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Acetonitrile d3

Manufactured by Merck Group
Sourced in United States, Belgium, Germany

Acetonitrile-d3 is a deuterated solvent commonly used in nuclear magnetic resonance (NMR) spectroscopy. It is a clear, colorless liquid with a high purity level. Acetonitrile-d3 is often employed as a reference standard and solvent in the analysis of organic compounds using NMR techniques.

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13 protocols using acetonitrile d3

1

Trace Element Analysis Protocol

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CoCl2·6H2O (analytical grade), Co(NO3)2·6H2O (99%), ethylene glycol (99.9%), p-cymene
(99%), nitric acid (70%), tetraethylammonium chloride (98%), tetraethylammonium
nitrate (99%), and tetraethylammonium hydrogen sulfate (99%) were
purchased from Acros Organics (Geel, Belgium). Co, Sm, and Ga standard
solutions (1000 ± 10 mg L–1) were purchased
from Chem-Lab (Zedelgem, Belgium). Acetonitrile-d3 (99.9%), Triton X-100 (for molecular biology), and 1-ethyl-3-methylimidazolium
chloride (>95%) were obtained from Sigma-Aldrich (Diegem, Belgium).
Cyanex 923 was purchased from Solvay (Vlaardingen, Netherlands). Isopropanol
(analytical reagent) and LiCl (analytical reagent grade) were supplied
by Fisher Scientific (Merelbeke, Belgium). SmCl3·6H2O (99.9%) was ordered from Strem Chemicals (Newburyport, MA).
A silicone solution in Isopropanol for the treatment of the TXRF quartz
glass carriers was obtained from SERVA Electrophoresis GmbH (Heidelberg,
Germany). Choline chloride (98%) was purchased from J&K Scientific
(Pforzheim, Germany). 1-Butyl-1-methylpyrrolidinium chloride (99%)
was obtained from IoLiTec (Heilbronn, Germany). Tetraethylammonium
bromide (99%) was ordered from J. T. Baker Chemicals (Deventer, Netherlands).
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2

Oligonucleotide Annealing Protocol

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8-MOP and 5-MOP were purchased from TCI (Tokyo, Japan, >98%) and TMP from Sigma-Aldrich (Steinheim, Germany, ≥98%). The lyophilized oligonucleotide 5′-(TA)20-3′ was purchased from Sigma-Aldrich. The manufacturer purified the sample by HPLC. Annealing of the oligonucleotide strands in solution was performed within 24 h before the measurements by heating the solution in a water bath up to 93 °C and letting it cool down to room temperature within several hours. Solvents used were pure water (Fisher Chemical, Loughborough, UK, HPLC gradient grade), deuterium oxide (Deutero GmbH, Kastellaun, Germany, 99.9% D) and acetonitrile-d3 (Sigma-Aldrich, ≥99.8% D). Solutions of the oligonucleotides were buffered with PBS (Sigma Aldrich, one tablet dissolved in 200 mL yielded 10 mM phosphate buffer, 2.7 mM potassium chloride, 137 mM sodium chloride, pH 7.4 at 25 °C).
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3

Deuterated Solvents Preparation

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Commercially available deuterated benzene-d6 (ACROS organics), methanol-d3, dimethyl sulfoxide-d6, acetonitrile-d3, deuterium oxide (Sigma-Aldrich), toluene, xylene, and chlorobenzene (Kanto Kagaku) were used without further purification.
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4

Ruthenium(II) Complexes Synthesis and Characterization

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All materials were used as received without further purification unless otherwise noted. Diethyl ether, acetone, acetonitrile, and methanol were procured from Fisher Scientific, and dichloromethane was obtained from Macron Fine Chemicals. N,N-Dimethylformamide was purchased from Sigma-Aldrich and was dried under nitrogen by passing through a column of activated alumina. Reineke salt, ammonium hexafluorophosphate, lithium chloride, sodium chloride, sodium acetate trihydrate, ascorbic acid, 1,3-diphenylisobenzofuran (DPBF), acetylacetonate, 1,10-phenanthroline, 4,4′-dimethylbipyridyl, acetonitrile-d3 and acetone-d6 were purchased from Sigma-Aldrich, and 2,2′-bipyridine was obtained from Alfa Aesar. Sulfuric acid and sodium bicarbonate were received from Fisher Scientific, and potassium ferrioxalate was purchased from Strem Chemicals. Neutral alumina was purchased from Fisher Scientific. The starting material [Ru(p-cymene)Cl2]2,21 (link) and the complexes [Ru(p-cymene)(bpy)Cl]Cl, [Ru(p-cymene)(4,4′-Me2bpy)Cl]Cl, [Ru(p-cymene)(phen)Cl]Cl, and Ru(p-cymene)(acac)Cl were synthesized according to published procedures.21b
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5

