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14 protocols using sulfuric acid

1

Synthesis and Characterization of Polymeric Materials

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Acetonitrile (#271004,
99.8%, MW = 41.08 g/mol), acrylamide (#A9909, 99%, MW = 71.08 g/mol),
azobis(2-methylpropionitrile) (#441090, 98%, MW = 164.31 g/mol), glyphosate
(#45521, 98%, MW = 169.07 g/mol), N,N′-methylenebis(acrylamide) (#146072, 99%, MW = 154.17 g/mol),
toluene (#244511, 99.8%, MW = 92.14 g/mol), and trimethoxy(7-octen-1-yl)silane
(#452815, 80%, MW = 232.39 g/mol) were purchased from Merck (Poznan,
Poland). Ethanol (#BA6480111, 99.8%, MW = 46.08 g/mol) and isopropanol
(#BA1500111, 99.7%, MW = 60.11 g/mol) were from POCh (Warsaw, Poland).
Hydrogen peroxide (#118851934, analytical grade, MW = 34.01 g/mol)
and sulfuric acid (#115750013, 98%, MW = 98.08 g/mol) were procured
from Chempur (Piekary Slaskie, Poland). Acetone (#50-8123, 99.8%,
MW = 58.08 g/mol) was obtained from Linegal Chemicals (Warsaw, Poland).
Fused silica slides were provided by TedPella (GE124, #26009; Redding,
CA), while commercial fused silica microcapillaries were purchased
from Postnova (#FSS-Z-200280; Landsberg, Germany).
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2

Synthesis and Characterization of Polyaniline Nanofibers

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Chemical substances used for synthesis of aniline nanofibers, aniline monomer, hydrochloric acid (HCl), ammonium persulfate (APS) and tetrahydrofuran (THF), were purchased from Chempur (Piekary Slaskie, Poland). Polyaniline nanofibers doped with Cl- ion-synthesized following the procedure described in the publication [39 (link)]. Substances necessary for preparation of the membrane mixture were purchased from Sigma-Aldrich (Saint Louis, MO, USA) (chloride ionophore III-selectophore, tridodecylmethylammonium chloride (TDMACl) and high-molecular-weight poly(vinyl) chloride) (PVC)) and Fluka (Buchs, Switzerland) (bis(2-ethylhexyl) sebacate (DOS)). Sulfuric acid and sodium hydroxide used to measure the dependence of the electrode potential on changes in pH were obtained from Chempur, while the salts of iron(II) (Na4Fe(CN)6 × 10H2O) and iron(III) (K3Fe(CN)6) were used to prepare the solutions differing in redox potential, respectively, from Alfa Aesar (Haverhill, MA, USA) and PPH (Polish Chemical Reagents, Gliwice, Poland). Other substances, such as inorganic salts, used to prepare the solution of the main ion (NaCl) and sodium salts of selected interfering anions (NaH2PO4, CH3COONa, Na2CO3, NaNO3, NaNO2, Na2SO4, NaF, NaBr) were purchased from Fluka. Salts of the highest purity available (pure pro analysis) and freshly deionized water were used to prepare all solutions.
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3

Surface Functionalization of Silicon Wafers

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Polished silicon wafers were purchased from ON Semiconductor (Rožnov pod Radhoštěm, Czech Republic). 3-Aminopropyl-trimethoxysilane (APTES), 2-bromoisobutyryl bromide (BriBBr, 98%), ethyl 2-bromo-2-methylpropionate (EBIB, 98%), triethylamine (TEA, >99.5%) tetrahydrofuran (THF, >99.9%), acetone (DMK, >99.9%), tetrabutylammonium perchlorate (TBAP, >98%), and sodium bromide (NaBr, >99%) were purchased from Sigma Aldrich (Saint Louis, MO, USA). Dichloromethane (DCM, >99.5%), toluene (>99.5%), methanol (MeOH, >99.8), ethanol (EtOH, 99.9%), hydrogen peroxide (H2O2, 30%), and sulfuric acid (>95%) were purchased from Chempur (Piekary Śląskie, Poland). N,N-Dimethylformamide (DMF, 99.9%) was purchased from Acros (Fair Lawn, NJ, USA). These reagents were used without further purification. Tris(2-pyridylmethyl)amine (TMPA) was synthesized according to a published procedure [61 (link)]. A CuIIBr2/TPMA stock solution was prepared according to reference [62 (link)]. 2-Hydroxyethyl acrylate (HEA; 96%; Aldrich) and tert-butyl acrylate (tBA; >99%; Aldrich) were passed through a column filled with basic alumina prior to use to remove monomethyl ether hydroquinone as an inhibitor. Al wire was purchased from Alfa Aesar (Tewksbury, MA, USA). LDPE cable ties were purchased from LUX-Tools (Wermelskirchen, Germany).
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4

