气相色谱-质谱联用法测定橡胶制品中多环芳烃（蒽）含量不确定度评定

目的对气相色谱-质谱联用仪法测定橡胶制品中多环芳烃（蒽）含量不确定度进行评定,确定影响不确定度的关键因素。方法依据《ZEK01.4-2008 GS认证过程中PAHs的测试和验证》,使用气相色谱-质谱联用仪法测定橡胶制品中多环芳烃（蒽）含量,并对结果的不确定度进行评定,分析影响测量不确定度的各个因素,对各个分量进行计算和合成。结果扩展不确定度U=5.7 mg/kg,置信概率95%。结论该实验的不确定度主要影响因素是曲线校准。     

分析测试经验介绍(243~248)原子荧光法测定金矿中砷和铋的不确定度评估

通过建立数学模型,分析了原子荧光法测定金矿中砷和铋的测量不确定度的影响因素,计算各影响因素的不确定度分量,并计算金矿中砷和铋的合成标准不确定度和扩展不确定度.结果表明:测量不确定度主要由样品制备过程和标准曲线拟合构成.金矿中砷的含量为18.398μg/g,其扩展不确定度为0.555 3μg/g(k=2),结果符合测试规范要求.铋的含量为0.359 3μg/g,扩展不确定度为0.441 1μg/g(k=2),铋的不确定度偏大,不符合测试规范要求,应通过降低铋标准溶液的浓度和减少待测液的稀释倍数来降低标准曲线拟合产生的不确定度.     

三维无溶剂含能Ag-MOF的制备、热分解动力学及爆炸性能

Solvent molecules can significantly reduce the heat of detonation and stability of energetic metal-organic framework (EMOF) materials, and the development of solvent-free EMOFs has become an effective strategy to prepare high-energy density materials. In this study, a solvent-free EMOF, [Ag₂(DTPZ)]_n (1) (N% = 32.58%), was synthesized by reacting a high-energy ligand, 2, 3-di(1H-tetrazol-5-yl)pyrazine (H₂DTPZ), with silver ions under hydrothermal conditions, and it was structurally characterized by elemental analysis, infrared spectroscopy, X-ray diffraction, and thermal analysis. In 1, the DTPZ²⁻ ligands that adopted a highly torsional configuration bridged the Ag⁺ ions in an octadentate coordination mode to form a three-dimensional framework (ρ = 2.812 g∙cm⁻³). The large steric effect and strong coordination ability of DTPZ²⁻ effectively prevented the solvent molecules from binding with the metal centers or occupying the voids of 1. Moreover, the strong π-π stacking interactions [centroid-centroid distance = 0.34461(1) nm] between the tetrazole rings in different DTPZ²⁻ ligands provided a high thermal stability to the framework (T_e = 619.1 K, T_p = 658.7 K). Thermal analysis showed that a one-step rapid weight loss with intense heat release primarily occurred during the decomposition of 1, suggesting potential energetic characteristics. Non-isothermal thermokinetic analyses (based on the Kissinger and Ozawa-Doyle methods) were performed using differential scanning calorimetry to obtain the thermoanalysis kinetic parameters of the thermodecomposition of 1 (E_a = 272.1 kJ·mol⁻¹, E_o = 268.9 kJ·mol⁻¹; lgA =19.67 s⁻¹). The related thermodynamic parameters [enthalpy of activation (ΔH^≠ = 266.9 kJ·mol⁻¹), entropy of activation (ΔS^≠ = 125.4 J·mol⁻¹·K⁻¹), free energy of activation (ΔG^≠ = 188.3 kJ·mol⁻¹)], critical temperature of thermal explosion (T_b = 607.1 K), and self-accelerating decomposition temperature (T_SADT = 595.8 K) of the decomposition reaction were also calculated based on the decomposition peak temperature and extrapolated onset temperature when the heating rate approached zero. The results revealed that 1 featured good thermal safety, and its decomposition was a non-spontaneous entropy-driven process. The standard molar enthalpy for the formation of 1 was calculated to be (2165.99 ± 0.81) kJ·mol⁻¹ based on its constant volume combustion energy determined using a precise rotating oxygen bomb calorimeter. Detonation and safety performance tests revealed that 1 was insensitive to impact and friction, and its heat of detonation (10.15 kJ·g⁻¹) was higher than that of common ammonium nitrate explosives, such as octogen (HMX), hexogene (RDX), and 2, 4, 6-trinitrotoluene (TNT), indicating that 1 is a promising high-energy and insensitive material.     

