Lead ferricyanide nitrate

Lead ferricyanide nitrate, Pb3[Fe(CN)6]2.Pb(N03)2.12H20, and Lead potassium ferricyanide, PbK[Fe(CN)6].3H20, have been described.3... 

Lead ferricyanide, Pb3[Fe(CN)6]2.16H20, is obtained by double decomposition of lead nitrate with potassium ferricyanide. It yields dark reddish brown crystals. 

A weighed amount of sample is dissolved in a mixture of propanone and ethanoic acid and titrated potentiometrically with standard lead nitrate solution, using glass and platinum electrodes in combination with a ferro-ferricyanide redox indicator system consisting of 1 mg lead ferrocyanide and 0.5 ml 10% potassium ferricyanide solution. The endpoint of the titration is located by graphical extrapolation of two branches of the titration plot. A standard solution of sodium sulfate is titrated in the same way and the sodium sulfate content is calculated from the amounts of titrant used for sample and standard. (d) Water. Two methods are currently available for the determination of water. 

Marchand and co-workers reported a synthetic route to TNAZ (18) involving a novel electrophilic addition of NO+ NO2 across the highly strained C(3)-N bond of 3-(bromomethyl)-l-azabicyclo[1.1.0]butane (21), the latter prepared as a nonisolatable intermediate from the reaction of the bromide salt of tris(bromomethyl)methylamine (20) with aqueous sodium hydroxide under reduced pressure. The product of this reaction, A-nitroso-3-bromomethyl-3-nitroazetidine (22), is formed in 10% yield but is also accompanied by A-nitroso-3-bromomethyl-3-hydroxyazetidine as a by-product. Isolation of (22) from this mixture, followed by treatment with a solution of nitric acid in trifluoroacetic anhydride, leads to nitrolysis of the ferf-butyl group and yields (23). Treatment of (23) with sodium bicarbonate and sodium iodide in DMSO leads to hydrolysis of the bromomethyl group and the formation of (24). The synthesis of TNAZ (18) is completed by deformylation of (24), followed by oxidative nitration, both processes achieved in one pot with an alkaline solution of sodium nitrite, potassium ferricyanide and sodium persulfate. This route to TNAZ gives a low overall yield and is not suitable for large scale manufacture. 

With certain compounds, such as pyrazoline carboxylic acids and esters, potassium ferricyanide or silver nitrate has been used,509 and for those compounds unsubstituted on nitrogen, mercuric oxide or acetate.76 Lead dioxide has been successful for the oxidation of 1-alkyl-and 1-arylpyrazolines,9i 76,83 and in certain instances even chromic acid, but not hydrogen peroxide or silver oxide.76 See also L. Smith521 and Birkinshaw et al.b22... 

Ferricyanide Dissolve about 10 mg of sample in 10 mL of water, and place 1 drop of this solution on a spot plate. Add 1 drop of a 1% solution of lead nitrate followed by a few drops of a solution prepared by saturating cold 2 A acetic acid with benzidine. No blue precipitate or blue color appears. Free Moisture Heat 20 g of sample at 105° for 6 h, cool in a desiccator, and weigh. Grind the dried sample rapidly, heat 3 g of the powder to constant weight at 105°, and calculate the total water content (W). Calculate the percent free moisture in the sample by the formula... 

Potassium permanganate. Dimethyl sulfide-Chlorine. Dimethyl sulfoxide. Dimethyl sulfoxide-Chlorine. Dimethylsulf-oxide Sulfur trioxide. Dipyridine chro-mium(VI) oxide. Iodine. Iodine-Potassium iodide. Iodine tris(trifluoroacetate). Iodosobenzene diacetate. Isoamyl nitrite. Lead tetraacetate. Manganese dioxide. Mercuric acetate. Mercuric oxide. Osmium tetroxide—Potassium chlorate. Ozone. Periodic acid. Pertrifluoroacetic acid. Potassium ferrate. Potassium ferricyanide. Potassium nitrosodisulfonate. Ruthenium tetroxide. Selenium dioxide. Silver carbonate. Silver carbonate-Celite. Silver nitrate. Silver oxide. Silver(II) oxide. Sodium hypochlorite. Sulfur trioxide. Thalli-um(III) nitrate. Thallium sulfate. Thalli-um(III) trifluoroacetate. Triphenyl phosphite ozonide. Triphenylphosphine dibromide. Trityl fluoroborate. 

Procedure. A drop of the neutral test solution (if necessary, treated with a drop of 1 % lead nitrate solution) is mixed on a spot plate with benzidine acetate solution. A blue precipitate or coloration appears, depending on the ferricyanide content. 

DEKTAL DEVELOPER KODAK FIXER KODAK SHORT STOP POTASSIUM ALUM POTASSIUM BICARBONATE POTASSIUM BICHROMATE POTASSIUM BORATE POTASSIUM BROMATE POTASSIUM BROMIDE POTASSIUM CARBONATE POTASSIUM CHROMATE POTASSIUM CHLORATE POTASSIUM CHLORIDE POTASSIUM CYANIDE POTASSIUM DICHROMATE POTASSIUM FERRICYANIDE POTASSIUM FERROCYANIDE POTASSIUM FLUORIDE POTASSIUM HYDROXIDE POTASSIUM NITRATE POTASSIUM PERBORATE POTASSIUM PERCHLORATE POTASSIUM PERMANGANATE. 10% POTASSIUM SULFATE PROPANE PROPANE GAS PLATING SOLUTIONS BRASS CADMIUM COPPER GOLD INDIUM LEAD NICKEL RHODIUM SILVER TIN ZINC... 

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