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%。     

煤与瓦斯共采在错层位巷道布置中的机理研究及应用构想

为了完善现有煤与瓦斯共采技术，创新煤与瓦斯共采方法，对错层位巷道布置下的煤与瓦斯共采系统展开研究，利用相似模拟试验，分析错层位巷道布置覆岩运动情况，预测其开采围岩裂隙发育和瓦斯运移形式，提出了创新煤与瓦斯共采技术构想。研究结果表明:采空区覆岩三带高度随接续工作面的增加而增大，相邻采空区垮落矸石压实区呈现“O-L-O”形变化，多个相邻采空区覆岩出现大“O”形圈裂隙带；相邻采空区内瓦斯可实现相互运移，大“O”形圈裂隙带内赋存大量瓦斯气体；研究提出了地面钻井抽采瓦斯、走向高位瓦斯抽采巷和外错尾巷穿层钻孔3种煤与瓦斯共采技术，比传统巷道布置情况下的煤与瓦斯共采技术在安全、经济等方面更具优势。     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

硬质聚氨酯泡沫和组合聚醚中消耗臭氧层物质的便携式GC-MS测定方法

建立了便携式顶空/气相色谱-质谱法测定硬质聚氨酯泡沫和组合聚醚中一氟三氯甲烷（CFC-11）、二氟二氯甲烷（CFC-12）、二氟一氯甲烷（HCFC-22）及一氟二氯乙烷（HCFC-141b）的定性分析方法，系统考察了色谱柱、顶空体系、顶空温度和顶空时间对测定结果的影响。结果表明，DB-WAX色谱柱对目标物质的分离效果最好，顶空温度为50℃、顶空时间为10 min条件下，目标物质的检测灵敏度最高。在优化条件下，硬质聚氨酯泡沫取样体积为1 cm³时，4种目标物的方法检出限为0.6~0.8 μg；组合聚醚取样量为10 mg时，4种目标物的方法检出限为0.5~0.6 μg。该方法具有较高的灵敏度，定性准确，适用于实际样品的现场快速定性分析。     

固相萃取-超高效液相色谱/三重四极杆质谱法同时测定地表水中8种亚硝胺类化合物

建立了固相萃取（SPE）-超高效液相色谱/三重四极杆串联质谱（UPLC-MS/MS）同时测定地表水中8种亚硝胺类化合物的方法。水样中目标物经椰壳活性炭固相萃取小柱吸附富集，小柱经氮气吹干后采用二氯甲烷洗脱。待测样品采用Atlantis T₃柱，以水-甲醇作为流动相进行梯度洗脱，大气压力化学电离源（APCI）正离子模式多反应监测方式（MRM）进行检测，内标法定量分析。8种目标物在相关线性范围内线性良好(r≥0.9950)，地表水加标回收率为55.4%~90.4%，相对标准偏差为3.1%~14.3%，方法检出限为1.1 ~1.8 ng/L。本方法准确度和灵敏度高，适用于快速测定地表水中8种亚硝胺类化合物含量。     

基于数字信息化的消防呼吸气瓶检验管理系统研究与开发

为解决碳纤维缠绕式消防呼吸气瓶检验中因单机作业而存在的检验效率低、检验质量差、受人为因素影响的问题，研究开发基于数字信息化的碳纤维缠绕式消防呼吸气瓶检验管理系统，该检验系统包括消防呼吸气瓶数据库、OA系统、呼吸气瓶检验软件和手机APP。利用二维码技术和计算机网络，实现呼吸气瓶数据库、检验软件、OA约检和报告审核审批系统、手机APP的数据传输。结果表明:该检验管理系统实现了呼吸气瓶检验的无纸化、过程的可追溯性、检验结果的防伪性等功能，其对于碳纤维缠绕式消防呼吸气瓶检验具有较强的适用性和可行性。     

肥煤自燃全过程热动力学特征参数研究

实验测定了林西矿肥煤样品30~900℃煤自燃全过程热动力学特征参数,得出:TG/DTG曲线显示煤样DTG初始临界温度45℃,干裂温度122℃,活性温度195℃,增速温度265℃,质量极大值温度342℃,着火温度465℃,最大热失重速率温度515℃和燃尽温度690℃;DSC曲线显示,煤样初始放热温度60℃、最大热释放速率温度511℃。结合TG-DTG-DSC曲线综合分析可知,煤温达到510℃左右时煤样反应最剧烈。由煤自燃标志气体测定实验系统得出:煤温130℃后CO,CO 2释放量迅速增加,210℃增加速度下降;CH 4,C 2 H 6含量变化具有规律性且两者变化相近;C 2 H 4出现温度为130℃;C 2 H 4/C 2 H 6比值在190~350℃有较强的规律性,呈上升趋势且上升速度较快;350℃之后,CH 4,C 2 H 6,C 2 H 4体积分数均开始急剧增大;C 2 H 4/CO与C 2 H 4/CO 2变化趋势大致相同,在130~350℃时缓慢增长,达到350℃后比值呈指数形式上升。经拟合曲线,得到活化能的3个突变点温度:70,180,220℃,其中180℃与交叉点温度相吻合。通过以上研究,得到了肥煤自燃全过程的热力学特征参数,为实际生产中防治煤自燃提供了理论依据。     

液氮泡沫发生器内流动特性研究

低温液氮与泡沫混合液直接接触产生氮气泡沫是一种新型的掺混形式,利用液氮高汽化比的特点,搭建液氮泡沫可视化实验装置,进行氮气-水两相流及液氮泡沫流动特性的研究。结果表明,液氮相变产生大量氮气,其与泡沫液混合产生泡沫,温度有所回升,最终趋于泡沫混合液温度;管路沿程压降较小;液氮射流破碎及流动过程可分为6个区域:低温液氮区、向上循环翻滚区、滞留区、泡沫与泡沫混合液混合区、致密泡沫区、泡沫混合液区。流体向下游流动过程中持续发泡;为防止管路结冰,需合理控制泡沫混合液与液氮流量。     

Experimental research of LNG accidental underwater release and combustion behavior

Evaluating potential hazards caused by accidental LNG release from underwater pipelines or vessels is a significant consideration in marine transportation safety. The aim of this study was to capture the dynamic behavior of LNG jet released under water and to analyze its vapor dispersion characteristics and combustion characteristics on the water surface during different release scenarios. Controlled experiments were conducted where LNG was jet released from a cryogenic storage tank. The dynamic process of LNG being jet released from orifices of different sizes and shapes, as well as the rising plume structure, were captured by a high-speed camera. The leakage flow rate and pipeline pressure were recorded by a flow meter and pressure gauge, respectively. The concentration distribution that emanated from the water surface was measured utilizing methane sensors in different positions with various wind speeds. The flame combustion characteristics of LNG vapor clouds, which immediately ignited upon the enclosed water tank, were also recorded. Additionally, the mass burning rate of the flame on the water surface was evaluated, and a new correlation between the ratio of flame length and width was established. The results indicated a large dimensionless heat release rate (Q*) and a continuous release flow rate in a limited burning area. This study could provide greater understanding of the mechanisms of LNG release and combustion behavior under water.