Method for measuring 63Ni in metal sample

A measurement method and sample technology, applied in the preparation of test samples, X/γ/cosmic radiation measurement, sampling, etc.

Pending Publication Date: 2021-04-02
THE 404 COMPANY LIMITED CHINA NAT NUCLEAR
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  • Abstract
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Problems solved by technology

[0004] for solid samples 63 There is no mature method for the determination of Ni in China, and there is ...

Method used

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  • Method for measuring 63Ni in metal sample
  • Method for measuring 63Ni in metal sample
  • Method for measuring 63Ni in metal sample

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Embodiment Construction

[0042] The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0043] 1) Sample pretreatment

[0044] Take 0.8-1.2g metal sample, add 8mL-12mL 12mol / L HCl and heat it on the electric heating plate. After the sample is dissolved, add appropriate amount of hydrogen peroxide, 5mL perchloric acid, and dilute to 50mL capacity with 9mol / L HCl In the bottle ①, the constant volume is V 1 .

[0045] 2) 63 Ni and 55 Fe, 60 Co separation and enrichment

[0046] Use 80-120 mesh 256×4 type anion-exchange resin to load the ion-exchange column, and the diameter-to-height ratio of the ion-exchange column after loading is 1:12-15.

[0047] After equilibrating the 256×4 type anion exchange column with 18mL~22mL 9mol / L HCl, take an appropriate volume (V 2 ) sample on the column, so that the iron content in it is not more than 150mg.

[0048] Add 18mL~22mL 9mol / L HCl to wash the 256×4 type anion exchange column, com...

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Abstract

The invention belongs to the technical field of nuclear facility decommissioning and three-waste treatment, and particularly relates to a method for measuring 63Ni in a metal sample. The method comprises the steps of taking a metal sample, adding HCl, heating on an electric heating plate, adding hydrogen peroxide and perchloric acid after the sample is dissolved, and fixing the volume to a volumetric flask (1) by using HCl; carrying out separation and enrichment on 63Ni, 55Fe and 60Co, and loading anion exchange resin into an ion exchange column; balancing the ion exchange column by using HCl,taking a sample with the volume of V2 from the volumetric flask (1), and putting the sample on the column to ensure that the iron content is not more than 150mg; adding HCl to wash the ion exchange column, combining and collecting an adsorption effluent and a washing effluent to serve as a nickel column-loading solution with the volume of V3; and carrying out separation and enrichment on 63Ni, 137Cs and 90Sr, placing a nickel resin column on a vacuum extraction box, and taking ammonium citrate, and adding ammonium citrate into the nickel resin column to be balanced. By adopting the analysis method, enrichment of low-content 63Ni in a sample can be realized, interference of nuclides such as 55Fe, 60Co, 137Cs and 90Sr on 63Ni measurement is eliminated, and the method has the advantages of short analysis period, high accuracy, good reloading recovery rate and the like.

Description

technical field [0001] The invention belongs to the technical field of decommissioning of nuclear facilities and treatment of three wastes, and in particular relates to a 63 Ni determination method. Background technique [0002] 63 Ni is a long half-life (100 years), low-energy β (maximum energy 65.9keV) radiation nuclide, is one of the important neutron activation products of reactors, and widely exists in reactor components such as stainless steel, aluminum alloy, graphite, concrete and other radioactive materials. solid waste and wastewater. In the decommissioning of reactor nuclear facilities, the various material media and radioactive waste produced 63 Determination of Ni, to understand its activity and distribution in the reactor components, for the estimation of the reactor body and its subsidiary structural materials 63 It is of great significance to provide a technical basis for the decommissioning scheme design and the reasonable treatment and disposal of compo...

Claims

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Application Information

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IPC IPC(8): G01T1/167G01T1/204G01N1/40
CPCG01T1/167G01T1/2047G01N1/405Y02E30/30
Inventor 徐丽霞韩雪梅李丽军时丽敏陈静孔雪艳靳小军冯军耀
Owner THE 404 COMPANY LIMITED CHINA NAT NUCLEAR
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