Method for improving precision and accuracy of hydrogen in oxygen-nitrogen-hydrogen combined determination of titanium or titanium alloy

Abstract

The invention provides a method for improving precision and accuracy of hydrogen in oxygen-nitrogen-hydrogen combined determination of titanium or a titanium alloy. The method comprises the following steps of: putting a graphite crucible into a high temperature furnace, filling inert gases into the high temperature furnace to discharge air in the furnace; carrying out heating, and maintaining temperature for more than 5h under a furnace temperature of 700 to 1000 DEG C; freely decreasing the temperature to the temperature of 400 to 500 DEG C, and then taking out the graphite crucible; then, mounting the graphite crucible into an electrode furnace of an oxygen-nitrogen-hydrogen analyzer, and carrying out degassing for 30-44 seconds under the temperature of 2300 to 2700 DEG C; and putting to-be-detected titanium or titanium alloy together with a nickel basket into the graphite crucible, and carrying out oxygen-nitrogen-hydrogen combined determination. According to the method provided by the invention, hydrogen baseline value of an oxygen-nitrogen-hydrogen combined determination system can be effectively reduced, and the obtained hydrogen baseline value is stable, so that the precision and the accuracy of the hydrogen in the oxygen-nitrogen-hydrogen combined determination of the titanium or the titanium alloy can be improved.

Description

technical field [0001] The present invention relates to the technical field of testing hydrogen in titanium or titanium alloy materials, and more specifically, relates to a graphite crucible pretreatment method for joint measurement of oxygen, nitrogen and hydrogen, so as to improve the precision of hydrogen in the joint measurement of oxygen, nitrogen and hydrogen of titanium or titanium alloys and accuracy methods. Background technique [0002] The TCH600 Oxygen, Nitrogen and Hydrogen Analyzer produced by American LECO Company can realize the simultaneous determination of oxygen, nitrogen and hydrogen in titanium or titanium alloy. This method greatly improves the analysis efficiency of gas elements in titanium or titanium alloy. In the determination of oxygen, nitrogen and hydrogen, the blank value of the analytical system directly affects the lower limit of determination, precision and accuracy of the method. In order to obtain a low and stable blank value, the degassin...

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Problems solved by technology

[0003] In the actual application of the method, it is found that only the above degassing method cannot effectively reduce the hydrogen blank value in the graphite crucible. Even if the degassing time is increased to 60-75s, the graphite crucibles of some manufacturers cannot meet the requirements. Hydrogen blank value

Of course, it is possible to obtain a low and stable hydrogen blank value by using the long-term degassing method of the instrument electrode furnace, but this method will prolong the analysis time of a single sample and shorten the service life of the electrode furnace

Due to the high and inconsistent hydrogen blank value obtained by the existing method, the precision and accuracy of the test data of hydrogen in the joint measurement of oxygen, nitrogen and hydrogen in titanium are poor, which greatly hinders the analysis efficiency of the joint measurement method of oxygen, nitrogen and hydrogen in titanium

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