固相膜萃取-气相色谱法测定地表水中有机氯农药研究

研究了固相膜萃取对地表水中有机氯农药(OCPs)物质的提取效果,并与液液提取法(LLE)进行比较.建立了固相膜萃取/气相色谱法检测地表水中20种有机氯农药的方法.结果表明:当萃取膜为HLB膜,洗脱液溶剂为丙酮和正己烷,萃取效果最理想,20种OCPs的回收率稳定在74.1%~94.3%之间,固相膜萃取法与传统液液提取法相比,既提高了萃取效率同时又减少了有机萃取溶剂的用量.该法检测实际样品时,同时加入2种内标指示剂对方法的性能进行了验证,2种内标示踪剂的回收率分别为71.6%~94.8%和69.9%~109.5%,样品中20种OCPs均未检出.     

高效液相色谱-电感耦合等离子体质谱联用测定生物样品中的有机汞

建立了酸提取-高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)测定生物样品中甲基汞、乙基汞、苯基汞等3种有机汞的分析方法。鱼肉和贝类样品经盐酸消解,苯萃取,硫代硫酸钠溶液反萃取后,采用醋酸铵/L-半胱氨酸缓冲盐及甲醇体系组成的流动相按一定比例进行梯度洗脱,经前处理的生物样品在液相色谱中经C18柱分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和苯基汞的浓度。3种有机汞化合物均在0.50~50.0μg/L范围内呈现良好的线性关系,线性相关系数(r)均大于0.9998。方法检出限为0.010~0.038mg/kg;3种有机汞样品加标的RSD均小于12.2%;两个水平的加标回收率在50.8~129%。     

基于放射性碳分析的多环芳烃源解析:技术进展和准确性评估

化石燃料燃烧和生物质燃烧是污染物多环芳烃(polycyclic aromatic hydrocarbon,PAHs)的两大来源.放射性碳(14C)分析近年用于评估这两类源对环境中PAHs的相对贡献.此方法基于化石燃料和生物质的14C含量差异,即化石燃料不含14C,而生物质的14C浓度有一个较稳定值.14C的自然丰度极低(约10-12),因此检测PAHs这样的痕量污染物的14C含量一度极具挑战.1990年代中期,加速器质谱的技术突破使得对环境样品PAHs的14C分析具有实用价值.要准确测出PAHs的14C含量,须先从化学成分复杂的环境样品中分离出高纯度的PAHs.制备气相色谱因其出色的分离能力而成为目前环境样品PAHs14C分析必备的工具.本文意在简介基于14C分析的PAHs源解析的基本原理、技术进展,以及评估该方法获得的PAHs源解析结果的准确性.     

An integrated EDIB model for probabilistic risk analysis of natural gas pipeline leakage accidents

Natural gas pipeline construction is developing rapidly worldwide to meet the needs of international and domestic energy transportation. Meanwhile, leakage accidents occur to natural gas pipelines frequently due to mechanical failure, personal operation errors, etc., and induce huge economic property loss, environmental damages, and even casualties. However, few models have been developed to describe the evolution process of natural gas pipeline leakage accidents (NGPLA) and assess their corresponding consequences and influencing factors quantitatively. Therefore, this study aims to propose a comprehensive risk analysis model, named EDIB (ET-DEMATEL-ISM-BN) model, which can be employed to analyze the accident evolution process of NGPLA and conduct probabilistic risk assessments of NGPLA with the consideration of multiple influencing factors. In the proposed integrated model, event tree analysis (ET) is employed to analyze the evolution process of NGPLA before the influencing factors of accident evolution can be identified with the help of accident reports. Then, the combination of DEMATEL (Decision-making Trial and Evaluation Laboratory) and ISM (Interpretative Structural Modeling) is used to determine the relationship among accident evolution events of NGPLA and obtain a hierarchical network, which can be employed to support the construction of a Bayesian network (BN) model. The prior conditional probabilities of the BN model were determined based on the data analysis of 773 accident reports or expert judgment with the help of the Dempster-Shafer evidence theory. Finally, the developed BN model was used to conduct accident evolution scenario analysis and influencing factor sensitivity analysis with respect to secondary accidents (fire, vapor cloud explosion, and asphyxia or poisoning). The results show that ignition is the most critical influencing factor leading to secondary accidents. The occurrence time and occurrence location of NGPLA mainly affect the efficiency of emergency response and further influence the accident consequence. Meanwhile, the weight ranking of economic loss, environmental influence, and casualties on social influence is determined with respect to NGPLAs.     

Impact of leakage location and downwind storage tank on the gas dispersion in a typical chemical tank storage area

Toxic gas leakage in a tank area can have catastrophic consequences. Storage tank leakage location (particularly for high leakage) and downwind storage tanks potentially influence gas diffusion in tank areas. In this study, we developed a numerical and experimental method to investigate the impact of a high leakage location and downwind storage tank on gas diffusion based on three (1.05H, 0.90H, and 0.77H, H was the tank height, 22m) leakage field experiments on the leeward side of storage tank, which have been not conducted before. The experiments revealed an unexpected phenomenon: the maximum ground concentration first decreased and then increased with increasing leakage height. The simulations illustrated that the differences in micrometeorological conditions caused the maximum ground concentration of gas emitted from the roof to be higher than that emitted from the tank wall near the storage tank height. The downwind storage tank 1) had little influence on the entire diffusion direction but altered the local diffusion pattern; 2) reduced the maximum ground concentration (∼18.7%) and the distance from the emission source (approximately a storage tank diameter); and 3) had strong influences on the concentration, velocity, turbulence, and pressure on the leeward side. The concentration negatively correlated with the velocity, pressure, and turbulence in the middle of the two storage tanks on wind centerline. Our results can improve understanding of gas dispersion in tank areas and provide references for mitigating loss and protecting lives during emergency response processes.     

