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11 protocols using acetic acid

1

Synthesis of Ag-modified TiO2 Nanoparticles

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Employing the bottom-up sol-gel procedure, the synthesis of the TiO2 nanoparticles, chemically modified with silver, was realized. Thus, 25 mL of titanium isopropoxide (97%, Sigma-Aldrich, Darmstadt, Germany) was added to acetic acid (48 mL) (99–100%, Chem-Lab NV, Zedelgem, Belgium) under stirring. Deionized water (150 mL), including 5 mol of 99.8% silver nitrate (Fisher Scientific Chemical, Loughborough, UK), was then added to the solution, drop-wise under vigorous stirring. After 5 h of stirring, the solution was a clear sol (titanium isopropoxide, acetic acid and water were used according to 1:10:100 molar ratio). The new solution was then heated until the solvent had been completely evaporated. Afterward, the prepared gel was consequently calcinated at 600 °C for 2 h. The resulting nanopowder was triturated, then purified via rinsing and centrifuged in order to remove any remaining impurities. In the end, it had a gray color (Figure 2).
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2

Chitosan-based Film Characterization

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Chitosan was obtained from Seikagaku Corporation (Tokyo, Japan). Inorganic salts (reagent grade) used for adjusting the relative humidity in chambers employed to determine the water sorption behavior of the Chitosan-based films were from Merck KGaA (Darmstadt, Germany). Folin–Ciocalteu was from Fluka (Steinheim, Germany). Gallic acid, glycerol (>99%), and choline cloride were from Sigma Chemical Co (St. Louis, MO, USA). Quercetin (quercetin dehydrate, 97%) was from Alfa Aesar GmbH & Co KG, whereas acetic acid (glacial 99–100% a.r.) was from Chem-Lab NV. All aqueous solutions were made using distilled water of HPLC quality.
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3

pH-Sensitive Textile Sensors Development

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The cotton and polyester jersey knits were provided by A. Ferreira & Filhos. One knit was composed of 100% polyester with a thickness of 0.68 mm and a mass per unit area of 207 g/m2 and the other of 100% cotton with a thickness of 0.89 mm and a mass per unit area of 187 g/m2. The pH indicators used for the development of the sensors were methyl red (C15H15N3O2), methyl red sodium salt (C15H15N3O2Na), methyl orange (C14H14N3NaO3S), bromocresol purple (C21H16Br2O5S), bromothymol blue (C27H28Br2O5S) and were purchased from Sigma-Aldrich (St. Louis, Mo., EUA). The chemicals used in the evaluation of samples sensitivity were the following: acetic acid acquired from Chem-lab (Zedelgem, Belgium); sodium hydroxide purchased from Normax (Marinha Grande, Portugal); formic acid obtained from Fisher Scientific (Hampton, NH., EUA); ammonia purchased from VWR Chemicals (Radnor, PA, EUA); and citric acid acquired from Scharlau (Barcelona, Spain). The polyurethane polymeric base employed in the preparation of pH-sensitive formulations before application on fibrous substrates, Edolan SN and Thickener A02 were purchased from ADI Center Portugal, S.A (Santo Tirso, Portugal). Glycerol was obtained from Scharlau. The filter paper, used as substrate in one part of this work, was purchased from Normax.
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4

Abiraterone Acetate: Characterization and Analysis

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Abiraterone, abiraterone acetate, their deuterated counterparts abiraterone-d4, abiraterone acetate-d4, N-oxide abiraterone sulfate, and abiraterone sulfate were kindly provided by Janssen Research & Development (Beerse, Belgium). Sigma-Aldrich (St. Louis, MO) supplied pancreatin from porcine pancreas (powder, suitable for cell culture, 4Â USP specifications). Methanol and ethanol absolute were purchased from VWR International (Leuven, Belgium). Acetonitrile and dimethyl sulfoxide were obtained from Acros-Organics (Geel, Belgium). Acetic acid was obtained from Chem-lab (Zedelgem, Belgium). Water was purified with a Maxima system (Elga Ltd., High Wycombe Bucks, UK). Methyl-tert-butyl ether was purchased from Merck (Overijse, Belgium). Ketamine (Anesketin) and xylazin (Xyl-M 2%) were obtained from Eurovet (Heusden, Belgium) and VMD (Arendonk, Belgium), respectively. Hanks' Balanced Salt Solution and 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid were obtained from Lonza (Verviers, Belgium). For the measurements of the pH, a Portamess 911 pH-meter (Knick GmbH & Company, Berlin, Germany) was used. All stock solutions were prepared in dimethyl sulfoxide.
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5

