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High‐Precision Density Measurements of Energetic Materials for Quality Assessment
Propellants, Explosives, Pyrotechnics ( IF 1.7 ) Pub Date : 2021-02-05 , DOI: 10.1002/prep.202000272
Dirk Herrmannsdörfer 1 , Thomas M. Klapötke 2
Affiliation  

Even though helium pycnometry is considered a very precise method of density determination, its use to analyse factors influencing crystal quality (e. g. solvent inclusions, amorphous states, crystal defects…) is limited due to the unknown inherent accuracy of the method. Previous studies have attempted to identify the best possible accuracy of helium pycnometry. However, no robust method has been proposed to validate even the precision obtained. This means that the often occurring, seemingly random density deviations have never been satisfactorily explained. In this study the influencing factors on density measurements of the CL‐20/HMX cocrystal and phase stabilised ammonium nitrate carried out with an AccuPyc 1340 TEC were quantified and a robust method of data analysis was developed to judge with certainty the quality and significance of the data obtained. This study shows that statistical tests such as the t‐test and ANOVA cannot be utilised to differentiate between samples or repeat measurements, even though the density data points exhibit a normal distribution. By utilising confidence intervals and quantifying the three major sources of error (sampling error, change in barometric pressure during the measurement, and weight in error), a repeatability of 0.015 % was achieved and a method was developed that enables differentiation between samples with a certainty as good as 0.05 %.

中文翻译:

含能材料的高精度密度测量,以进行质量评估

尽管氦比重瓶法被认为是非常精确的密度测定方法,但由于该方法固有的未知性,其用于分析影响晶体质量的因素(例如溶剂夹杂物,非晶态,晶体缺陷……)的方法仍然受到限制。先前的研究试图确定氦比重瓶法的最佳精度。但是,还没有提出鲁棒的方法来验证所获得的精度。这意味着从未令人满意地解释了经常发生的看似随机的密度偏差。在这项研究中,量化了使用AccuPyc 1340 TEC进行CL-20 / HMX共结晶和相稳定的硝酸铵密度测量的影响因素,并开发了一种可靠的数据分析方法来确定其质量和意义。获得的数据。这项研究表明,即使密度数据点呈正态分布,也不能利用t检验和ANOVA之类的统计检验来区分样本或重复测量。通过利用置信区间并量化三个主要误差源(采样误差,测量过程中的大气压变化和误差重量),可重复性达到0.015%,并且开发了一种方法,可以确定样品之间的差异高达0.05%。这项研究表明,即使密度数据点呈正态分布,也不能利用t检验和ANOVA之类的统计检验来区分样本或重复测量。通过使用置信区间并量化三个主要误差源(采样误差,测量过程中的大气压变化和误差重量),可重复性达到0.015%,并且开发了一种方法,可以确定样品之间的差异高达0.05%。这项研究表明,即使密度数据点呈正态分布,也不能利用t检验和ANOVA之类的统计检验来区分样本或重复测量。通过使用置信区间并量化三个主要误差源(采样误差,测量过程中的大气压变化和误差重量),可重复性达到0.015%,并且开发了一种方法,可以确定样品之间的差异高达0.05%。
更新日期:2021-03-04
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