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10 protocols using concentrated hydrochloric acid

1

Synthesis of Lithium-Ion Battery Materials

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p-Toluenesulfonyl
chloride (97%), p-toluenesulfonyl amide (97%), lithium
hydroxide monohydrate, potassium permanganate, calcium chloride, N-methyl-2-pyrrolidone (NMP, anhydrous, 99.8%), pyridine
(anhydrous, 99.8%), lithium aluminum hydride (95%), tetrahydrofuran
(THF, anhydrous, 99.8%), lithium bis(trimethylsilyl) amide solution
(1 M in THF), tributyl phosphate (≥99%), and titanium(IV) isopropoxide
(97%) were purchased from Sigma-Aldrich. Aluminum nitrate (Al(NO3)3 × 9H2O), 3-(aminopropyl)triethoxysilane,
1-propanol, and propionic acid were acquired from Merck. 4,4-(Hexa-fluoroisopropylidene)dianiline
(98%) was obtained from TCI Europe, poly(vinylidene difluoride-co-hexafluoropropylene)
(PVdF-HFP, Kynar FLEX LBG) from Arkema, and lithium
nitrate (LiNO3 × xH2O)
from Alfa Aesar. Concentrated hydrochloric acid, methanol, dimethyl
sulfoxide (DMSO), and triphenyl phosphite were acquired from VWR.
Ethylene carbonate, propylene carbonate, and NMC622 were purchased
from BASF. Carbon black (Super C65) was obtained from Imerys Graphite
& Carbon and polyvinylidene difluoride (PVdF, Solef 5130) from
Solvay. Prior to use, calcium chloride was dried at 180 °C under
reduced pressure (10–3 mbar) for 48 h.
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2

Electrochemical Analysis of Vanilloids

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All aqueous solutions were prepared with ultrapure water (0.055 μS cm−1). Vanillin (Sigma Aldrich, reagent plus, 99%), vanillyl alcohol (Sigma Aldrich, supelco, ≥99%), vanillic acid (Sigma Aldrich, purum, ≥98%), sodium hydroxide (Carl Roth, p.a., ≥98%), 1 M hydrochloric acid (Carl Roth, standard solution/p.a.), concentrated hydrochloric acid (VWR Chemicals, supelco), methanol (Carl Roth, LC-MS grade), ethanol absolute (VWR Chemicals, LC-MS grade), acetic acid (Carl Roth, Ph. Eur., 100%), H2O2 solution (Sigma Aldrich, Supelco, ≥30%), horseradish peroxidase (Sigma Aldrich, Type I, ≥50 units per mg), acetonitrile (Sigma Aldrich, HPLC grade), ortho-phosphoric acid (Carl Roth, Ph. Eur., 85%), DMSO-d6 (Sigma Aldrich, 99.9 atom% D), pyridine-d5 (Sigma Aldrich, for NMR spectroscopy, min. 99.8% D), CDCl3 (Sigma Aldrich, for NMR spectroscopy, min. 99.9% D), 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane also called Cl-TMDP (Sigma Aldrich, 95%, for in situ labelling in 31P-NMR-analysis), cyclohexanol (Sigma Aldrich, 99%, internal standard) were used as received for all experiments. As electrode materials Pb sheets (ChemPur, 99.99%), Zn sheets (ChemPur, 99.99%), glassy carbon (GC – HTW Germany, SIGRADUR®) and Ni-foam (AQUA-TITAN, Germany) were used.
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3

Synthesis of Functionalized Organic Compounds

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(TiCl3)3AlCl3 (76.0–78.5% TiCl3) and acetyl
chloride (98%) were purchased from Alfa Aesar. Dry toluene (99.85%,
extra dry, AcroSeal), 4-bromoacetophenone (98%), potassium pyrosulfate
(98%), n-BuLi (1.6 M in hexanes), and 2,4,6-trimethylaniline
(97%) were purchased from Acros Organics. Dry THF (≥99.9%,
with 250 ppm of butylated hydroxytoluene (BHT) as an inhibitor), aluminum
chloride (99.9%), and 2-aminoterephthalic acid (99%) were purchased
from Sigma-Aldrich. DMF (HiPerSolv, CHROMANORM), dichloromethane (DCM)
(HiPerSolv, CHROMANORM), sulfuric acid (96%), chloroform (HiPerSolv,
CHROMANORM), concentrated hydrochloric acid (37%), glacial acetic
acid (ACS reagent grade), and ethanol (technical grade) were purchased
from VWR. The acetone used was of technical grade. Triethylamine (99.7%)
was purchased from Fisher Chemicals. CDCl3, NaOD (40% w/w
in D2O, ≥99.00%), and D2O were purchased
from Eurisotop. Carbon dioxide (Alphagaz 1) was purchased from Air
Liquide. Potassium permanganate crystals were purchased from J.T.
Baker Chemicals N.V. (Holland).
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4