Fabrication of Fluorinated Chitosan Hydrogels

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Tetraethyl orthosilicate (TEOS) was purchased from Merck (Germany); ammonia solution 25% from LabCHEM (Portugal); chitosan 95/20 (degree of deacetylation ≥ 92.6%; molecular weight = 40 – 150 kDa) from HMC Chitosan (Germany); and acetic acid from Chem-Lab (Belgium). 1H,1H,2H,2H-perfluorodecyltriethoxysilane, methacrylic anhydride, dialysis tubing cellulose membrane (flat width 33 mm, MWCO 14 kDa), 2-Hydroxy-4’-(2-hydroxyethoxy)-2-methylpropiophenone, albumin from bovine serum (BSA), phosphate buffered saline (PBS), DMEM (Dulbecco's Modified Eagle Medium) low glucose, sodium bicarbonate were purchased from Sigma-Aldrich (USA). Fetal bovine serum (FBS) was purchased from Biochrom AG (Germany); penicillin-streptomycin (100U/100 g.mL-1), trypsin (TrypleExpress), DPBS (PBS without calcium and magnesium), Calcein-AM, propidium iodide (PI), and Micro BCA Protein Assay Kit™ were supplied by ThermoFisher Scientific (USA).
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6

TDF Degradation Protocol for Mono-ester Intermediate

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TDF was provided by the NIH AIDS Research and Reference Reagent Program (Germantown, MD). TFV was obtained from Watson International (Kunshan City, China). Dimethylsulfoxide (DMSO) and tetrabutylammonium sulfate were obtained from Acros-Organics (Geel, Belgium). Acetic acid was obtained from Chem-lab (Zedelgem, Belgium). Acetonitrile was purchased from Fisher Scientific (Leicestershire, UK). Monobasic potassium phosphate monohydrate (KH2PO4.H2O), bis-4nitrophenylphosphate, chloroacetaldehyde and pancreatin from porcine pancreas (powder, suitable for cell culture, 4× USP specifications) were obtained from Sigma-Aldrich (St. Louis, MO). Methanol and sodium acetate were purchased from VWR International (Leuven, Belgium). Water was purified with a Maxima system (Elga Ltd., High Wycombe Bucks, UK). All stock solutions were prepared in dimethyl sulfoxide. The mono-ester intermediate of TDF was obtained by degradation of TDF at neutral pH: a 100µM solution of TDF was made in a phosphate buffer (pH 7); following chemical degradation during 7h at 60°C, an equal amount of 1M HCl was added to the solution; quantitative transformation into the intermediate without formation of TFV was confirmed.
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7

Polyphenol Analytical Standards Protocol

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Analytical standards of the polyphenols were a kind offer from the lab of Dr. Nadjet Benaida-Debbache in Université de Bejaia, in Algeria and were obtained from Sigma-Aldrich (Sigma-Aldrich Chemie GmbH, Taufkirchen, Germany).
Acetonitrile (ACN), for LC-MS (CHEM-LAB NV, Zedelgeme, Belgium), Methanol (MeOH) for LC-MS (CHEM-LAB NV, Zedelgeme, Belgium) and Acetic acid (CHEM-LAB NV, Zedelgeme, Belgium) were used for mobile phase preparation for LC–MS analysis.
Polyphenols are highly antioxidant molecules thus should carefully handle and be kept in dark during the experimental process.
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8

