温度交变下液态乙烷回气管线热应力数值计算与现场测试*

为解决低温交变载荷下液态乙烷回气管线面临的安全问题,采用有限元法和现场试验研究管线在低温交变载荷下无裂纹和含轴向裂纹管线的热应力分布。结果表明:管内温度沿周向和轴向分布具有较大的不均匀性,内外壁温度分布趋势基本相似;随着计算时间的延长,管线整体热应力先增大再减小;卸压、温度回升过程中,管内温差逐渐减小,热应力逐渐减小;裂纹处的热应力大于远离裂纹及无裂纹处的热应力;对管线热应力变化进行现场监测,试验数据与仿真结果吻合。研究结果可为低温情况下液态乙烷回气管线的方案设计提供参考和指导。     

液体推进剂职业中毒风险评价及防护对策研究

本文以某发射场为例,通过主要危险源辨识、作业单元划分、现场调查和监测统计,利用风险指数评估法对液体推进剂职业中毒风险进行量化评价,结果表明:液体推进剂作业存在极度和高度职业中毒风险,发射场液体推进剂作业职业中度风险主要来源于液体推进剂及氮气;液体推进剂设备维修、应急救援及进罐作业存在极度职业中毒风险,转注/加注、取样为高度风险,化验及"三废"处理属于中度风险。根据评价结果并借鉴以往事故经验教训,指出职业中毒伤害与工程控制、个体防护措施和安全意识密切相关,不使用或不能正确使用呼吸防护装备是引发职业中毒的主要原因,并提出针对性的防护措施建议。     

蒙德法在火电厂液氨储罐评价单元的应用

火电厂液氨储罐单元存在大量高纯度的液氨,一旦发生火灾、爆炸,后果极其严重。为了研究液氨储罐的火灾爆炸危险性及毒性,在对火电厂液氨储罐危险性辨识的基础上,依据液氨储罐单元的主要参数,运用蒙德法分别确定评价中需要的各种危险性系数,从而进行各项指标计算,查询危险性等级表,将各项指标进行等级划分,结论表明各项危险等级都很高。在得出结论基础上,进行安全措施补偿评价,补偿后的各种危险等级均降低,可见采取补偿措施后能够一定程度的降低火灾、爆炸、毒性的危险性,防止事故的发生。     

高效液相色谱-串联质谱法同时检测地表水中13种药物及个人护理品

采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调p H值至7.0左右,过固相萃取小柱进行富集,用14 m L甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/m L)和58.0%~107.8%(加标水平50 ng/m L),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。     

基于ACF-AMDF的气井环空液面回波特征提取方法

为了精确有效地提取声波法检测气井环空液位的回波周期，在分析环空中测试波的传播特征及基音周期检测的基础上，提出1种基于检测信号短时自相关函数(ACF)及平均幅度差函数(AMDF)的液面回波周期提取方法；利用自主搭建的室内模拟实验系统开展了不同初始环空压力下环空液位检测实验；对检测信号进行中心削波处理并计算ACF/AMDF，提取出液面回波周期并与理论计算值对比分析；同时分析了现场环空液位检测信号，提取其回波周期。研究结果表明:提出的新方法能有效地用于提取环空液面回波周期；室内实验中，该方法最大误差绝对值为1.54%；该方法能够有效抑制液面回波信号中的随机噪声及接箍反射波等，处理后的信号曲线在回波周期处峰值更加突出、集中，而在其他位置更加平滑，提高了对液面回波周期特征的辨识能力。     

Pressurized liquid extraction of six tetracyclines from agricultural soils

Veterinary antibiotics used in agriculture can be introduced into the environment through land application of animal manure, accumulating in soils and groundwaters and posing a significant risk to human health and animal well-being. As the analysis of tetracyclines in soil is challenging due to their strong interaction with soil minerals and organic carbon, the objective of this study was to develop a reliable and reproducible method for quantitative analysis of chlortetracycline and oxytetracycline, and their respective metabolites in soils. A method based on pressurized liquid extraction (PLE) with in-cell clean-up was developed for the extraction of chlortetracycline and oxytetracycline and four likely metabolites from a set of four soils. Optimized conditions included a cell size of 22?mL, soil loading of 5?g, pH of 8.0, methanol:water ratio of 3:1, 50?°C, and two cycles. Soil extracts were analysed by high-performance liquid chromatography (HPLC) coupled with ion trap mass spectrometry (MS). Recoveries of seven tetracyclines from soil ranged from 41% to 110%. The limits of detection for tetracyclines were 0.08–0.3 µg g^?1 soil, and intra- and inter-day variation ranged from 0.12–0.34%. The proposed PLE method is suitable for quantification of tetracyclines in agricultural soils at typical concentrations expected in contaminated environments.     

