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Method for determination of trace element Na in pure Hf (hafnium)

A trace element, quality technology, applied in the field of pure metal trace element analysis, to achieve the effect of fast measurement, saving manpower and material resources, and eliminating ionization effect

Active Publication Date: 2014-07-02
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the advancement of technology, the determination of trace element content in pure substances is a new field. There is no method for measuring trace element sodium in pure Hf by flame atomic absorption spectrometry at home and abroad.

Method used

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  • Method for determination of trace element Na in pure Hf (hafnium)
  • Method for determination of trace element Na in pure Hf (hafnium)
  • Method for determination of trace element Na in pure Hf (hafnium)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] To measure the sodium content in pure Hf1, an atomic absorption spectrometer A (PE AAnalyst 100 atomic absorption spectrometer) is used. The working conditions and analysis lines of the instrument are shown in the following table:

[0037]

[0038] The reagents used in the determination process of this method are:

[0039] Cesium chloride solution: the mass-volume concentration of cesium in the solution is 10mg / mL. The preparation method is to weigh 2.53g of spectrally pure cesium chloride, place it in a 100mL beaker, add water to dissolve it, transfer it into a 200mL volumetric flask, and dilute it with water to scale, shake well;

[0040] Na standard solution Ⅰ: the mass-volume concentration is 0.10 mg / mL. The preparation method is to weigh 0.2541 g of sodium chloride which has been burned at 550 °C for 2 hours and cooled to room temperature in a desiccator. The mass fraction of sodium chloride is not Less than 99.95%, put it in a 250mL beaker, add water to dissol...

Embodiment 2

[0062] To measure the sodium content in pure Hf2, an atomic absorption spectrometer A (PE AAnalyst 100 atomic absorption spectrometer) is used. The working conditions and analysis lines of the instrument are shown in the following table:

[0063]

[0064]

[0065] The reagents used in the determination process of this method are:

[0066] Cesium chloride solution: the mass-volume concentration of cesium in the solution is 10mg / mL. The preparation method is to weigh 2.53g of spectrally pure cesium chloride, place it in a 100mL beaker, add water to dissolve it, transfer it into a 200mL volumetric flask, and dilute it with water to scale, shake well;

[0067] Na standard solution Ⅰ: the mass-volume concentration is 0.10 mg / mL. The preparation method is to weigh 0.2541 g of sodium chloride which has been burned at 550 °C for 2 hours and cooled to room temperature in a desiccator. The mass fraction of sodium chloride is not Less than 99.95%, put it in a 250mL beaker, add wat...

Embodiment 3

[0089] To measure the sodium content in pure Hf3, an atomic absorption spectrometer A (PE AAnalyst 100 atomic absorption spectrometer) is used. The working conditions and analysis lines of the instrument are shown in the table below:

[0090]

[0091] The reagents used in the determination process of this method are:

[0092] Cesium chloride solution: the mass-volume concentration of cesium in the solution is 10mg / mL. The preparation method is to weigh 2.53g of spectrally pure cesium chloride, place it in a 100mL beaker, add water to dissolve it, transfer it into a 200mL volumetric flask, and dilute it with water to scale, shake well;

[0093] Na standard solution Ⅰ: the mass-volume concentration is 0.10 mg / mL. The preparation method is to weigh 0.2541 g of sodium chloride which has been burned at 550 °C for 2 hours and cooled to room temperature in a desiccator. The mass fraction of sodium chloride is not Less than 99.95%, put it in a 250mL beaker, add water to dissolve, ...

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Abstract

The invention belongs to the analysis technics of trace element in pure metal, and relates to a method for determination of trace element Na in pure Hf (hafnium). A FAAS (flame atomic absorption spectrometry) is applied to the determination of the trace element Na in pure Hf, and the analysis range is 0.001%-0.005%. A pure Hf sample is processed by hydrochloric acid, nitric acid and hydrofluoric acid, the measurement condition is optimized, and interference and method for controlling the interference are researched as emphasis. The cesium chloride is chosen as ionization inhibitor, the influence test in the dosage of the acid for dissolution and matrix interference is carried and strict control is performed, and the standard addition method is applied to determine the content of Na. The method has the advantages that the established method for determination of trace element Na in pure Hf is accuracy and reliable, and the requirement of scientific research is also satisfied. The determination lower limit of the methodis low and is 0.001%. The ionization effect is eliminated and the sensitivity of determination is improved by adoption of cesium chloride as the ionization inhibitor. The method is quick, the operation is simple, and labour power and material resources are saved largely.

Description

technical field [0001] The invention belongs to pure metal trace element analysis technology, and relates to a method for measuring trace element sodium in pure Hf by atomic absorption spectrometry. Background technique [0002] Hf is a shiny silver-gray transition metal with a melting point of 2233°C, a boiling point of 4602°C and a density of 13.31g / cm 3 . Hf is inactive in nature and forms an oxide coating on the surface. It is very stable at room temperature. Powdered Hf is easy to spontaneously ignite in the air and does not react with water, dilute acid or strong alkali, but is easily soluble in aqua regia and hydrofluoric acid. . Hf is useful because it is easy to emit electrons, such as the filament of an incandescent lamp, the cathode of an X-ray tube, the alloy of Hf and tungsten or molybdenum is used as an electrode of a high-voltage discharge tube, and Hf is also used for nuclear reactor control rods. With the development of industry, new materials are constan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31G01N1/38
Inventor 任慧杨春晟叶晓英
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS