Ammonium molybdate

Phosphorus. The presence of phosphorus may be indicated by a smell of phosphine during the sodium fusion. Treat 1 ml. of the fusion solution with 3 ml. of eoneentrated nitric acid and boil for one minute. Cool and add an equal volume of ammonium molybdate reagent. Warm the mixture to 40-50°, and allow to stand. If phosphorus is present, a yellow erystalline precipitate of ammonium phosphomolybdate wUl separate. 

It is usually preferable to oxidise the compound directly as follows. Intimately mix 0 02-0 05 g. of the eompound with 3 g. of sodium peroxide and 2 g. of anhydrous sodium carbonate in a niekel erucible. Heat the crueible and its eontents with a small flame, gently at first, afterwards more strongly until the eontents are fused, and eontinue heating for a further 10 minutes. Allow to stand, extract the contents of the crucible with water, and filter. Add exeess of eoneentrated nitrie acid to the filtrate and test with ammonium molybdate reagent as above. A yellow preeipitate indicates the presenee of phosphorus. It must be borne in mind that the above treatment 1 eonvert any arsenie present into arsenate. 

Molybdenum is also recovered as a by-product of copper and tungsten mining operations. The metal is prepared from the powder made by the hydrogen reduction of purified molybdic trioxide or ammonium molybdate. 

Sonnenschein s reagent (alkaloid detection) a nitric acid solution of ammonium molybdate is treated with phosphoric acid. The precipitate so produced is washed and boiled with aqua regia... 

Molybdenum. The commonly used molybdenum materials are sodium molybdate [7631-95-0] ammonium molybdate [12027-67-7] molybdenum trioxide [1313-27-5] molybdenum sulfate [51016-80-9] and frits. Molybdenum is used in smaller amounts than any of the other micronutrients, ranging from a few grams to 3 kg/hm of Mo. 

Chemical products are produced from technical-grade oxide in two very different ways. Molybdenum trioxide can be purified by a sublimation process because molybdenum trioxide has an appreciable vapor pressure above 650°C, a temperature at which most impurities have very low volatiUty. The alternative process uses wet chemical methods in which the molybdenum oxide is dissolved in ammonium hydroxide, leaving the gangue impurities behind. An ammonium molybdate is crystallized from the resulting solution. The ammonium molybdate can be used either directly or thermally decomposed to produce the pure oxide, MoO. ... 

Manufacturing Processes. Ammonium molybdate or molybdenum trioxide is reduced to molybdenum metal powder by hydrogen in a two-stage process. In the first stage, MoO or ammonium molybdate is reduced to molybdenum dioxide, M0O2, at temperatures around 600°C in the... 

In this process, catalysts, such as boric acid, molybdenum oxide, zirconium, and titanium tetrachloride or ammonium molybdate, are used to accelerate the reaction. The synthesis is either carried out in a solvent (aUphatic hydrocarbon, trichlorobenzene, quinoline, pyridine, glycols, or alcohols) at approximately 200°C or without a solvent at 300°C (51,52). 

In an alternative industrial process, resorcinol [108-46-3] is autoclaved with ammonia for 2—6 h at 200—230°C under a pressurized nitrogen atmosphere, 2.2—3.5 MPa (22—35 atm). Diammonium phosphate, ammonium molybdate, ammonium sulfite, or arsenic pentoxide maybe used as a catalyst to give yields of 60—94% with 85—90% selectivity for 3-aminophenol (67,68). A vapor-phase system operating at 320°C using a siUcon dioxide catalyst impregnated with gallium sesquioxide gives a 26—31% conversion of resorcinol with a 96—99% selectivity for 3-aminophenol (69). 

Phosphate. Phosphoms occurs in water primarily as a result of natural weathering, municipal sewage, and agricultural mnoff The most common form in water is the phosphate ion. A sample containing phosphate can react with ammonium molybdate to form molybdophosphoric acid (H2P(Mo202q)4). This compound is reduced with stannous chloride in sulfuric acid to form a colored molybdenum-blue complex, which can be measured colorimetrically. SiUca and arsenic are the chief interferences. 

Silica. The siUca content of natural waters is usually 10 to (5 x lO " ) M. Its presence is considered undesirable for some industrial purposes because of the formation of siUca and siUcate scales. The heteropoly-blue method is used for the measurement of siUca. The sample reacts with ammonium molybdate at pH 1.2, and oxaUc acid is added to reduce any molybdophosphoric acid produced. The yellow molybdosiUcic acid is then reduced with l-amino-2-naphthol-4-sulfoiiic acid and sodium sulfite to heteropoly blue. Color, turbidity, sulfide, and large amounts of iron are possible interferences. A digestion step involving NaHCO can be used to convert any molybdate-unreactive siUca to the reactive form. SiUca can also be deterrnined by atomic... 

AMMO 2.5 EC , cypermetlu-in, 13 Ammonia, 13 Ammonium acetate, 13 Ammonium arsenate, 13 Ammonium benzoate, 13 Ammonium bicarbonate, 13 Ammonium bifluoride, 14 Ammonium bisulfite, 14 Ammonium carbamate, 14 Ammonium carbonate, 14 Ammonium chloride, 14 Ammonium chlorplatmate, 14 Ammonium clu omate, 14 Ammonium citrate, 14 Ammonium diclu omate, 14 Ammonium fluoride, 14 Ammonium fomiate, 15 Ammonium hexafluorosilicate, 15 Ammonium hydroxide, 15 Ammonium metavanadate, 15 Ammonium molybdate, 15 Ammonium nitrate, 15 Ammonium oxalate, 15 Ammonium perfluorooctanoate, 15 Ammonium persulfate, 15 Ammonium phosphate, 15 Ammonium picrate, 16 Ammonium salicylate, 16... 

