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Zirconium and zirconium alloy lithium content measuring method

A zirconium alloy and content technology, applied in the field of chemical analysis, can solve the problems of poor stability of measurement results, difficulty in lithium content, interference of easily ionized elements, etc., and achieve the effect of high international recognition, high accuracy and fast analysis speed

Active Publication Date: 2017-12-12
国核宝钛锆业股份公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Second, the current mainstream inductively coupled plasma emission spectrometer is a vertical observation rectangular tube. The vertical observation technology is extremely susceptible to interference in the determination of easily ionizable elements (alkali metals and alkaline earth metals), and the matrix effect is particularly harmful to the interference of easily ionizable elements. Obviously, it leads to poor stability of the measurement results and does not meet the requirements of quantitative analysis
Lithium is the third element in the periodic table. It has a light atomic weight and is easily ionized. It is extremely difficult to determine the content of lithium with vertical observation technology.

Method used

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  • Zirconium and zirconium alloy lithium content measuring method
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  • Zirconium and zirconium alloy lithium content measuring method

Examples

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Embodiment 1

[0026] The method for determining lithium content in zirconium and zirconium alloys in the present embodiment comprises the following steps:

[0027] Step 1, turning pure zirconium or zirconium alloy to obtain chip-like samples, then cleaning the chip-like samples and drying them for later use;

[0028] In the specific implementation process of this embodiment, the pure zirconium or zirconium alloy chip-like sample was soaked and cleaned with absolute ethanol for more than 30 seconds, and then the sample was rinsed with pure water for more than 10 times, and then the chip-like sample was kept at a temperature not exceeding 50°C. Dry under the condition of high temperature; the absolute ethanol is above the analytical grade, and the pure water meets the requirements of GB / T 6682 laboratory grade water;

[0029] Step 2, using the heap cone quartering method to shrink and select the chip sample after drying in step 1 to obtain the sample to be tested;

[0030] In this embodiment...

Embodiment 2

[0044] The method for determining lithium content in zirconium and zirconium alloys in the present embodiment comprises the following steps:

[0045] Step 1, turning pure zirconium or zirconium alloy to obtain chip-like samples, then cleaning the chip-like samples and drying them for later use;

[0046] In the specific implementation process of this embodiment, the pure zirconium or zirconium alloy chip-like sample was soaked and cleaned with absolute ethanol for more than 30 seconds, and then the sample was rinsed with pure water for more than 10 times, and then the chip-like sample was kept at a temperature not exceeding 50°C. Dry under the condition of high temperature; the absolute ethanol is above the analytical grade, and the pure water meets the requirements of GB / T 6682 laboratory grade water;

[0047] Step 2, using the heap cone quartering method to shrink and select the chip sample after drying in step 1 to obtain the sample to be tested;

[0048] In this embodiment...

Embodiment 3

[0062] The method for determining lithium content in zirconium and zirconium alloys in the present embodiment comprises the following steps:

[0063] Step 1, turning pure zirconium or zirconium alloy to obtain chip-like samples, then cleaning the chip-like samples and drying them for later use;

[0064] In the specific implementation process of this embodiment, the pure zirconium or zirconium alloy chip-like sample was soaked and cleaned with absolute ethanol for more than 30 seconds, and then the sample was rinsed with pure water for more than 10 times, and then the chip-like sample was kept at a temperature not exceeding 50°C. Dry under the condition of high temperature; the absolute ethanol is above the analytical grade, and the pure water meets the requirements of GB / T 6682 laboratory grade water;

[0065] Step 2, using the heap cone quartering method to shrink and select the chip sample after drying in step 1 to obtain the sample to be tested;

[0066] In this embodiment...

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Abstract

The invention provides a zirconium and zirconium alloy lithium content measuring method. The zirconium and zirconium alloy lithium content measuring method comprises the following steps of, firstly, turning pure zirconium or zirconium alloy to obtain scrap samples, cleaning and drying the scrap samples; secondly, performing a sampling process through coning and quartering; thirdly, dissolving the samples, transferring the solution into a volumetric flask for volume fixing to obtain a solution to be detected; fourthly, preparing a series of lithium calibrating solutions of different concentrations; fifthly, performing measurement one by one through an inductively coupled plasma emission spectrograph to establish a calibration curve of the correspondence between the concentration of the lithium calibrating solutions and lithium characteristic spectrum intensity; sixthly, measuring the lithium characteristic spectrum intensity of the solution to be detected through the inductively coupled plasma emission spectrograph, and according to the calibration curve, computing the mass content of lithium in the pure zirconium or zirconium alloy. The zirconium and zirconium alloy lithium content measuring method overcomes the difficulties that the vertical observation technology for detecting easily ionizable elements is vulnerable to interference as well as the inductively coupled plasma emission spectrograph cannot meet the requirements of trace analysis on detection limit during measurement of a zirconium-based hypersaline environment, thereby meeting the zirconium and zirconium alloy detecting requirements of the nuclear industry.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for measuring lithium content in zirconium and zirconium alloys. Background technique [0002] Metal zirconium and its alloys are widely used in cladding materials and core structural materials of water-cooled power reactors. At present, the chemical analysis methods of zirconium and zirconium alloys publicly reported in China are mainly GB / T13747 national standard for chemical analysis methods of zirconium and zirconium alloys promulgated in 1992, and inductively coupled plasma emission spectrometry published by Li Gang et al. in 2012 for the determination of nuclear-grade zirconium alloys 17 kinds of constant and trace elements. None of these documents involves the determination of lithium in zirconium and zirconium alloys. The main technical difficulties are as follows: [0003] First, the upper limit of lithium element content is extremely low, no more th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/28
CPCG01N1/28G01N21/73
Inventor 李刚汪澜党翠玉
Owner 国核宝钛锆业股份公司
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