固相萃取-气质联用法测定固体废物浸出液中的二硝基苯

建立了一种利用固相萃取法对固体废物浸出液(TCLP)中二硝基苯进行萃取,DB-5石英毛细管柱(30 m×0.25 mm×0.25μm)进行分离,质谱检测器检测二硝基苯的方法。方法在0.002 0~0.020 0 mg/L之间线性关系良好,二硝基苯三种同分异构体的检出限均为0.5μg/L,模拟样品加标回收率为93%~96%,RSD≤2%;实际固体废物样品测定的加标回收率为95%~98%。     

气相色谱-串联质谱法测定沉积物中多环芳烃

采用ASE法提取沉积物中16种多环芳烃,以固相萃取法净化提取液,用气相色谱-串联质谱法测定。通过优化测定条件,使方法在5.00μg/L~1 600μg/L范围内线性良好,方法检出限为0.15μg/kg~0.66μg/kg。空白石英砂的加标回收率为61.9%~121%,7次测定结果的RSD为2.6%~11.1%。     

Feasibility of honeycomb monolith supported sugar catalyst to produce biodiesel from palm fatty acid distillate (PFAD)

Carbon coated monolith was prepared by sucrose solution 65 wt.% via dip-coating method. Sulfonation of incomplete carbonized carbon coated monolith was carried out in order to synthesize solid acid catalyst. The textural structure characteristics of the solid acid catalyst demonstrated a low surface area and pore volume. Palm fatty acid distillate (PFAD), a by-product of palm oil refineries, was utilized as oil source in biodiesel production. The esterification reaction subjected to different reaction conditions was performed by using the sulfonated carbon coated monolith as heterogeneous catalyst. The sulfonation process had been performed by using vapour of concentrated H₂SO₄ that was much easier and efficient than liquid phase sulfonation. Total acidity value of carbon coated monolith was measured for unsulfonated sample (0.5 mmol/g) and sulfonated sample (4.2 mmol/g). The effect of methanol/oil ratio, catalyst amount and reaction time were examined. The maximum methyl ester content was 89% at the optimum condition, i.e. methanol/oil molar ratio (15:1), catalyst amount (2.5 wt.% with respect to PFAD), reaction time (240 min) and temperature 80 °C. The sugar catalyst supported on the honeycomb monolith showed comparable reactivity compared with the sugar catalyst powder. However, the catalyst reusability studies showed decrease in FFA% conversion from 95.3% to 68.8% after four cycles as well as the total acidity of catalyst dropped from the value 4.2 to 3.1 mmol/g during these cycles. This might be likely due to the leaching out of SO₃H group from the sulfonated carbon coated monolith surface. The leaching of active species reached a plateau state after fourth cycle.     

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。     

Effect of admixture of solid inertant on fire hazard of dust layers oriented at varying degrees of inclination

Unlike metallic dust layers, the layer flammability levels (LFL) of non-metallic dust layers exhibit a wide range from Class 1 (No self-sustained combustion) to Class 6 (explosive combustion). However, determinations of layer flammability have not considered the effect of inclination angle, thereby potentially underestimating fire hazard of combustible dust layers in many industrial situations. In this research, inclined dust layers showed greater fire hazard than did horizontally oriented dust layers. For example, LFL of wood dust jumped from class 3 to class 5 when layers were positioned with an incline. Flame spread rate of PMMA dust layers increased from 1.8 to 3.6 mm/s when the angle of inclination increased from 0 to 40°. Even small amounts of solid inertant significantly decreased surface layer fires. The required amount of inertant to completely inert layer fires was far less than that for smoldering layer fires or dust explosions.     

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.     

某基岩区工业固体废物填埋场地递进式场地环境调查实例

针对某基岩区简易封场后的固体废物填埋场,采用多层次、递进式调查策略,配合使用地球物理探测、直压式土壤快速取样、现场快速检测等技术,分3个阶段开展填埋场及其周边环境调查。第1阶段,调查地质环境特征,开展地球物理探测;第2阶段,调查填埋物、渗滤液主要组分及对周边积水、农田土壤、民用井水的污染情况;第3阶段,划定重点污染区域,开展土壤和地下水污染调查。调查结果显示,填埋区已发生明显渗漏,对邻近区域土壤、地下水及地表积水造成了一定污染,但未对周边农用地土壤、民用井水质等产生不利影响,总体处于可控范围。提出,通过削减污染源,切断污染物迁移、暴露途径,消除已有污染影响,长期跟踪监测等多项管控治理措施进行综合整治。     

A bayesian network-based safety assessment method for solid propellant granule-casting molding process

The safety of the solid propellant molding process is vital for the stable production of high-quality propellants. Failure events caused by abnormal parameters in the molding process may have catastrophic consequences. In this paper, a Bayesian network (BN) model is proposed to assess the safety of the solid propellant granule-casting molding process. Fault tree analysis (FTA) is developed to construct a causal link between process variables and process failures. Subsequently, expert experience and fuzzy set theory (FST) are used to obtain failure probabilities of the basic events (BEs). Based on the mapping rules, FTA provides BN with reliable prior knowledge and a network structure with interpretability. Finally, when new evidence is obtained, the probability is updated with the diagnostic reasoning capability of BN. The results of the sensitivity analysis and diagnostic inference were combined to identify key parameters in the granule-casting molding process, including curing temperature, vacuum degree, extrusion, calendering roll distance, length setting value, holding time, and polish time. The results of this paper can provide effective supporting information for managers to conduct process safety analysis.     

微波消解-火焰原子吸收分光光度法测定固体废物中的钡

采用微波消解法对固体废物浸出液样品进行前处理,采用乙炔-空气火焰原子吸收法测定钡的含量,检出限为2．04mg／L,加标回收率为94．5％,精密度为4．85％-6．81％。     

A 1-dodecanethiol-based phase transfer protocol for the highly efficient extraction of noble metal ions from aqueous phase

A 1-dodecanethiol-based phase-transfer protocol is developed for the extraction of noble metal ions from aqueous solution to a hydrocarbon phase, which calls for first mixing the aqueous metal ion solution with an ethanolic solution of 1-dodecanethiol, and then extracting the coordination compounds formed between noble metal ions and 1-dodecanethiol into a non-polar organic solvent. A number of characterization techniques, including inductively coupled plasma atomic emission spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis demonstrate that this protocol could be applied to extract a wide variety of noble metal ions from water to dichloromethane with an efficiency of >96%, and has high selectivity for the separation of the noble metal ions from other transition metals. It is therefore an attractive alternative for the extraction of noble metals from water, soil, or waste printed circuit boards.