Synthesis of Sodium Fluoride Solution

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Sodium chloride was purchased from Carl Roth (>99.5%, CAS 7647-14-5), sodium fluoride from Merck (99.99%, CAS 7681-49-4), and concentrated hydrochloric acid from VWR (37 w% CAS 7647-01-0). All reagents were used as received without further purification.
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5

Synthesis of Cobalt-based Electrocatalysts

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All manipulations during sample
preparation were carried out in an Ar-filled dry box (content of O2 < 0.5 ppm). A lanthanum rod (≥99.9%), cobalt powder
(99.9%), phosphorus powder (99.9%), tin powder (99.85%), and concentrated
hydrochloric acid (36.5–38.0%) were obtained from VWR. The
lanthanum rod was filed to powder immediately before the reaction.
cobalt powder was additionally purified by heating in a flow of H2 gas at 500 °C for 5 h. Nafion ionomer solution (5% in
aliphatic alcohols and water) and platinum wire (99.9%) were acquired
from Sigma-Aldrich, while the IrO2 (99.99%, #43396) reference
material was purchased from Alfa Aesar. Ultrapure water (18.2 MΩ
cm–2) was produced using a Milli-Q Advantage A10
system (Millipore). For electrolyte preparation, purified NaOH (98.5%)
from Acros Organics and H2SO4 (95–98%)
from Sigma-Aldrich were used.
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6

Polycyclic Aromatic Hydrocarbon Analysis Protocol

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The 8270 MegaMix® standard (see Electronic Supplementary Material (ESM) Table S1 for compound information) was bought from Restek (Bellefonte, PA, USA). Deuterated PAHs (see ESM Table S2 for more information) were obtained from Cambridge Isotope Laboratories (Tewksbury, MA, USA). Sand (Fontainebleau PROLABO®) and 2-propanol (HiPerSolv Chromanorm 100%, PROLABO) were purchased from VWR (Leuven, Belgium), whereas concentrated hydrochloric acid was obtained from VWR, Fontenay-sous-Bois (France). Sodium sulfate, silica gel 60, acetone (≥99.8%), n-hexane (≥98.0%), and cyclohexane were obtained from Merck KGaA (Darmstadt, Germany). DCM (99.99% purity), isooctane (99.94% purity), ethyl acetate (99.96% purity), and methanol (99.99% purity) were purchased from Fisher Scientific (Loughborough, UK). Copper of mesh size 10–40 (≥99.9% purity) and sodium sulfite (≥98%) were acquired from Sigma-Aldrich (St. Louis, MO, USA). TBA hydrogen sulfate was purchased from Molekula (Shaftesbury, UK). Glass fiber filter papers (GFFs) with a diameter of 27 mm were acquired from Dionex (Sunnyvale, CA, USA). An Omnifit glass column (L 50 cm, i.d. 25 mm) from Diba Industries Ltd. (Cambridge, United Kingdom) and SX-3 Bio-Beads from Bio-Rad Laboratories AB (Hercules, CA, USA) were used for GPC.
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7

Characterization of Naturally Occurring Zeolites

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The naturally occurring zeolites used in this study are the same as reported previously18 (link),19 (link) and were obtained from Cuba, San Andrés and Mina San Francisco, San Felipe, Guanajuato in Mexico. The zeolites were used as received from the respective supplier without any further chemical or thermal treatment. The zeolite sample from Mexico was sieved and the fraction below 40 µm was used in this study. This corresponded to the particle size of the Cuban zeolite, which was about 40 µm. The Mexican sample contains 65 wt% HEU (three letter code assigned by the international zeolite association (IZA) for clinoptilolite) 35 wt% of amorphous non-identified material, while the Cuban zeolite consists of 43 wt% HEU, 35 wt% MOR and 22% non-identified materials as described19 (link). As a comparative sample MOR was synthesized following the recipe by Kim et al.35 (link). 5-HT-hc had a purity of 98% and was supplied by Alfa Aesar. Sodium hydroxide pellets and concentrated hydrochloric acid were acquired from VWR Chemicals.
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8

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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9

Ceftazidime Synthesis and Characterization

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Ceftazidime ((6R,7R,Z)-7-(2-(2-aminothiazol-4-yl)-2-(2-carboxypropan-2-yloxyimino)acetamido)-8-oxo-3-(pyridinium-1-ylmethyl)-5-thia-1-aza-bicyclo[4.2.0]oct-2-ene-2-carboxylate) was obtained from Sigma-Aldrich (St. Louis, MO, USA). Carbonate-free 1.0 M NaOH solution was purchased from J.T. Baker (Radnor, PA, USA). Perchloric acid solution from Laborchemie Apolda (Apolda, Germany) was standardized by titrations with NaOH. A standard solution of sodium perchlorate monohydrate (Laborchemie Apolda, Germany) was used to adjust the ionic medium. Argon of high purity (Linde, Dublin, Ireland) was used. Iron(III) chloride was obtained from Sigma-Aldrich, and 1.0 M HCl solution was prepared from concentrated hydrochloric acid (Avantor Performance Materials, Gliwice, Poland). All solutions were prepared in double-distilled water.
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10

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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