水环境中26种类固醇激素的分析方法研究

建立了固相萃取-超高效液相-串联质谱法同时测定水环境中26种类固醇激素的分析方法。明确了取样体积为500 m L,Cleanert PEP为富集柱,乙酸乙酯为洗脱剂,甲醇为溶剂进行提取操作。选择了正离子模式,以0. 1%甲酸/甲醇-水为流动相,负离子模式以0. 1%氨水/乙腈-水为流动相,试样经AcquityTMUPLC BEH C18色谱柱分离后,选用质谱检测模式进行定性、定量分析。通过方法验证,26种类固醇激素的方法检出限为0. 3～1. 5 ng/L,测定下限为1. 2～6. 0 ng/L,代表性样品测定结果的相对标准偏差为2. 6%～13. 7%(n=6),加标回收率为71. 2%～121%。该方法操作便捷,灵敏度高,精密度和准确度良好,可适用于水环境中多种痕量、超痕量类固醇激素的定性定量分析。     

高效液相色谱-二极管阵列检测器测定邻苯二甲酸酯色谱条件优化

采用高效液相色谱-二极管阵列检测器对6种PAEs类物质进行测定,并对梯度洗脱条件、流速、检测波长等影响化合物色谱响应的关键参数进行优化。综合考虑样品测试效率、分析精度、实际样品中存在杂质干扰等因素,确定以乙腈-水为流动相进行梯度洗脱,洗脱0~11 min流动相乙腈-水梯度比例为50∶50,11 min后流动相调整为100%乙腈,各化合物均能完全分离;色谱分析流速为0.8 m L/min;PAEs的最佳吸收波长为225 nm。在优化的色谱条件下,6种PAEs的线性良好,相关系数均大于0.999 8,仪器检出限为0.08~0.12 mg/L,保留时间、峰面积的相对标准偏差分别为0.02%~0.60%、0.13%~0.86%。方法灵敏度较高,适合土壤等邻苯二甲酸酯含量较高基质样品的快速分析。     

Experimental investigation of the lower flammability limit of volatile liquid fuel-aluminum powder mixtures in air

Aluminum powder was always chosen as an additive to improve the explosive performance. In this work, experiments were performed to investigate the lower flammability limit (LFL) of volatile liquid fuel-aluminum powder mixtures using a 20 L closed spherical stainless steel vessel at a temperature of 20 °C (293 K) and 40 °C (313 K). The volatile liquid fuels tested in the work were diethyl ether (DEE), epoxypropane (PO), n-pentane and n-hexane. DEE, PO and n-pentane are in the liquid phase at room temperature and can easily transition to the gas phase at 40 °C (313 K). Through a series of experiments carried out, it was found that the change in phase would affect the interaction between the components. Aluminum powder always has an inhibitory effect on the flammability of the mixtures when it is mixed with gas-phase fuels. The inhibition effect was most obvious when the aluminum powder concentration reached 200 g/m³. While the interaction between aluminum powder and liquid-phase volatile fuels was promotion and was influenced by the component proportion and the type of the volatile fuels.     

Morphological characteristics of flashing jet throughout superheated liquid release

Many release problems involve two-phase releases of hazardous materials of superheated liquids with high energy into the atmosphere. Such accidents are accompanied by violent phase transition and form catastrophic flashing jets. In this work, experimental and theoretical analyses were conducted to investigate dynamic characteristics of flashing jet morphology and their dependence on pressure-decay dynamics under different storage pressures, superheats, and nozzle diameters. Flashing jet morphology and angle throughout two-phase releases were captured by a high-speed camera, and the corresponding source pressure in the superheated liquid tank was measured simultaneously. Results show that three typical phases, expansion, stabilization, and decay, are characterized throughout two-phase release based on the evolution of flashing jet morphology. The jet initially expands gradually due to the enhancement of phase transition intensity, and then keeps stable when the intensity reaches its maximum, and terminally decays rapidly due to the depletion of superheated liquid. Phase transition intensity at the nozzle exit is mainly controlled by the pressure-decay dynamics. Bubbles nucleation inception sites gradually move upstream of the nozzle during the pressure decay process increasing the phase transition intensity. The increase of storage pressure, superheat and nozzle diameter promotes the mechanical and thermodynamic effects on the jet breakup. The significant increase of mechanical and thermodynamic effects effectively accelerates droplets evaporation and further affects flashing jet morphology.