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8 protocols using concentrated sulfuric acid

1

Cellulose-based Biomaterials Characterization

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Cellulose fiber, microcrystalline cellulose, chitosan (low molecular weight: MW = 50 kDa, deacetylation degree = 75–85%), sodium periodate, diiodomethane (pure for analysis), glycerol, human serum albumin (HSA), bovine serum albumin (BSA), and diclofenac sodium were purchased from Sigma-Aldrich and used without further purification. Acetic acid, sodium hydroxide, concentrated hydrochloric acid (35%), concentrated sulfuric acid (96%), acetone, dimethylformamide (DMF), and phosphate-buffered saline (PBS, pH = 7.4) were purchased from Avantor Performance Materials (Gliwice, Poland). Gelatin was purchased from CHEMPUR (20 mesh pure). Diluent solution 2% NaCl and the bacteria A. fischeri to toxicity assessment were supplied by the producer Microtox.
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2

Electrophoretic Deposition of Functionalized CNTs on Titanium

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Coatings of carbon nanotubes (MWCNT–multi-walled carbon nanotubes, NanoAmor, Houston, TX, USA) ranging from 5–15 nm in diameter and 10–20 μm in length were deposited on titanium substrates. They were functionalized in a 3:1 mixture of concentrated sulfuric acid (Avantor Performance Materials) and concentrated nitric acid (Avantor Performance Materials) to remove metal particles, used as a catalyst during the preparation of nanotubes. Dissociation of the carboxyl groups formed in this way provide a negative charge that is necessary for electrophoretic deposition. A 4%(w/w) suspension of CNT was prepared in a mixture of isopropanol (≥99.5%, Avantor Performance Materials), acetone (≥99.5%, Avantor Performance Materials) and distilled water in a volume ratio of 3:1:1, respectively. The solution was sonicated for 10 min using an ultrasonic cleaner (Sonic-0.5, Polsonic, Warszawa, Poland) and directly used for electrophoretic deposition.
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3

Biopolymer-based Composite Materials

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Corn starch, chitosan (low molecular weight: MW = 50 kDa, deacetylation degree = 75–85%), sodium periodate, diiodomethane (pure for analysis), glycerol, human serum albumin, and acid glycoprotein were purchased from Sigma-Aldrich (St. Louis, MO, USA) and used without further purification. Acetic acid, sodium hydroxide, concentrated hydrochloric acid (35%), concentrated sulfuric acid (96%), acetone, and phosphate-buffered saline (PBS, pH = 7.4) were purchased from Avantor Performance Materials (Gliwice, Poland). Gelatin was purchased from CHEMPUR (Piekary Slaskie, Poland)—20 mesh pure. Diluent solution 2% NaCl and bacteria A. fischeri for toxicity assessment were supplied by the producer of Microtox (Modern Water, Cambridge, UK).
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4

Functionalization of Multi-walled Carbon Nanotubes

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Multi-walled CNT (CNT Co. Ltd., South Korea) with a diameter in the range of 5–20 nm and a length of about 10 µm were chemically oxidized in the 3:1 (v/v) mixture of concentrated sulfuric acid (≥ 95%, Avantor Performance Materials, Poland) and concentrated nitric acid (35–38%, Avantor Performance Materials, Poland). For this, they were treated in the solution under a reflux condenser for 4 h at 70 °C and then washed with distilled water and dried. The process was performed to introduce the negatively charged carboxyl (COO) functional groups into the surface of CNT, as well as carbonyl (C=O) groups and ether (C–O–C) moieties42 (link). Therefore, the resulting negative zeta potential made possible to conduct their electrophoretic deposition (EPD) on the substrate as an anode. Furthermore, the remnants of metallic catalysts from the CNT synthesis could been removed during the process.
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5

