Journal of Loss Prevention in the Process Industries ( IF 3.6 ) Pub Date : 2023-06-26 , DOI: 10.1016/j.jlp.2023.105130 Ye-Cheng Liu , Jun-Cheng Jiang , Yan Tang , Zhi-Xiang Xing , Juan Zhai , Chi-Min Shu , An-Chi Huang
Analytical reagents identify and manage metal pollution, a major environmental issue. Regrettably, these compounds' safety concerns, especially when heated, have been neglected. This research examines the thermal hazard of the extremely reactive analytical reagent styphnic acid. Differential scanning calorimetry, thermogravimetric analysis, and accelerating rate calorimetry examined styphnic acid's thermodynamics. Thermogravimetric analysis showed weight loss reactions starting at 127 °C and peaking at 208 °C. Differential scanning calorimetry showed an endothermic peak at 176 °C. The accelerating rate calorimetry test showed that styphnic acid self-accelerates at 237 °C after 196.5 °C. Kissinger, Ozawa-Flynn-Wall, and Kissinger-Akahira-Sunose thermokinetic models calculated apparent activation energy from 131.677 to 155.718 kJ/mol. A nonlinear regression analysis showed that styphnic acid undergoes a two-step autocatalytic reaction during heat degradation. Thermal safety was assessed by measuring time to conversion limit, maximum rate, total energy release, self-accelerating decomposition temperature, and adiabatic temperature rise. Styphnic acid is less stable at higher temperatures and its thermal hazards depend on heating rate. The computed SADT was 109.04 °C, with alarm and control temperatures of 104.04 and 99.04 °C, respectively. The risk matrix analysis based on Tad and TMRad suggests reducing thermal instability. This study on styphnic acid's thermal risks and safe storage and transit during analytical applications is beneficial.
中文翻译:
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高能芪酸分析试剂在量热分析中的实验危险风险调查
分析试剂可识别和管理金属污染,这是一个主要的环境问题。遗憾的是,这些化合物的安全问题,尤其是加热时的安全问题,却被忽视了。这项研究研究了极具反应性的分析试剂斯蒂夫酸的热危害。差示扫描量热法、热重分析和加速量热法检查了斯蒂芬酸的热力学。热重分析显示失重反应在 127 °C 开始,在 208 °C 达到峰值。差示扫描量热法显示吸热峰176℃。加速量热测试表明,芪酸在196.5℃后在237℃自加速。Kissinger、Ozawa-Flynn-Wall 和 Kissinger-Akahira-Sunose 热动力学模型计算出的表观活化能为 131.677 至 155.718 kJ/mol。非线性回归分析表明,斯蒂芬酸在热降解过程中经历了两步自催化反应。通过测量达到转化极限的时间、最大速率、总能量释放、自加速分解温度和绝热温升来评估热安全性。芪酸在较高温度下稳定性较差,其热危害取决于加热速率。计算得出的 SADT 为 109.04 °C,报警温度和控制温度分别为 104.04 °C 和 99.04 °C。这基于T ad和TMR ad的风险矩阵分析表明可以降低热不稳定性。这项关于苯乙烯酸在分析应用过程中的热风险和安全储存和运输的研究是有益的。