Cobalt blue molybdate

Modras (51) reported spot test reactions to differentiate hydralazine from closely related drugs. Reagents used were aqueous copper (I) chloride, aqueous ammonium molybdate, iodine in potassium iodide solution, aqueous cobalt (II) nitrate, alcoholic ninhydrin, and alcoholic bromophenol blue. The tests were performed on paper or on Silica Gel G. 

Synthesis of phthalocyanine-2,9,16,23-tetracarboxylic acid cobalt(II) complex 48 (R = -COOH M = Co(II)) 0.26 g (2 mmol) water-free cobalt chloride, 1.54 g (8 mmol) 1,2,4-benzenetricarboxylic acid anhydride, 4.8 g (80 mmol) urea and around 20 mg ammonium molybdate are intensively mixed and heated under inert gas in a 100-mL glass vessel at 270 °C for 1 h. The blue-colored reaction mixture was pulverized, stirred in 400 mL 6 M aqueous HCl, filtered, intensively washed with 6 M HCl and then water and acetone. The product was treated in a Soxhlet apparatus with acetone and dried. The phthalocyanine tetracarboxylic acid amide obtained was saponified to the tetracarboxylic acid as follows. 1 g of the tetracarboxylic acid amide was heated in a mixture of 6 g KCl and 15 mL 2 M aqueous KOH at 90 °C until the ammonia evolution became weak. The filtered product was dissolved in a fairly small amount of 2 M NaOH and after filtration from byproducts separated with 2 M HCl and isolated by centrifugation. Purification was achieved by dissolving in 0.05 M NaOH, separation with 2 M HCl and centrifugation until the filtrate is free of chloride ions. Yield from 1 g tetracarboxylic acid amide 0.56 g (38%). IR (KBr) 1698, 1373, 1326, 1150, 1091, 743 cm . 

It can also be detected with diphenylcarbazide or diphenylcarbazone, which yields a blue-violet color in acidic medium, even in 0.2mol/L nitric acid. The diphenylcarbazone/Hg + complex is extractible into benzene. Copper, iron, and cobalt are not disturbing in 0.2mol/L nitric acid. However, Cr04 , Cr207 , and molybdic anions are. 

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