Peptide Fragmentation Analysis via TEP Labeling

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A variety of peptides, either commercially available, synthesized or from protein digests, were labeled with the TEP charge tag to investigate the effects that sequence composition have on fragmentation. Angiotensin I (DRVYIHPFHL), bradykinin 2–9 (PPGFSPFR), bradykinin 1–8 (RPPGFSPF), Glu-fibrinopeptide B (EGVNDNEEGFFSAR), hemoglobin, trypsin, α-cyano-4-hydroxycinnamic acid (CHCA), chloroacetonitrile, ethanethiol, N-hydroxysuccinimide, N,N′-dicyclohexylcarbodiimide, triethylphosphine, and iodoacetamide were purchased from Sigma (St. Louis, MO, USA). Other peptides included in this work were synthesized in-house. The monoclonal antibody, Rituximab, was provided by Genentech (South San Francisco, CA, USA). Concentrated sulfuric acid was obtained from Avantor Performance Materials (Center Valley, CA, USA) and p-dioxane was from JT Baker (Phillipsburg, NJ, USA). Sodium chloride, anhydrous diethyl ether, and dichloromethane were from VWR Analytical (Radnor, PA, USA). Bromoacetic acid was acquired from Acros Organics (Morris Plains, NJ, USA) and toluene was purchased from Mallinckrodt Chemicals (Phillipsburg, NJ, USA). Dithiothreitol was from Bio-Rad (Hercules, CA, USA).
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6

Phosphorene Production and Membrane Fabrication

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To produce few-layered phosphorene, bulk black phosphorus was purchased from Smart Elements, Vienna, Austria. Polysulfone (PSf), poly ether ether ketone (PEEK), N-methyl pyrrolidone (NMP), used to prepare the dope solution for ultrafiltration membranes, were purchased from VWR, Radnor, PA, USA. Methylene blue was purchased from VWR, Radnor, PA, USA. Sodium hydroxide (NaOH), bovine serum albumin (BSA), sodium chloride (NaCl), concentrated sulfuric acid, phenolphthalein indicator and citric acid were also purchased from VWR, Radnor, PA, USA. The cross flow cell was designed in the laboratory. The ultrasonicator model P70H was purchased from Elmasonic P, Singen, Germany. A dead-end cell, Amicon stirred-cell 8010–50 mL, was purchased from EMD Millipore, Burlington, MA, USA. Total organic carbon analyzer TOC-5000A was purchased from Thermo Scientific, Waltham, MA, USA.
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7

Analytical Grade Chemicals for Research

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All the chemicals used in the present study were of analytical grade purity and were used without any further purification. Nickel sulfate hexahydrate (NiSO4·6H2O, ≥98% pure), cobalt sulfate heptahydrate (CoSO4·7H2O, ≥99% pure), manganese sulfate monohydrate (MnSO4·H2O, ≥99% pure), lithium sulphate monohydrate (LiSO4·H2O, ≥99% pure), potassium permanganate (KMnO4, ≥99% pure), and potassium dichromate (K2Cr2O7, ≥99% pure) were purchased from Sigma Aldrich Canada (Oakville, Canada). Deionized water was produced by the Milli-Q Integral water purification system of MilliporeSigma (Merck KGaA, Darmstadt, Germany). Concentrated orthophosphoric acid (H3PO4, 85.0 wt%) and concentrated sulfuric acid (H2SO4, 95.0–98.0 wt%) were supplied by VWR International LLC (Mississauga, Ontario, Canada). Quartz cuvette cells of 10 mm and 2 mm path length (200–2500 nm scan range) with a volume of 1.2 mL (with slits) and 0.7 mL, respectively, were purchased from Lianyungang Highborn Technology Co. Ltd (Lianyungang, Lianyungang Jiangsu Province, China).
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8

Sulfonation of Polysulfone and Phosphorene Synthesis

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Perfluorooctanoic acid (PFOA) was purchased from Sigma Aldrich (St Louis, MO, USA). For the sulfonation reaction, polysulfone (PSf), N-methyl pyrrolidone (NMP), poly ether ether ketone (PEEK), and concentrated sulfuric acid were purchased from VWR (Radnor, PA, USA). Black phosphorus used for the synthesis of phosphorene was purchased from Smart Elements (Vienna, Austria).
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