A method for measuring hydrogen content in nuclear-grade zirconium materials

A technology of hydrogen element and hydrogen content, which is applied in the preparation of test samples, test metals, material inspection products, etc., can solve the problems of long analysis period, high cost, difficult to support chemical wet analysis, etc., to ensure accuracy Effect

Active Publication Date: 2016-08-24
国核锆铪理化检测有限公司 +1
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  • Abstract
  • Description
  • Claims
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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

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  • A method for measuring hydrogen content in nuclear-grade zirconium materials

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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

A method for determining the content of hydrogen in nuclear-grade zirconium materials. Step 1: Cut the nuclear-grade zirconium material into solid samples with a mass of 0.1g-0.3g; Step 2: First pickle the solid sample for 5-30s to remove the oxygen-rich layer on the surface and the hydrogen adsorbed during the machining process or other gas elements; then use acetone to clean the sample after pickling for 10s~50s, and then put it in an oven to dry at 50~60°C to remove the stained layer on the surface of the sample to ensure that the sample is clean; step 3: Put the sample pretreated in step 2 into the hydrogen meter, and use the hydrogen meter to measure the hydrogen content in the solid sample. The invention overcomes the shortcomings of the existing measurement methods and meets the actual detection requirements of nuclear-grade zirconium materials.

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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Patent Type & Authority Patents(China)
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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