Page 96 - 理化检验-化学分册2025年第三期

张 庸，等：不同加热方式测定铝及铝合金中氢的差异性初步探讨

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Preliminary Discussion on Differences in Determination of Hydrogen in Aluminum
and Aluminum Alloy by Different Heating Methods

ZHANG Yong , YAO Jiaren , BAO Zhichao , LIU Pan , WANG Huaming , YU Yingjie 1*
5
3
4
1
2
(1. Liaoning Academy of Materials, Shenyang 110167, China; 2. Shanghai Key Laboratory of Engineering Material Application
and Evaluation, Shanghai Research Institute of Materials Co., Ltd., Shanghai 200437, China; 3. AECC Shenyang Liming Aero-
engine Co., Ltd., Shenyang 110043, China; 4. National Key Laboratory of Marine Corrosion and Protection, Luoyang Ship
Material Research Institute, Luoyang 471023, China; 5. Hongxing Iron & Steel Co., Ltd., Jiuquan Iron and Steel Group Corporation,
Jiayuguan 735100, China)
Abstract: There was "secondary hydrogen" phenomenon in aluminum and aluminum alloy determination by pulse inert
gas melting method (hereinafter referred to as the pulse method), which meant, there was still a significant hydrogen release after
reheating the measured sample. Domestic scholars tended to believe that the interference caused by the release of hydrogen from
graphite crucibles, while Russia scholars tended to believe that the heating time was too short to completely release hydrogen. In
order to compare the different views, hydrogen in aluminum and aluminum alloy was determined by pulse method and thermal
desorption method. The results were as follows: there was still obvious hydrogen released when the samples which were analyzed by
pulse method were tested again by thermal desorption method, which meant "secondary hydrogen" phenomenon. The hydrogen in
aluminum reference materials GBW (E) 020030[certified value （0. 19±0. 04） μg·g −1 ], GBW (E) 020030a[certified value（0. 24±
−1 −1
0. 06）μg·g , and GBW (E) 020031a [certified value （0. 25±0. 05）μg·g ] which were certified by the pulse method, were

tested by thermal desorption method, and the results were 0. 38, 0. 58, and 0. 71 μg · g −1 , with the release peaks of the former two
located at approximately 450, 380 ℃, respectively; The AlSi samples from different batches were simultaneously analyzed by pulse
−1
method and thermal desorption method, with results of 0. 13, 0. 16, 0. 16 μg · g −1 for pulse method and 0. 70, 0. 53, 0. 48 μg · g
for thermal desorption method, respectively. The release peaks of the former two were mainly located at 350 ℃ and 580 ℃. As shown
by the above results, the testing results of thermal desorption method were generally higher than those of pulse method. Considering
that the former used quartz tube heating, did not involve graphite crucible and slowly heated up, and the analysis time was measured
in hours, it was preliminarily believed that the viewpoint that the heating time was too short to completely release hydrogen, was
more convincing. However, considering the widespread use of pulse method for determination of hydrogen in aluminum alloys in
China, more detailed comparison and verification were still needed in order to obtain more convincing conclusions.
Keywords: pulse inert gas melting method; thermal desorption method; aluminum and aluminum alloy; secondary hydrogen

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