Ammonium acetate Ammonium adipate Ammonium benzoate Ammonium bicarbonate Ammonium biflluoride Ammonium binoxalate Ammonium bisulfate Ammonium bitartrate Ammonium tetraborate Ammonium bromide Ammonium carbonate Ammonium chloride Ammonium citrate Ammonium diclnomate Ammonium fluoride Ammonium fluorosilicate Ammonium gluconate Ammonium iodide Ammonium molybdate Ammonium nitrate Ammonium oxalate Ammonium perchlorate Ammonium picrate Ammonium polysulfide Ammonium salicylate Ammonium stearate Ammonium sulfate Ammonium sulfide (hydrosulfide) Ammonium tartrate Ammonium tliiocyanate Ammonium thiosulfate... 

On Merck Silica G using benzene as the solvent and 5% ammonium molybdate in 10% sulfuric acid followed by brief heating at 150° to develop the spots. Under these conditions... 

Discussion. When a solution of an orthophosphate is treated with a large excess of ammonium molybdate solution in the presence of nitric acid at a temperature of 20-45 °C, a precipitate is obtained, which after washing is converted into ammonium molybdophosphate with the composition (NH4)3[P04,12Mo03]. This may be titrated with standard sodium hydroxide solution using phenolph-thalein as indicator, but the end point is rather poor due to the liberation of ammonia. If, however, the ammonium molybdate is replaced by a reagent containing sodium molybdate and quinoline, then quinoline molybdophosphate is precipitated which can be isolated and titrated with standard sodium hydroxide ... 

Procedure. Weigh out accurately about 2.5 g ammonium molybdate... 

The reaction velocity is comparatively slow, but increases with increasing concentration of acid. The addition of three drops of a neutral 20 per cent ammonium molybdate solution renders the reaction almost instantaneous, but as it also accelerates the atmospheric oxidation of the hydriodic acid, the titration is best conducted in an inert atmosphere (nitrogen or carbon dioxide). 

Better results are obtained by transferring 25.0 mL of the diluted hydrogen peroxide solution to a conical flask, and adding 100 mL 1M(1 20) sulphuric acid. Pass a slow stream of carbon dioxide or nitrogen through the flask, add 10 mL of 10 per cent potassium iodide solution, followed by three drops of 3 per cent ammonium molybdate solution. Titrate the liberated iodine immediately with standard 0.1M sodium thiosulphate in the usual way. 

Determination of phosphate as ammonium molybdophosphate. This may be readily effected by precipitation with excess of ammonium molybdate in warm nitric acid solution arsenic, vanadium, titanium, zirconium, silica and excessive amounts of ammonium salts interfere. The yellow precipitate obtained may be weighed as either ammonium molybdophosphate, (NH4)3[PMo12O40], after drying at 200-400 °C, or as P205,24Mo03, after heating at 800-825 °C for about 30 minutes. 

Note. Prepare the ammonium molybdate reagent as follows. Dissolve 125 g ammonium nitrate in 125 mL water in a flask and add 175 mL nitric acid, sp. gr. 1.42. Dissolve 12.5 g ammonium molybdate in 75 mL of water and add this slowly and with constant shaking to the nitrate solution. Dilute to 500 mL with water, heat the flask in a water bath at... 

This process is to ensure that the silica is in the correct form for reaction with ammonium molybdate. If the solution is too hot, the red colour may not develop. 

Prepare the 10 per cent ammonium molybdate solution by dissolving 25 g ammonium molybdate in water and diluting to 250 mL in a polythene bottle. It keeps for about 4 weeks. 

Molybdenum blue method. When arsenic, as arsenate, is treated with ammonium molybdate solution and the resulting heteropolymolybdoarsenate (arseno-molybdate) is reduced with hydrazinium sulphate or with tin(II) chloride, a blue soluble complex molybdenum blue is formed. The constitution is uncertain, but it is evident that the molybdenum is present in a lower oxidation state. The stable blue colour has a maximum absorption at about 840 nm and shows no appreciable change in 24 hours. Various techniques for carrying out the determination are available, but only one can be given here. Phosphate reacts in the same manner as arsenate (and with about the same sensitivity) and must be absent. 

Ammonium molybdate-hydrazinium sulphate reagent. Solution (a) dissolve 1.0 g ammonium molybdate in 10 mL water and add 90 mL of 3M sulphuric acid. Solution (b) dissolve 0.15 g pure hydrazinium sulphate in 100 mL water. Mix 10.0 mL each of solutions (a) and (b) just before use. 

Rapidly add 2.0 g of zinc to the vessel A, immediately insert the stopper, and allow the gases to bubble through the solution for 30 minutes. At the end of this time the solution in D should still contain some iodine. Disconnect the delivery tube C and leave it in the absorption tube. Add 5.0 mL of the ammonium molybdate-hydrazine reagent and a drop or two of sodium disulphite solution. Heat the resulting colourless solution in a water bath at 95-100 °C, cool, transfer to a lOmL graduated flask, and make up to volume with water. 

B. Phosphovanadomolybdate method Discussion. This second method is considered to be slightly less sensitive than the previous molybdenum blue method, but it has been particularly useful for phosphorus determinations carried out by means of the Schoniger oxygen flask method (Section 3.31). The phosphovanadomolybdate complex formed between the phosphate, ammonium vanadate, and ammonium molybdate is bright yellow in colour and its absorbance can be measured between 460 and 480 nm. 

Ammonium molybdate solution. Dissolve 50 g ammonium molybdate, (NH4)6 Mo7024,4H20, in warm water and dilute to 1 L in a graduated flask. Filter the solution before use. 

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