电动分离统一理论

在真空、气相和液相中实施线性电动分离,创造出了质谱、离子淌度谱、电泳和毛细管电泳等,但它们却未成体系,各自发展,各有理论,互不相关。该文从牛顿力学第二定律出发结合静电学理论,推导出了它们的统一运动方程,并由此推演出并简要讨论了上述各法自己的通用运动子方程和测量模式。这些方程不仅有利于系统化这些现存方法,也可用于推导和发现新型电动分离模式。     

依托度酸哌嗪盐的制备及其性能表征

制备了依托度酸和哌嗪的有机盐,并得到了其晶体结构。 结构解析结果表明,依托度酸羧基上的氢转移到哌嗪的氮原子上,N—H••••O氢键是维持结构稳定的主要分子间相互作用。 与原药相比,新合成的盐的本征溶出速率和平衡溶解度分别提高了2.1倍和4.8倍。 此外,新合成的盐具有良好的水合稳定性,在25 ℃,相对湿度95%的条件下暴露28 d未发生相变。作为依托度酸的第一个有机盐,该盐是依托度酸有前景的固体存在形式。     

焊接管结构的非线性推覆简化模型

有限元分析方法中,采用三维实体单元对焊接管结构进行离散是最为精确的建模方法,但对三维实体模型分析时会划分大量单元,导致计算时间冗长。工程中常把焊接管结构简化为刚架模型,即刚性连接的杆系系统。这种建模方式忽略了节点的局部柔度,过高地估计了整体结构的刚度,使计算结果偏于危险。为解决上述问题,在节点处引入虚拟梁单元,使其等效模拟节点的局部变形,还原支管真实长度。为了验证节点柔度对焊接管结构的影响,对典型的焊接管结构缩尺,进行了推覆试验。分别采用壳单元模型、刚架模型及引入虚拟梁单元的简化模型进行有限元模拟,并与试验结果对比分析。结果表明,刚架模型会过高的估计焊接管结构的刚度,而简化模型计算结果与壳模型、试验结果较为吻合。     

一种基于区间q-rung Orthopair模糊投影模型的多属性群决策方法

本文提出一种基于区间q-rung Orthopair模糊投影模型的多属性群决策方法。首先,定义一种度量向量间相关程度的区间q-rung Orthopair模糊投影,研究其性质。其次,基于区间q-rung Orthopair模糊环境中各备选方案与正负理想方案之间的投影关系,提出一种基于区间q-rung Orthopair模糊投影优化模型的TOPSIS多属性群决策方法。该方法能实现对备选方案的有效排序。最后,通过将该方法应用于为制造企业选择供应商的多属性群决策问题中,验证新方法的可行性和有效性。     

牛顿环实验测量结果不确定度的评定

详细分析了牛顿环实验中测量结果不确定度评定,由于干涉图样中各级暗环弦长左右读数的测量为不等精度测量,因此本文提出一种既简单又易操作的不确定度评定方法。     

丙烯腈-衣康酸基纳米纤维纱线的热稳定及碳化研究

碳纳米纤维主要以聚丙烯腈(PAN)作为前驱体,通过纺丝、热稳定、碳化等后处理工艺制备而得.但是,PAN基纳米纤维取向度低、致密性差,热稳定后环化度低,碳化后导电性差等缺点阻碍其在高性能碳纳米纤维领域的发展.因此,在PAN分子链中引入衣康酸(IA),通过溶液聚合法合成了P(AN-co-IA)共聚物并通过静电纺丝法制备了P...     

石墨炉原子吸收光谱法测定土壤中铅量的测量不确定度评定

通过石墨炉原子吸收光谱法对土壤中的铅量进行了测定,对影响测量结果的不确定度分量进行了量化的计算.从而得出影响铅量测量不确定度的主要因素是测量样品消解液中的铅的质量浓度引起的不确定度.