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Method for measuring content of hydrogen element in nuclear-grade zirconium material

A technology of hydrogen element and hydrogen content, which is applied in the preparation of test samples, testing metals, material inspection products, etc., can solve the problems of long analysis cycle, complicated operation and high cost, and achieve the effect of ensuring accuracy

Active Publication Date: 2014-04-09
国核锆铪理化检测有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the vacuum melting method and the vacuum heating method need to use a vacuum system, the cost is high, the operation is relatively complicated and the analysis cycle is long, while the chemical wet method analysis is more complicated and difficult to support, and the analysis cycle is longer

Method used

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  • Method for measuring content of hydrogen element in nuclear-grade zirconium material

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Effect test

Embodiment 1

[0028] Example 1: Cut a pure zirconium sample (identified value of hydrogen: 0.00007% to 0.00015%) into a solid sample with a mass of 0.21g, and mix it with a mixed acid (recipe: 45ml HNO 3 +8ml HF+47ml H 2 O) pickling for 15s; then put the solid sample in acetone and wash it for 20s, and then dry it at 50-60°C; put the pretreated solid sample into the RH-600 hydrogen determination instrument, and measure the pure zirconium sample The hydrogen content in is measured three times respectively (promptly measuring three times), and the measured results are shown in the table below. Among them, the operating parameters of the hydrogen determination instrument are: analysis time 40s, purge time 20s, exhaust time 20s, degassing power 5200w, analysis power 4900w.

Embodiment 2

[0029] Embodiment 2: Zirlo product (hydrogen identification value: less than 0.00020%) is cut into the solid sample that quality is 0.25g, and with mixed acid (recipe is: 40ml HNO 3 +10ml HF+50ml H 2 O) pickling for 10s; then put the solid sample in acetone and wash it for 15s, and then dry it at 50-60°C; put the pretreated solid sample into the RH-600 hydrogen determination instrument, and measure the Zirlo sample The hydrogen content of the hydrogen content is measured three times respectively (promptly measuring three times), and the measured results are shown in the table below. Among them, the operating parameters of the hydrogen determination instrument are: analysis time 20s, purge time 10s, exhaust time 15s, degassing power 5400w, analysis power 5000w.

Embodiment 3

[0030] Embodiment 3: The Zr-4 product (certified value of hydrogen: less than 0.00020%) is cut into a solid sample with a quality of 0.15g, and mixed acid (recipe: 50ml HNO 3 +5ml HF+45ml H 2 O) Pickling for 20s; then put the solid sample in acetone and wash it for 40s, and then dry it at 50-60°C; put the pretreated solid sample into the RH-600 hydrogen determination instrument, and measure the Zr-4 test The hydrogen content in the sample was measured three times respectively (i.e. measured three times), and the measured results are shown in the table below. Among them, the operating parameters of the hydrogen determination instrument are: analysis time 60s, purge time 30s, exhaust time 30s, degassing power 5000w, analysis power 4700w.

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Abstract

The invention discloses a method for measuring the content of a hydrogen element in a nuclear-grade zirconium material. The method comprises the following steps: 1, cutting the nuclear-grade zirconium material into 0.1-0.3g of a solid test sample; 2, firstly, pickling the solid test sample for 5-30s so as to remove an oxygen enrichment layer on the surface of the solid test sample and hydrogen and other gas elements adsorbed in the machining process, subsequently washing the pickled test sample for 10-50 seconds by using acetone, subsequently putting the test sample into an oven to be dried at 50-60 DEG C, and removing a contaminated layer on the surface of the test sample so as to ensure the cleanness of the test sample; 3, putting the test sample pretreated in the step 2 into a hydrogen measuring instrument so as to measure the content of the hydrogen in the solid test sample by using the hydrogen measuring instrument. By adopting the method, the defects of the conventional measuring method are overcome, and requirements of practical detection on the nuclear-grade zirconium material are met.

Description

technical field [0001] The invention relates to the technical field of analysis of nuclear-grade zirconium materials, in particular to a method for determining the content of hydrogen in nuclear-grade zirconium materials. Background technique [0002] The gas element H contained in nuclear-grade zirconium materials mainly comes from the moisture and humid air in the smelting process, and the hydrogen content plays a vital role in the performance of nuclear-grade zirconium materials. Therefore, for nuclear-grade zirconium materials, H gas content is a must-test item, so its analysis method should be studied. At present, the methods for measuring hydrogen in metals include vacuum melting method, vacuum heating method and chemical wet method. However, since the vacuum melting method and the vacuum heating method need to use a vacuum system, the cost is high, the operation is relatively complicated and the analysis cycle is long, while the chemical wet method analysis is more c...

Claims

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Application Information

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IPC IPC(8): G01N33/20G01N1/28G01N1/34G01N1/44
Inventor 李刚张娟萍李艳陈苏马晓龙麻凯袁改焕王晨阳
Owner 国核锆铪理化检测有限公司
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