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A method for measuring hafnium isotopic abundance by thermal ionization mass spectrometer

A technology of isotope abundance and ionization mass spectrometer, which is applied in the field of measuring hafnium isotopic abundance with thermal ionization mass spectrometer, can solve the problems of low ion emission efficiency, insignificant improvement effect, weak ion current signal, etc. The effect of improving the measurement sensitivity and prolonging the time when the signal is stable

Active Publication Date: 2022-03-11
NUCLEAR POWER INSTITUTE OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the propellant used is generally phosphoric acid (H 3 PO 4 ), although the emission efficiency of hafnium ions is improved to a certain extent, but the improvement effect is not significant
[0004] In summary, the existing methods for measuring hafnium isotopes by thermal ionization mass spectrometry have problems such as low hafnium ion emission efficiency, weak ion current signal, and low sensitivity. efficiency, enhance the hafnium ion current signal, and improve the purpose of hafnium measurement sensitivity

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  • A method for measuring hafnium isotopic abundance by thermal ionization mass spectrometer

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Embodiment 1

[0039] This embodiment proposes a method for measuring the abundance of hafnium isotopes with a thermal ionization mass spectrometer, such as figure 1 As shown, the method of the present embodiment includes the following steps:

[0040] Step S1, Emitter preparation: prepare the emissive agent required for measurement, the emissive agent is a mixed suspension of carbon nanotubes; specifically include:

[0041] 1.1 Preparation of carbon nanotube mixed suspension: choose composite-walled carbon nanotubes (CNTs) with a diameter of 60-100 nm and a length of 5-15 μm, and weigh 0.1-1 g of carbon nanotubes and 0.1-1 g of boric acid (H 3 BO 3 ), add 100mL saturated sucrose solution, and ultrasonically disperse for 10-20min to form a uniform suspension.

[0042]Step S2, sample loading: load the sample and propellant on the rhenium belt and dry it, and install the plug-in in a single belt; specifically include:

[0043] 2.1 Preparation of sample insert: Weld metal rhenium strip (width...

Embodiment 2

[0052] In this example, the method proposed in the above example is used to measure the loading amount of 1 μg hafnium, which specifically includes:

[0053] Step S1, launcher preparation:

[0054] 1.1 Preparation of carbon nanotube mixed suspension: select composite-walled carbon nanotubes (CNTs) with a diameter of 60-100 nm and a length of 5-15 μm, and weigh 0.5 g of carbon nanotubes and 0.5 g of boric acid (H 3 BO 3 ), add 100mL saturated sucrose solution, ultrasonically disperse for 15 minutes to form a uniform suspension.

[0055] Step S2, sample loading:

[0056] 2.1 Preparation of sample insert: Weld metal rhenium strip (width 0.75 mm, thickness 0.04 mm) on the sample insert, and degas the rhenium strip in a degassing device.

[0057] 2.2 Sample loading: Add the hafnium sample solution to be tested dropwise on the center of the rhenium strip, the loading amount of hafnium is 1 μg, and dry at a current below 1.5A.

[0058] 2.3 Loading of carbon nanotube mixed suspens...

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Abstract

The invention discloses a method for measuring the abundance of hafnium isotopes by a thermal ionization mass spectrometer, which sequentially comprises: the first step, preparation of the propellant: preparing the propellant required for measurement, and the propellant is a mixed suspension of carbon nanotubes; the second step 1. Sample loading: load the sample and emitter on the rhenium belt and dry it, and install the plug-in in a single belt; the third step, sample measurement: set the thermal ionization mass spectrometer to positive ion mode, and the ion to be detected is Hf + , the temperature of the sample belt rises to 5.5-5.8A, and is measured after stabilization. The invention significantly improves the ion emission efficiency, enhances the ion current signal, improves the measurement sensitivity, weakens the fractionation effect, prolongs the stable time of the signal, and improves the repeatability and accuracy of the measurement result.

Description

technical field [0001] The invention relates to the technical field of isotope measurement, in particular to a method for measuring hafnium isotope abundance with a thermal ionization mass spectrometer. Background technique [0002] Hafnium (Hf) has an atomic number of 72 and an atomic weight of 178.49. It is a lustrous silver-gray transition metal. Hafnium has 6 natural stable isotopes: 174 Hf, 176 Hf, 177 Hf, 178 Hf, 179 Hf, 180 Hf. Hafnium is a by-product of zirconium production. Metal hafnium has a high neutron absorption cross section and can be used as a control rod material for nuclear reactors. Hafnium control rods have the advantages of good mechanical properties, corrosion resistance, and long life. In order to study the performance of hafnium control rods, it is necessary to accurately measure the change of hafnium isotope abundance before and after irradiation. [0003] As a classic isotope measurement method, thermal ionization mass spectrometry has the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 梁帮宏苏冬萍罗婷李顺涛张劲松陈云明李兵
Owner NUCLEAR POWER INSTITUTE OF CHINA