Quantitative Analysis of Sulfonamide and Trimethoprim

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Analytical standards of sulfamethoxazole (SMX) and trimethoprim (TRI) were purchased from Sigma-Aldrich (St. Louis, MO, USA). Hypergrade acetonitrile, formic acid, and water were purchased from Merck (Darmstadt, Germany). Analytical-grade methanol, hydrochloric acid, sulfuric acid, and disodium phosphate were purchased from CHEMPUR (Piekary Śląskie, Poland). Analytical-grade acetic acid was purchased from POCH S.A. (Gliwice, Poland). Analytical-grade acetonitrile was purchased from Eurochem (Tarnów, Poland). Analytical-grade citric acid, formic acid, and acetic acid were purchased from ChemLand (Stargard, Poland). Analytical-grade sodium hydroxide was purchased from POCH S.A. (Gliwice, Poland). Oasis HLB cartridges of varying masses of sorbent (500 mg, 6 mL; 400 mg, 6 mL; 200 mg, 3 mL) from Waters (Eschborn, Germany) were used for solid-phase extraction.
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5

Synthesis of Boron Nitride Nanoparticles

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Hexagonal boron nitride, gold(III) chloride trihydrate, phosphate buffered saline, polyethylene glycol, Pluronic F-127, dehydrate trisodium citrate were purchased from Sigma-Aldrich (St. Louis, MO, USA). Hydrogen peroxide solution, sulfuric acid, potassium permanganate and 1-methyl-2-pyrrolidinone were obtained from Chempur (Piekary Slaskie, Poland).
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6

Surface Functionalization of Silicon Wafers

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Silicon wafers were obtained from ON Semiconductor (Roznov, Czech Republic). Hydrogen peroxide (30%, p.a.), sulfuric acid (96%, p.a.), hydrochloric acid (35–38%, p.a.), toluene (p.a.), tetrahydrofuran (THF, p.a.), dichloromethane (DCM, p.a.), ethanol (p.a.), and methanol (p.a.) were purchased from Chempur (Piekary Slaskie, Poland). In addition to this, (3-aminopropyl) trimethoxysilane (APTES, 99%), α-bromophenylacetyl chloride (BPA-Cl, technical, 80%), triethylamine (TEA, puriss. p.a., ≥99.5%, GC), ethyl α-bromophenylacetate (EBPA, 97%), and methyl methacrylate (MMA, 99%, ≤30 ppm MEHQ as an inhibitor) were purchased from Sigma Aldrich. Anisole (>99%), tetrabutylammonium bromide (TBABr, 99%) were purchased from Fluorochem (Hadfield, UK). Iron (III) bromide (FeBr3, anhydrous, >98%) was obtained from Alfa Aesar and stored in an argon atmosphere. MMA was passed through the basic alumina column to remove inhibitors before the polymerization, while anisole was passed through a neutral alumina column and dried over molecular sieves under argon atmosphere. Rest of chemicals were used as received.
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7

