Method for accurately determining zirconium and hafnium components in zirconium compound by using extraction spectrophotometric method

A zirconium compound and photometric technology, which is applied in the direction of material analysis by chemical reaction of materials, and material analysis by observing the influence of chemical indicators, can solve the problem of high testing costs for instruments and equipment, and reduce testing costs. The effect of high sensitivity and easy operation of the instrument

Inactive Publication Date: 2012-10-03
WUHAN INSTITUTE OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have high requirements for equipment and testing costs, which limits their use to a certain extent.

Method used

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  • Method for accurately determining zirconium and hafnium components in zirconium compound by using extraction spectrophotometric method
  • Method for accurately determining zirconium and hafnium components in zirconium compound by using extraction spectrophotometric method
  • Method for accurately determining zirconium and hafnium components in zirconium compound by using extraction spectrophotometric method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step (1): Drawing of standard curves for zirconium and hafnium: prepare 1.0×10 -5 mol / L atomic level zirconium standard solution and hafnium standard solution, add 0.500mL, 0.750mL, 1.000mL, 1.250mL, 1.500mL zirconium standard solution and hafnium standard solution into two sets of 25mL volumetric flasks respectively, then add 4.0 mL 0.10 %(wt) arsenazo III solution for color development of zirconium and hafnium, then add 4.0 mL 5.0% (wt) urea solution for stable color development, add 8.0 mol / L nitric acid to the scale of the volumetric flask for color development environment, and take another blank The sample was used as the background, and after 1.0 h of color development, the absorbance was measured with a UV spectrometer. The absorbance of the solution after color development was measured at 665±5 nm. The mass concentration of zirconium and hafnium was taken as the abscissa, and the absorbance was taken as the ordinate to draw zirconium. and hafnium standard curve...

Embodiment 2

[0040] Step (1): The drawing of the standard curves of zirconium and hafnium is the same as the step (1) in Example 1.

[0041] Step (2): Mix MIBK and 3.0 mol / L HSCN at a volume ratio of 1:1, saturate for 15.0 min at an interface stirring speed of 200 r / min, separate the liquid, and use the upper organic phase as the extraction agent; accurately weigh 3.00 g zircon sand, decompose by sintering with sodium hydroxide, wash, leach zirconium and hafnium with hydrochloric acid, add 22.840 g ammonium thiocyanate, and dilute to 100 mL of feed solution as the extraction water phase.

[0042] Step (3): According to the volume ratio: extraction agent: tested material liquid: washing liquid: stripping liquid = 7: 3: 1: 2, take 5.0 mL of the material liquid in the separatory funnel, add the extraction agent, and shake for 3 Min, liquid separation, the raffinate aqueous phase was extracted twice with fresh saturated HSCN MIBK, the organic phases after three extractions were combined, washe...

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Abstract

The invention relates to a method for accurately determining zirconium and hafnium components in a zirconium-hafnium mixture by using an extraction spectrophotometric method. In the presence of a large amount of zirconium, the zirconium and hafnium are extracted and separated by using a methylisobutylketone-thiocyanic acid (MIBK-HSCN) system solvent, and the zirconium and hafnium components are accurately determined by combining an arsenazo III spectrophotometry. By the method, the zirconium and hafnium components in tested objects of zirconium oxychloride, baddeleyite, zircon sand, zirconium oxide, ferrozirconium and the like can be accurately determined; and the method has the advantages of high sensitivity, good selectivity, simplicity, convenience and quickness for instrument operation, accurate determination result and the like, and the test cost and the requirement on instrument equipment can be effectively reduced.

Description

technical field [0001] The invention belongs to the technical field of analysis methods for zirconium and hafnium content, and in particular relates to a method for precisely measuring zirconium and hafnium components in zirconium compounds by extraction photometry, which can precisely measure zirconium oxychloride, baddeleyite, zircon sand, zirconium oxide and zirconium The content of zirconium and hafnium in the measured object such as iron alloy. Background technique [0002] Zirconium and hafnium have the same external electronic structure, and due to the influence of lanthanide contraction, the atomic radius, ionic radius and even chemical properties of zirconium and hafnium are very similar. In nature, zirconium and hafnium are often symbiotic, and almost all zirconium contains 1% to 3% of hafnium. At present, the main methods for analyzing the content of zirconium and hafnium include weight precipitation method, complexometric titration method, spectrophotometry meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78
Inventor 徐志高池汝安吴明张臻悦余军霞张越非
Owner WUHAN INSTITUTE OF TECHNOLOGY
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