Analysis method for phosphor in high temperature alloy

A high-temperature alloy and analysis method technology, applied in the field of analysis and testing, can solve problems such as phosphorus loss, eliminate the influence of high content of interfering elements, and achieve accurate and reliable analysis results.

Inactive Publication Date: 2006-12-20
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, experiments have shown that the hydrolyzate itself can absorb a small amount of phosphorus, and the lower the phosphorus content, the greater the loss of phosphorus
The...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] W is not contained in the sample of embodiment 1

[0016] Weigh 0.3000g sample (reagent blank with the sample) into a 150mL polytetrafluoroethylene beaker, add 4mL nitric acid and 12mL hydrochloric acid, heat to dissolve, add 5mL perchloric acid and heat until perchloric acid fumes are emitted to oxidize chromium To form hexavalent chromium, add hydrochloric acid dropwise to remove chromium, evaporate until the volume of the test solution is less than 1mL, cool slightly, add 5mL nitric acid (1+3), heat to dissolve soluble salts, add 3 drops of sodium nitrite (150g / L) Slightly boil to remove nitrogen oxides, take it off, add solid sodium hydroxide and heat to dissolve until the solution is alkaline, cool, add nitric acid (1+1) dropwise until the pH test paper is neutral. Add 5mL nitric acid (1+1), add 3mL hydrofluoric acid (1+2), heat until the solution is clear and transparent, remove it, add 12mL boric acid (50g / L), mix well, cool to room temperature, transfer the sol...

Embodiment 2

[0017] Containing W in the sample of embodiment 2

[0018] Weigh 0.4000g sample (with the sample as reagent blank) into a 150mL polytetrafluoroethylene beaker, add 4mL nitric acid and 12mL hydrochloric acid, heat to dissolve, add 8mL perchloric acid and heat until perchloric acid fumes are emitted to oxidize chromium To form hexavalent chromium, add hydrochloric acid dropwise to remove chromium, evaporate until the volume of the test solution is less than 1mL, cool slightly, add 6mL nitric acid (1+3), heat to dissolve soluble salts, add 3 drops of sodium nitrite (150g / L) Slightly boil to remove nitrogen oxides, take it off, add 10mL citric acid (100g / L), add solid sodium hydroxide and heat to dissolve until the solution is alkaline, cool, add nitric acid (1+1) dropwise to pH The test paper is neutral. Add 4mL of nitric acid (1+1), add 3mL of hydrofluoric acid (1+2), heat until the solution is clear and transparent, remove it, add 12mL of boric acid (50g / L), mix well, cool to...

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PUM

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Abstract

The invention discloses a phosphor analyzing method in the high-temperature alloy, which is characterized by the following: heating to dissolve sample through compound acid such as azotic acid and hydrochloric acid or azotic acid, hydrochloric acid and hydrofluoric acid (or microwave sample-fusing furnace); adding perchloric acid to heat until smoke; dripping hydrochloric acid to remove chromium; adding complex citrate in the alkali dielectric; adding complex niobium, tantalum, zirconium, hafnium, titanium, vanadium, tungsten fluohydric acid in the azotic acid dielectric; extracting phosphor through butanol-chloroform composite agent and ammonium molybdate; reextracting organic phase through hydrochloric solution of tin chloride; testing absorbance of water phase at 680nm. The invention eliminates influence of high-content interference element, whose result is accurate and reliable with testing greatest lower limit as 0.0002%(m/m).

Description

technical field [0001] The invention relates to an analysis and test method, in particular to an analysis method for phosphorus in superalloys. Background technique [0002] Superalloys are widely used in aviation, aerospace, petrochemical and other fields. The development of superalloy technology and the improvement of smelting process level have put forward higher requirements for the analysis of impurity elements in superalloys. Among them, it is required to accurately measure less than 0.002% ( m / m) of phosphorus. At present, methods for determining low-content phosphorus in superalloys include Chinese national standard GB 223.62-1988 and American ASTM E354-93(2000)e1, etc. In the Chinese national standard GB 223.62-1988, the interfering element tungsten is used in EDTA (disodium ethylenediaminetetraacetic acid) ammonia solution to precipitate and separate phosphorus with beryllium as a carrier; niobium, tantalum, titanium and zirconium use copper iron reagent-chlorofor...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N1/28G01N21/80G01N21/3563
Inventor 陈明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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