Polyphenol Quantification and Antioxidant Assays

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Cyanidin 3 O-glucoside (Cy3-glc) was purchased from Extrasynthese (Lyon Nord, France). 5 O-caffeoylquinic acid (5-CQA, chlorogenic acid), quercetin 3 O-rutinoside, (+)-catechin, sugar standards, 1,1-diphenyl-2-picrylhydrazyl radical (DPPH); 2,4,6-tri(2-pyridyl)-s-triazine (TPTZ), 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox); acetonitrile (gradient grade for HPLC), methanol, and formic acid (98–100%) were acquired from Sigma-Aldrich (Germany, Schnelldorf). Organic acids were purchased from Supelco Analytical (Bellefonte, PA, USA). Sulfuric acid, Folin–Ciocalteu reagent, hydrochloric acid, acetic acid, sodium carbonate and sodium acetate were purchased from Chempur (Piekary Śląskie, Poland).
All reagents were of analytical grade.
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8

Fabrication of Graphene Oxide Sheets

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Copper sheets (purity: 99.99%, size 10 × 15 mm, thickness: 1 mm, not annealed), graphite powder (325 mesh, purity: 99.9995%, Alfa Aesar, Haverhill, MA, USA), potassium permanganate (KMnO4, purity: 99.0%, POCH, Gliwice, Poland), orthophosphoric acid (H3PO4, 85%, POCH), sulfuric acid (H2SO4, 95%, POCH), hydrogen peroxide (H2O2, 30%, CHEMPUR, Piekary Slaskie, Poland), ethanol (C2H5OH, 96%, POCH), hydrochloric acid (HCl, 35–38%, POCH), acetone ((CH3)2CO, POCH), ammonium thiocyanate (NH4SCN, purity: 99.0%, POCH), and sodium chloride (NaCl, purity: 99.5%, POCH) were used.
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9

Oxidative Functionalization of Cyclic Ketones

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The following were used: cyclopentanone (Sigma-Aldrich, St. Louis, MI, USA, ≥99%), cyclohexanone (Sigma-Aldrich, ≥99%), cycloheptanone (Sigma-Aldrich, ≥99%), cyclooctanone (Sigma-Aldrich, ≥98%), cyclododecanone (Merck, Rahway, NJ USA, ≥98%), 2-methylcyclohexanone (Aldrich, St. Louis, MI, USA, ≥98%), 3-methylcyclohexanone (Aldrich, ≥97%), 4-methylcyclohexanone (Aldrich, ≥99%), cyclohexanol (Sigma-Aldrich, >99%), cyclohexane (Sigma-Aldrich, >99%), manganese(II) acetylacetonate (Sigma-Aldrich, 99%), cobalt(II) acetylacetonate (Sigma-Aldrich, 97%), manganese(II) acetate tetrahydrate (Sigma-Aldrich, 99.99%), cobalt(II) acetate tetrahydrate (Sigma-Aldrich, 99.99%), manganase(II) nitrate tetrahydrate (Sigma-Aldrich, ≥97%), cobalt(II) nitrate hexahydrate (Sigma-Aldrich, >99%), isopentyl nitrite (Sigma-Aldrich, 96%), tert-butyl nitrite (Sigma-Aldrich, 90%), N-hydroxyphthalimide (Acros, Waltham, MA, USA, 98%), methyl ethyl ketone (Sigma-Aldrich, 99.7%), nitric acid (Sigma-Aldrich, 60%), pentyl nitrite (Sigma-Aldrich, 98%), acetic acid (Chempur, Karlsruhe, Germany, 99.5%), acetonitrile (Chempur, 99.5%), benzonitrile (Sigma-Aldrich, 99%), sulfuric acid (Chempur, 98%), and methanol (Chempur, 99.8%).
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10

Selective Oxidation of Cyclohexane

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Cyclohexanone (Grupa Azoty S.A., Puławy, Poland, ≥99.9%), cyclohexane (Grupa Azoty S.A., Puławy, Poland, ≥99,9%), cyclohexanol (Grupa Azoty S.A., Puławy, Poland, ≥99.9%), manganese(II) acetylacetonate (Sigma-Aldrich, 99%), cobalt(II) acetylacetonate (Sigma-Aldrich, 97%), sulfuric acid (Chempur, 95%), methanol (Chempur, 99.8%), acetic acid (Chempur, 99.5%), acetonitrile (Chempur, 99.5%), benzonitrile (Chempur 99.5%), N-hydroxyphthalimide (Sigma-Aldrich, 97%).
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