An experiment was carried out to establish an accurate method for the determination of microamounts of phosphorus in high alloy steels such as heat resisting steels and alloys containing large amounts of niobium, tantalum, titanium and other elements.
The phosphorus was separated from the various elements by coprecipitating it with beryllium hydroxide in an ammoniacal solution containing EDTA and the coprecipitated niobium, tantalum and other elements with beryllium hydroxide and phosphorus were separated from the phosphorus by extracting as cupferrates with
n-bthylalcohol-chloroform mixture in a sulfuric acid solution containing hydrofluoric acid. By using jointly these separation techniques, microamounts of phosphorus could be separated accurately from large amounts of chromium, cobalt, iron, molybdenum, nickel, niobium, tantalum, titanium, tungsten, vanadium, zirconium and other elements.
The separated phosphorus was determined by the spectrophotometric method with molybdenum blue. In this method, the phosphorus was extracted as phosphomolybdic acid with
n-bthylalcohol-chloroform mixture in 1.2 N sulfuric acid solution and back extracted as molybdenum blue into 10 mL or 20 mL of a reducing solution containing 1 g of stannous chloride per 100 mL of 0.6 N hydrochloric acid, and the absorbance of the obtained molybdenum blue was measured at a wavelength of 945 nm.
As a result of the experiment, the author succeeded in establishing a method in which 0.0005 to 0.02% of phosphorus in high alloy steels such as heat resisting steels and alloys containing large amounts of niobium, tantalum, titanium and other elements can precisely be measured.
The phosphorus contents in synthetic and actual samples were measured by this method with satisfactory results.
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