Ramie Fiber Reinforced PLA Composites

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Pure
ramie fibers were
obtained from Stucken Melchers GmbH & Co. (Germany). l-Lactide was supplied by Purac (The Netherlands) and recrystallized
from dry toluene. Poly(ethylene glycol) monomethyl ether (PEGME) (Mn = 2000 g·mol–1, with
a polydispersity index of 1.05) was provided
by Fluka Chemika. DBU as a metal-free catalyst was purchased from
Aldrich and distilled over barium oxide before use. Chloroform was
dried using a MBRAUN Solvent Purification System (model MB-SPS 800)
equipped with alumina drying columns. Heptane was purchased from VWR
used as received. Acetic acid was purchased from ChemLab. 1-Methylimidazole
(99%, Merck) and 11-bromoundecanol (Aldrich, 98%) were used as received.
A commercially available extrusion-grade PLA (NatureWorks 4032D) designed
especially for the production of biaxially oriented films was used
as received (Mn = 133 500 ±
5000 g·mol–1, = 1.94
± 0.06 as determined from SEC, and 1.4 ± 0.2% d-isomer content as determined by the supplier).
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9

Bovine Progesterone Enzyme Immunoassay Protocol

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All chemicals were of analytical reagent grade. Progesterone (P4) and buffer reagents were supplied by Sigma-Aldrich (Belgium), unless stated otherwise. Solutions were prepared with deionized water purified by a Milli-Q Plus system (Millipore, Marlborough, MA, USA). Acetic acid, hydrochloric acid and sodium hydroxide were purchased from Chem-Lab (Belgium). Sodium chloride, 1ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) and Nhydroxysuccinimide (NHS) were supplied by Fischer Scientific (Belgium) and Tween-20 by Applichem (Germany). Progesterone-BSA conjugate (P4-BSA) and mouse anti-progesterone antibody (anti-P4 Ab) were purchased from AbD Serotec (UK). Goat antimouse antibody (GAM Ab) was supplied by Life Technologies (Belgium). Au NPs (ø 20 nm) were produced by BBI Solutions (UK) and carboxylic acid-SAM formation reagent was purchased from Dojindo (Japan). The milk progesterone enzyme-immunoassay (Mkit Elisa) and ELISA milk standards were purchased from Ridgeway Science (UK). A milk sample was collected for 6 cow (numbered Cow 1e6) selected from a 50 headed herd on an experimental farm (Hooibeekhoeve, Geel) in Flanders, Belgium. These samples were taken from cows in heat.
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10

Enzymatic Hydrolysis of Cellulose and Pectin

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Pectinase from Aspergillus aculeatus (Pectinex® Ultra Clear, a blend of pectinases, hemicellulases and arabinases with activity of 8600 PGNU/g) and (Pectinex® Ultra SP-L, a blend of pectinases, hemicellulases and beta-glucanases with activity of 3300 PGNU/g), cellulase from Trichoderma reesei (Celluclast® 1.5L, a cellulase aqueous solution with activity of ≥700 units/g) were obtained from Sigma Aldrich (Darmstadt, Germany). Information about the optimal conditions of these enzymes as declared by the producer can be found in Table 1. Microcrystalline cellulose Avicel® PH-101, pectin from citrus peel, 3,5-dinitro salicylic acid, D-(+)-galacturonic acid monohydrate and D-(+)-glucose were purchased from Sigma Aldrich (Darmstadt, Germany). Sodium carbonate anhydrous, citric acid, sodium hydroxide, and L (+)-potassium sodium tartrate tetrahydrate were purchased from VWR Chemicals (Leuven, Belgium), while di-sodium hydrogen phosphate anhydrous, sodium acetate trihydrate, and acetic acid 99–100 % were obtained from Chem-Lab (Zedelgem, Belgium).

Conditions range of activity of the used enzymes as declared by the producer.

EnzymepH range of activityTemperature range of activity
Pectinex® Ultra Clear1.8–3.025–40 °C
Pectinex® Ultra SP-L2.8–6.515–55 °C
Celluclast® 1.5L4.0–6.050–60 °C
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