This experiment was conducted to establish a simple and accurate method for determination of the zirconium content in a steel containing tungsten. First of all, the fundamental condition for the spectro-photometric determination of zirconium with xylenol orange was studied.
Next, the condition for the separation of zirconium from tungsten by cupferron was examined, and the procedure was decided.
The absorption maximum of the xylenol orange complex salt of zirconium is at 545∼550 milli microns. However, the relation between the zirconium content (0.00∼0.30 mg/100 mL) and the absorbance follows Beer’s law only at the wave-length of 532 milli microns. Therefore, in this experiment, the absorbance was measured at 532 milli microns. Hydrochloric, nitric and perchloric acids do not interfere with the formation of the xylenol orange complex salt of zirconium, if these acids are neutralized with ammonium hydroxide. In this method, there is no significant effect even in case 200 mg of iron, 15 mg each of manganese and molybdenum, 50 mg each of nickel and chromium, 5 mg each of copper and titanium, 0.25 mg of tungsten, 20 mg each of vanadium and cobalt, 80 mg of aluminum, and 2 mg of selenium are contained in the separated sample solution. Niobium interferes.
The complex salt of zirconium cupferrate is formed quantitatively in a solution of pH 5.0∼7.5 containing tartaric and oxalic acids. Potassium salt interferes with the formation of the complex salt of zirconium cupferrate, but sodium salt does not. Therefore, the oxides of tungsten and zirconium were fused with sodium pyrosulfate. By means of this separation method with cupferron, zirconium can be separated from tungsten easily and accurately.
As a result of the experiment, the author succeeded to establish a method by which 0.005 to 1% zirconium in a steel containing tungsten can precisely be measured without difficulty. The zirconium contents in synthetic and actual samples were measured by this method with satisfactory results.
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