A method for measuring magnesium content in nuclear-grade zirconium sponge particles

A nuclear-grade sponge zirconium and magnesium content technology, applied in the field of chemical analysis, can solve the problems of accuracy and precision interference of instrumental analysis methods, failure to meet the detection requirements of zirconium and zirconium alloys, backward flame atomic absorption spectrometry technology, etc., to achieve Improve monitoring ability, broaden the measurement range, good representative effect

Active Publication Date: 2020-04-24
国核宝钛锆业股份公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Due to the extremely low content of magnesium in sponge zirconium, it is difficult to measure it. Currently, GB / T13747.9-92 "Methods for Chemical Analysis of Zirconium and Zirconium Alloys for the Determination of Magnesium by Flame Atomic Absorption Spectrometry" promulgated in 1992 is mainly used in this field. Atomic absorption spectrometry is outdated in technology, cumbersome in operation, low in sensitivity, low in precision, and narrow in its measurement range, which has been unable to meet the increasingly stringent detection requirements for zirconium and zirconium alloys; in 2012, Li Gang and others reported "Inductively Coupled Plasma Determination of 17 constant and trace elements in nuclear-grade zirconium alloys by spectroscopic method", which mentioned a method for the determination of magnesium in zirconium and zirconium alloys. This method is used to determine the amount of magnesium in a high-salt zirconium matrix. The measurement results are greatly affected by the matrix effect, which will greatly interfere with the accuracy and precision of the instrument analysis method, and the measurement range of this method is narrow, which has no obvious improvement compared with GB / T 13747.9-92

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  • A method for measuring magnesium content in nuclear-grade zirconium sponge particles
  • A method for measuring magnesium content in nuclear-grade zirconium sponge particles
  • A method for measuring magnesium content in nuclear-grade zirconium sponge particles

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Embodiment 1

[0023] The method for measuring the magnesium content in the nuclear grade sponge zirconium particles of the present embodiment comprises the following steps:

[0024] Step 1. Sampling and weighing the nuclear-grade zirconium sponge particles by the heap cone quartering method;

[0025] In the specific implementation process of this embodiment, at first randomly extract nuclear-grade zirconium sponge particle samples from each batch of zirconium sponge, and the extraction quantity accounts for 20% of the number of buckets (but not less than 2 buckets). Take samples from the middle and lower parts respectively, each part takes about 1000g of samples, then mix the samples evenly, and divide them into about 500g by the heap cone quartering method, and then accurately weigh 400g of nuclear-grade zirconium sponge particle samples from it , accurate to 1.000g; the particle size of the nuclear-grade zirconium sponge particles is 1 mm to 100 mm;

[0026] Step 2, adding the nuclear-gr...

Embodiment 2

[0040] The method for measuring the magnesium content in the nuclear grade sponge zirconium particles of the present embodiment comprises the following steps:

[0041] Step 1. Sampling and weighing the nuclear-grade zirconium sponge particles by the heap cone quartering method;

[0042] In the specific implementation process of this embodiment, at first randomly extract nuclear-grade zirconium sponge particle samples from each batch of zirconium sponge, and the extraction quantity accounts for 20% of the number of buckets (but not less than 2 buckets). Take samples from the middle and lower parts respectively, each part takes about 1000g of samples, then mix the samples evenly, and divide them into about 700g by the heap cone quartering method, and then accurately weigh 625g of nuclear-grade zirconium sponge particle samples , accurate to 1.000g; the particle size of the nuclear-grade zirconium sponge particles is 1 mm to 100 mm;

[0043] Step 2, adding the nuclear-grade zirc...

Embodiment 3

[0056] The method for measuring the magnesium content in the nuclear grade sponge zirconium particles of the present embodiment comprises the following steps:

[0057] Step 1. Sampling and weighing the nuclear-grade zirconium sponge particles by the heap cone quartering method;

[0058] In the specific implementation process of this embodiment, at first randomly extract nuclear-grade zirconium sponge particle samples from each batch of zirconium sponge, and the extraction quantity accounts for 20% of the number of buckets (but not less than 2 buckets). Take samples from the middle and lower parts respectively, each part takes about 1000g of samples, then mix the samples evenly, and divide them into about 300g by the heap cone quartering method, and then accurately weigh 250g of nuclear-grade zirconium sponge particle samples , accurate to 1.000g; the particle size of the nuclear-grade zirconium sponge particles is 1 mm to 100 mm;

[0059] Step 2, adding the nuclear-grade zirc...

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Abstract

The invention provides a method for measuring the magnesium content in nuclear-grade zirconium sponge particles, comprising the following steps: 1. Sampling and weighing the nuclear-grade zirconium sponge particles by stacking cone quartering method; 3. Prepare magnesium standard solution, measure magnesium standard solution with inductively coupled plasma emission spectrometer and establish calibration curve; 4. Measure leachate with inductively coupled plasma emission spectrometer, and calculate nuclear-grade zirconium sponge Magnesium content in pellets. The invention uses inductively coupled plasma emission spectrometry to measure the magnesium content in nuclear-grade zirconium sponge particles, which has a wide measurement range, high sensitivity, high precision, high accuracy, simple analysis steps and easy to grasp, and can effectively monitor the quality of zirconium sponge to meet Testing requirements for zirconium and zirconium alloys in the nuclear industry.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a method for measuring magnesium content in nuclear-grade sponge zirconium particles. Background technique [0002] The magnesium element contained in sponge zirconium mainly comes from the magnesium reduction process in the production process of sponge zirconium. The content of magnesium element is very important to the performance of zirconium alloys. Magnesium is a chemical component that must be strictly controlled in various grades of zirconium alloys in the nuclear industry. Due to the extremely low content of magnesium in zirconium sponge, it is very difficult to measure. Currently, GB / T13747.9-92 "Methods for Chemical Analysis of Zirconium and Zirconium Alloys for the Determination of Magnesium by Flame Atomic Absorption Spectrometry" promulgated in 1992 is mainly used in this field. Atomic absorption spectrometry is backward in technology, cumberso...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/68
CPCG01N21/68
Inventor 李刚张娟萍马晓龙
Owner 国核宝钛锆业股份公司
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