By W. T. Elwell

ISBN-10: 0080118038

ISBN-13: 9780080118031

E-book by means of Elwell, W T wooden, D F

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Additional resources for Analysis of the New Metals. Titanium, Zirconium, Hafnium, Niobium, Tantalum, Tungsten and Their Alloys

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1 is a direct method based on the reaction of cupric ions with biscyclohexanone oxalyldihydrazone in alkaline solution, to form a blue-coloured c o m p e x . This method is primarily intended for the examination of samples containing between 50 p p m and about 3 % of copper. Biscyclohexanone oxalyldihydrazone was first suggested as an analytical reagent by N i l s s o n , and was later applied to the quantitative determination of copper by Wetlesen and G r a n . The complex is not formed in acid solution; in strongly alkaline solution the colour fades rapidly.

Record the burette reading at the end-point and calculate the chlorine content of the sample. 6. Procedure for Chlorine Contents Below 50 ppm Remove any extraneous chloride by heating the sample turnings (or drillings) in boiling water for a few minutes. Cool and rinse the turnings with acetone, then dry. Transfer 1 g of the cleaned sample to a conical flask (50 ml) fitted with an air condenser, add 20 ml of sulphuric acid (1 +4) and 10 ml of fluoroboric acid; warm gently to assist solution. Oxidize with a slight excess of cone, nitric acid, added dropwise, heat the solution just to its boiling-point, then cool.

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.

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Analysis of the New Metals. Titanium, Zirconium, Hafnium, Niobium, Tantalum, Tungsten and Their Alloys by W. T. Elwell


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