Influence of sewage culvert cover plate thickness on dynamic response and damage of the cover plate under gas explosion

In order to address the risk of combustible gas explosions in sewage culverts, a numerical model was established using ANSYS/LS-DYNA software. The model consisted of a culvert and a cover plate, and was used to study the effect of cover plate thickness (ranging from 0.08 m to 0.12 m) on the dynamic response and damage of the structure under explosive loads. The results indicated that, during the loading negative pressure stage, the equivalent stress peak value of the central monitoring unit of the cover plate first increased and then decreased with increasing cover plate thickness. Additionally, the maximum principal stress peak value first decreased and then increased, while the maximum shear stress peak value first increased and then decreased. During the loading positive pressure stage, the maximum principal strain peak value of the monitoring unit decreased overall with increasing cover plate thickness. However, the equivalent plastic strain peak value initially increased and then decreased gradually. The equivalent strain indicated that plastic damage occurred in the cover plate. Beyond a thickness of 0.11 m, increasing the cover thickness did not appear to enhance its resistance to plastic damage. The damage analysis revealed that as cover plate thickness increased, the peak displacement and velocity of the monitoring unit continued to decrease, while the overall stability and explosive resistance of the cover plate increased. Additionally, the number of damaged fragments decreased. However, once the cover plate thickness reached 0.11 m, the bonding performance of the reinforced concrete structure had been fully developed, increasing the thickness of the cover plate no longer had a significant impact on the explosive resistance of the cover plate.     

Study on acceleration and suppression properties of coal gangue with different void fractions on gas explosion propagation

Gas explosion is one of the main disasters in coal mining. Plenty of coal gangue are generally distributed in the disaster areas in gob. Experiments were carried out to explore the propagation law of the gas explosion distributed by coal gangue. The variation characteristics of the overpressure, pressure rise rate, and flame shape with void fractions were analyzed. The results showed that the effect of the coal gangue on the explosion intensity changed from suppression to acceleration with the increase of void fraction, the flame front upstream blockage area changed from laminar state to turbulent divergent state, and a reverse flame was formed. When the void fraction of the coal gangue was 0.50–0.65, the maximum overpressure downstream of the blocked area were positively correlated with the void fraction and the critical suppression range was between 0.50 and 0.55. When the void fraction was lower than 0.50, the flame was quenched in the coal gangue, neither the flame nor the pressure could pass through the blocked area. It is helpful to guide the improvement of coal recovery process to avoid the expansion of the explosion impact in coalmine gob.     

超高效液相色谱-串联质谱法同时分析地下水中24种内分泌干扰物

建立了基于超高效液相色谱-串联质谱法同时测定地下水中9种雌激素、5种雄激素、3种肾上腺皮质激素、4种酚类和3种非甾类激素共24种内分泌干扰物的方法。在活化后的MCX固相萃取柱中加入水样,再加入pH=5的水溶液淋洗,随后用碱化乙腈(4.5%,体积分数)洗脱。收集洗脱液并用氮气吹至近干后,用甲醇定容。采用Poroshell 120 Bonus-RP色谱柱(2.7 μm,100 mm×2.1 mm),以0.1%氨水溶液-乙腈为流动相进行梯度洗脱,实现液相分离。质谱检测采用MRM模式进行采集,通过正负离子模式切换同时进行测定,使用内标法定量。检测结果显示,目标物在线性范围内,决定系数R²均大于0.995,方法检出限为0.05~2.00 ng/L,加标回收率为68.8%~108%。该方法灵敏度高、准确度好,具有较强的实用价值。     

气相色谱法测定室内空气中挥发性卤代烃

建立了活性炭吸附-溶剂解吸-气相色谱测定室内空气中7种挥发性卤代烃的分析方法。样品经活性炭采样管富集后,用二硫化碳解吸,Agilent HP-1色谱柱分离,使用带有电子捕获检测器的气相色谱仪测定,以保留时间定性,外标法定量。当采样体积为10 L时,方法检出限范围是0.03~0.18 g/m3,加标回收率在72%~114%之间,相对标准偏差小于15%。结果表明,该方法可以应用于室内空气中痕量挥发性卤代烃样品的检测分析。     

顶空气相色谱法测定水中甲醛、乙醛和丙烯醛

建立了顶空气相色谱法同时测定水中甲醛、乙醛、丙烯醛的方法。目标化合物连续测定9次的相对标准偏差分别为0.01,1.89,3.54;检出限分别为0.03μg/L,5.68μg/L,10.3μg/L,实际水样加标回收率在98%~101%。方法简便,快速,灵敏度高,基体干扰小。适用于地表水、地下水和工业废水中甲醛、乙醛、丙烯醛的同时、快速测定。