NMR Measurements with Deuterated Solvents

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For all NMR measurements, we used deuterated solvents from Sigma Aldrich: Chloroform-d (99.8 atom % D), Methanol-d4 (99.8 atom % D) and Acetonitrile-d3 (99.8 atom % D).
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6

Synthesis and Characterization of Ethylammonium Nitrate

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Ethylamine (70 wt% in water), ethanol (analytical reagent) and dimethyl sulfoxide (analytical reagent) were purchased from Fisher Scientific (Merelbeke, Belgium); nitric acid (65%), tri‐n‐butyl phosphate (>99%), formamide (99%), Co(NO3)2·6H2O (99%) and gallium standard solution (1,000 ± 10 mg·L−1) were supplied by Chem‐lab (Zedelgem, Belgium); n‐decane (99%), ethylene glycol (99.5%) and Ni(NO3)2·6H2O (99%) were obtained from Acros Organics (Geel, Belgium); LiNO3 (99%), Mn(NO3)2·4H2O (>97%), Zn(NO3)2·6H2O (99%), Triton™ X‐100 (for molecular biology), CDCl3 (99.8%) and acetonitrile‐d3 (99.9%) were obtained from Sigma‐Aldrich (Diegem, Belgium); Fe(NO3)3·9H2O (99%) was provided by VWR Chemicals (Leuven, Belgium); Cu(NO3)2·6H2O (99.5%) was purchased from BDH Chemicals (Poole, UK). Milli‐Q water (18.2 MΩ∙cm at 25°C) was used to prepare the aqueous solutions. Ethylammonium nitrate was prepared from ethylamine and nitric acid by a simple acid‐base reaction27 and dried on a Schlenk line to a final water content of <0.5 wt%. Drying of protic ionic liquids with nitrate ions, such as EAN, has to be done very carefully.28
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7

Characterization of Synthetic Compounds

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Compound 1 (98%) was supplied by Aldrich Chemical Company whereas 2 (99%) and 3 (99%) by Sigma-Aldrich. Acetonitrile (ACN, HPLC 99.5%) and ethanol (99.8%) were provided by Sintorgan and Merck, respectively. Water was purified using a reverse osmosis RIOS 5 and Synergy (Millipore) (resistivity 18.2 MΩcm, DOC <0.1 mg L−1). Acetone-d6 and acetonitrile-d3 were used to obtain the NMR spectra, both provided by Sigma-Aldrich. All solvents and chemicals were used as received without further purification.
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8

Solvent and Reagent Acquisition for Analytical Chemistry

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Dichloromethane, ethyl acetate, n-butanol, n-hexane, acetone, acetonitrile, acetonitrile far UV and methanol (all HPLC grade) were purchased from Fisher Scientific (Leicestershire, UK).
All reagents, such as sulphuric acid and formic acid (eluent additive for HPLC) were purchased from Acros Organics (Geel, Belgium) or Sigma-Aldrich (St. Louis, MO, USA). acetonitrile and formic acid (both for UPLC-MS) were obtained from Biosolve Chimie (Dieuze, France).
Ultrapure water was obtained using a Milli-Q system from Millipore (Bedford, MA, USA).
NMR deuterated solvents (CDCl3, acetonitrile-d3, methanol-d4, DMSO-d6, pyridine-d5) were obtained from Sigma-Aldrich.
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9

Antioxidant Compounds Characterization

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Acetic acid was purchased from Carl Roth GmbH + Co., KG (Karlsruhe, Germany). Acetonitrile, ethyl acetate, and methanol were purchased from VWR International GmbH (Darmstadt, Germany). Acetonitrile-d3, 2,2′-azinobis(3-ethylbenzothiazoline-6-suflonate), caffeic acid, chlorogenic acid, and potassium persulfate were purchased from Sigma-Aldrich Chemie GmbH (Steinheim, Germany). Ferulic acid, hydrocaffeic acid, and para-coumaric acid were purchased from Fluka Chemicals Ltd. (Wales, UK). Potassium dihydrogen phosphate and potassium hydrogen phosphate were purchased from Merck KGaA (Darmstadt, Germany).
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10

Electrochemical Conversion of Biomass Derivatives

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Sodium bicarbonate, sodium carbonate, and DMF were obtained from Alfa Aesar. HMF, 5‐MF, DMTHF, DHMTHF, sulfuric acid, benzyl alcohol, acetonitrile (HPLC gradient grade), and acetonitrile‐d3 (≥99.8 at.% D) were purchased from Sigma Aldrich. DHMF was obtained from Cayman Chemical and MFA from Acros Organics. All solutions were prepared using ultrapure (18 MΩ cm) water from a Milli‐Q IQ 7000 system (Merck). GC plates were obtained from HTW Germany. BDD electrodes were purchased from Condias and details on the material characteristics can be found in the work by Hutton et al.[24] Graphite foil was purchased from Alfa Aesar and Ir mixed metal oxide (MMO) plates as counter electrodes were obtained from Metakem.
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