.200 mm, for column chromatography) were purchased from Merck (Germany). Diethyl ether (glass distilled grade) was purchased from Rathburn (Scotland). Isopropanol (chromosolv) and DMSO (for molecular biology) were purchased from Sigma. FBS Gold, defined foetal bovine serum, and Minimum Essential Medium (MEM) alpha modification were purchased from PAA laboratories (Germany). D-Luciferin was purchased from BioThema AB (Sweden). ATP was purchased from Saveen Werner AB (Sweden). The internal standards used for the chemical analysis of dioxins and PCBs in the study were from Cambridge Isotope Laboratories (CIL) and purchased from Promochem (Sweden). The dioxin standards used in the chemical-activated luciferase gene expression (CALUX) assay were purchased from Bio Detection Systems BV (Amsterdam). All other reagents used were analysis grade laboratory chemicals from standard commercial suppliers.
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7

Quantification of Halogenated Organic Compounds

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Chemicals: acetone and methanol were from Rathburn (Walkerburn, UK); hexane, ethanol, acetic acid and concentrated sulphuric acid were from Merck (Darmstadt, Germany); anhydrous sodium sulphate from VWR (Radnor, US-PA); the water was from a Milli-Q Gradient A10 system (Millipore, Bedford, MA, USA).
The solutions α-, β-, γ-Hexabromocyclododecane (50.0 ± 2.5 µg mL -1 ) as well as 13 C 12 -α-HBCD were from Wellington Laboratories (Ontario, Canada). Native and 13 C 12 -labelled PCB and PBDE congeners were from Cambridge Isotopes Laboratories Inc. (Andover, MA, USA).
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8

Synthesis of Transition Metal-Doped Graphite

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Graphite Powder (≥99.99%, Daejung Korea), Sodium Nitrate (≥99.0%, Sigma-Aldrich), Concentrated Sulphuric acid (clear, assay: 99.99%, Sigma-Aldrich), Hydrogen peroxide (30 %, Sigma-Aldrich, Germany), Iron (III) Chloride hexahydrate (99.0%, Daejung Korea) Iron (II) Sulphate heptahydrate (≥98.0%, Sigma-Aldrich), Cobalt chloride hexahydrate (99.0%, Daejung Korea), and Liquid ammonia (Sigma-Aldrich) were used in this study. All chemicals were analytical grade reagents and were used as received without further purification. Distilled water was used throughout the study.
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9

Oxidative Functionalization of MWCNTs

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1 g of MWCNTs (purchased from Aladdin, China) was mixed with 60 mL concentrated sulphuric acid (99%, Sigma-Aldrich, Shanghai, China) for one hour of ultrasonication until a uniform dispersion was formed. Then, 40 mL concentrated nitrogen acid (Sigma-Aldrich, Shanghai, China) was slowly added into the mixture and refluxed at 115 to 120 °C for 15 min under vigorous stirring. The mixture was cooled to room temperature after the reaction, filtrated and washed with deionized (DI) water until the pH of the filtrate was neutral. The remaining black residue was dried in an oven at 60 °C for ten hours and milled into a powder for use.
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10

Phytochemical Screening and Antioxidant Assays

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MEthanol (absolute) was bought from FlukaChemie GmbH (Sigma-Aldrich®, Zwijndrecht, Netherlands) and Dimethyl sulfoxide (DMSO) was purchased from RFCL Limited, Hayana, India. Dicholoro methane, ethyl acetate and Ethanol were purchased from LobaChemiePvt Ltd, Mumbai, India). 2,2-Diphenyl-1-picrylhydrazyl (DPPH) was bought from Sigma-Aldrich®.
Reagent for determination of active metabolites namely; Vanillin, Ascorbic acid, Gallic acid, Ammonium solution Concentrated sulphuric acid, Aluminium chloride, Catechin, Folin-Ciocateu’phenol reagent, Ferric chloride, Mayer’s reagent and Qualija were purchased from Sigma-Aldrich®.
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