By W. T. Elwell
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Extra info for Analysis of the New Metals. Titanium, Zirconium, Hafnium, Niobium, Tantalum, Tungsten and Their Alloys
Dissolve 0-5 g of high-purity copper in 25 ml of nitric acid (1 + 1), boil the solution for 2-3 min to expel oxides of nitrogen, cool, and dilute to 11. Dilute 10 ml of this solution to 500 ml. 2. Preparation of Calibration Graphs Graph 1. For Copper Contents 20-800 ppm. Add, separately, 0-5, 1-0, 2 0 , 3 0 and 4 0 ml of the standard copper solution (1 ml = 001 mg Cu) to each of five 50-ml calibrated flasks. Proceed with each solution (and a blank) as follows: Add 8 0 ml of ammonium citrate solution (20%), one drop of neutralred indicator solution (005 %), and shake the solution.
1. 1. Special Reagen ts Sym-Diphenylcarbazide Solution. This solution must be freshly prepared. Dissolve 0-125 g of the reagent in 50 ml of ethanol (1+1). Standard Chromium Solution. Dissolve 0-5657 g of potassium dichromate (dried at 140-150°C) in water and dilute to 1 1. Dilute 100 ml of this solution to 1 1. 2. Preparation of Calibration Graph (Note) Transfer 40 ml of sulphuric acid ( 1 + 4 ) to each of six conical beakers (250ml) and add, separately, 5 0 , 1 0 0 , 1 5 0 , 2 0 0 and 2 5 0 m l of the standard chromium solution (1 ml = 0 0 2 m g Cr).
Oxidize the solution with a slight excess of cone, nitric acid, added dropwise, boil for 2-3 min to expel oxides of nitrogen, then cool to room temperature. Transfer to a 100-ml calibrated flask and dilute to the mark. Transfer a 10-ml aliquot to a 50-ml calibrated flask, add 5 ml of citric acid solution (50%) and continue as described for preparation of the calibration graphs. Calculate the iron content of the sample, using the appropriate calibration graph. REPRODUCIBILITY: 0005 AT 0 1 % LEVEL Notes.