Abstract:The influence of crucible on analysis results of oxygen, nitrogen and hydrogen in superalloy was investigated using four instruments. The experiments firstly started from the blank test. The oxygen blank of imported and domestic graphite crucible was stabilized at 0.0Xμg/g, while the nitrogen blank was stabilized at 0.Xμg/g, which could meet the analysis requirements of oxygen and nitrogen in superalloy. The quality of domestic graphite crucible reached the level of international crucible with similar type, and it could meet the basic requirements in the study. The results showed that the oxygen blank of graphite duplex crucible was lowest. The blank value of nitrogen was the same for graphite duplex crucible and single crucible. The blank value of hydrogen was lowest for quartz crucible. With the help of certified reference material (CRM, 502-863) for simultaneous determination of oxygen and nitrogen, the analysis difference of oxygen and nitrogen in three instruments was compared between graphite duplex crucible and single crucible. The results indicated that the analysis results of oxygen and nitrogen was lower for the duplex crucible compared to the single crucible when same internal calibration curve was used for calculation. If two corresponding calibration curves prepared separately for duplex crucible and single crucible were used for calculation, the analysis results of oxygen and nitrogen were basically consistent. In terms of analysis and detection for hydrogen, the graphite single crucible had serious data deviation, and it could not be used. The duplex crucible was applicable for the analysis of sample with high hydrogen content (not less than 0.6μg/g). For the analysis of ultralow hydrogen in steel CRM, only the result of quartz crucible was best. Based on the calibration curves and methods established using the existing steel CRMs, three types of crucible, and four instruments, the content of oxygen, nitrogen and hydrogen in superalloy sample was determined. There were more than 45 data points in each group. The results showed that the data of oxygen content in actual superalloy sample were most dispersed, while the determination results of nitrogen were relatively concentrated. The analysis results of hydrogen had great difference among different crucibles. The analysis data of build-in internal control sample of superalloy indicated that the determination results of oxygen and nitrogen by graphite single crucible were slightly higher than those obtained by graphite duplex crucible. Meanwhile, the difference among three instruments was very little. During the determination of hydrogen in superalloy, the interaction between graphite crucible and sample cause interference, so the determination results were higher than those obtained by quartz crucible. Particularly, the interference caused by graphite single crucible was higher than that of graphite duplex crucible, and was not suggested for use. The quartz crucible was the best choice for the analysis of ultralow hydrogen in superalloy. The abnormal data caused by crucible damage and bubbling could be timely discovered and removed by observation of crucible after use. And it was one of effective approaches to reduced the adverse effect of crucible.
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