温度扰动对量热仪测量偏差的影响及修正研究

Study on Effect of Temperature Disturbances on Calorimeter Measurement Deviation and Its Correction

  • 摘要: 氚的计量是核材料衡算与核保障监督的关键环节,量热法通过测量衰变热功率实现氚的无损计量。等温差式量热仪在非理想条件下运行易产生相对测量偏差。为了探究温度扰动对等温差式量热仪测量偏差的影响规律,并建立测量偏差的修正模型,本文采用Box-Behnken响应面法设计实验,系统研究温度变化幅度、温度变化时长及样品功率对量热仪测量偏差的影响,建立二次多项式回归模型。结果表明:温度变化幅度是主导因素且呈现正效应,即幅度越大,偏差绝对值越大;样品功率呈现负效应,高功率样品因热容大、热惯性增强,可缓冲温度波动冲击,显著抑制偏差;时间效应与温度正效应耦合会加剧原始偏差。据此推导出温度-时间-功率三维耦合修正公式,可将实验研究范围内超过精度要求的量热仪测量偏差修正到1%以下。该修正方法为等温差式量热仪在非理想温度条件下的精确计量提供了有效工程修正手段,未来可通过积累量热数据以完善偏差修正公式库。

     

    Abstract: Tritium metrology is critical for nuclear material accountability and safeguards, as accurate knowledge of tritium inventory is fundamental to both proliferation resistance and operational safety. Calorimetry offers a nondestructive and direct approach for tritium quantification by measuring the decay heat power. Among various calorimeter configurations, the isothermal differential calorimeter is widely employed due to its stability and simplicity. However, under working conditions, ambient temperature fluctuations are unavoidable, and such non-ideal thermal environments introduce systematic measurement deviations. Therefore, understanding how temperature disturbances affect calorimetric performance and establishing a practical correction strategy are of significant importance for improving measurement reliability. Box-Behnken response surface methodology was selected to design a three-factor, three-level experiment. The independent variables investigated were temperature variation amplitude, temperature variation duration, and sample power. The response variable was the relative measurement deviation of the calorimeter. A quadratic polynomial regression model was then fitted to the experimental data to quantify the main effects, interaction effects, and quadratic effects of the three factors on the deviation. Model adequacy was verified through analysis of variance (ANOVA) and residual diagnostics. The results reveal that temperature variation amplitude is the most influential factor and exhibits a positive effect: As the amplitude increases, the absolute value of the measurement deviation increases. In contrast, sample power exerts a negative effect; Higher-power samples, which possess larger heat capacity and consequently greater thermal inertia, effectively dampen the impact of external temperature fluctuations and thus significantly reduce the deviation. The duration of temperature variation, while less influential individually, shows a notable coupling effect with amplitude: Longer duration combined with larger amplitude exacerbates the original deviation, indicating that the thermal history of the environment cannot be neglected. Based on these findings, a three-dimensional coupled correction formula incorporating temperature amplitude, duration, and sample power was derived. The formula takes the form of a polynomial function that directly maps the measured raw deviation to a corrected value. Validation experiments conducted within the same parameter space demonstrate that the correction method reduces all deviations that initially exceed the precision requirement to below 1%, meeting the typical accuracy threshold for tritium accounting. In conclusion, the proposed correction approach provides an effective and practical engineering solution for isothermal differential calorimeters operating under non-ideal temperature conditions. It requires no hardware modification and relies only on recording parameters during measurement. Future work will focus on expanding the correction formula library by accumulating more calorimetric data under diverse disturbance patterns, including cyclic and stepwise temperature changes, and extending the method to other calorimeter types. With further refinement, this strategy will enhance the traceability and accuracy of tritium calorimetry in routine safeguards.

     

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