离子色谱法测定化工废水中有机醇胺类化合物

采用固相萃取-离子色谱法同时测定化工废水中乙醇胺、二乙醇胺、三乙醇胺、N-甲基二乙醇胺和N-丁基二乙醇胺等5种有机醇胺类化合物。通过试验,对固相萃取、离子色谱条件进行优化,优选C_(18)为固相萃取填料,使方法在1.10 mg/L～26.0 mg/L范围内线性良好,方法的检出限为0.72 mg/L～1.02 mg/L。废水样品3个质量浓度水平的加标回收率为84.0%～101%,测定6次结果的RSD为1.7%～12.0%。将该方法用于医药化工企业废水的测定,结果部分醇胺类化合物检出。     

沈阳市大气中PM2.5来源解析研究

通过2015年在沈阳市采集PM2.5样品及源类样品,分析样品的质量浓度和化学组成,用化学质量平衡(CMB)模型对该市PM2.5来源进行解析。结果表明:沈阳市大气中PM2.5浓度时空变化特征明显;各主要源类对沈阳市PM2.5的分担率依次为煤烟尘(28.03%)、二次无机离子(22.63%)、机动车尾气尘(17.27%)、城市扬尘(13.28%)、建筑尘(5.94%)、土壤风沙尘(5.82%)、道路尘(3.04%)、生物质燃烧尘(2.74%)和冶金尘(1.25%)。燃煤和机动车的有效控制既能降低本类源的贡献,也能降低二次无机离子,体现了多源类综合治理原则。     

Ultra trace simultaneous determination of 50 polycyclic aromatic hydrocarbons in biota using pMRM GC-MS/MS

Abstract

A saponification extraction method with gas chromatography pseudo-MRM (pMRM) mass spectrometry detection was developed for the determination of 50 total polycyclic aromatic hydrocarbons (TPAH50, a combination of parent and alkylated homologues) in biota. The method was aimed at monitoring and identification of potential TPAH contaminants in bitumen impacted environments. Alkylated PAHs were determined by multi-level, quantitative calibration using parent PAHs. The developed and thoroughly validated method required only one injection for TPAH50 analysis which represents significant saving of time and expensive authentic alkylated standards. The current method was tested with certified reference mussel tissue NIST 1974c and performed well. In a comparison study, the method reached a limit of quantitation (LOQ) for the TPAH50 between 0.1 and 0.2?ng g^?1, while the QuEChERs enhanced matrix removal – lipid (EMR) kit produced by Agilent showed an LOQ of 5–10?ng g^?1. The current method relied on response factors (RF) for the quantitation of alkylated PAHs determined against parent PAHs. These RFs were shown to be stable and consistent over the course of 1 year, during which over 200 routine environmental biota monitoring samples were analyzed. The environmental biota monitoring samples analyzed include muscle, carcass and liver, with an average total PAH50 concentration of 13, 90 and 135?ng g^?1, respectively. Results show significant differences in the distributions of 1 ringed, 2 ringed, 3 ringed, 4 ringed, and 5+ ringed TPAHs between the types of biota samples.     

QuEChERS-气相色谱法快速测定土壤中8种有机氯农药

建立QuEChERS-气相色谱法同时检测土壤中8种有机氯农药的方法,优化分散固相萃取剂用量。土壤样品通过分散固相萃取净化技术,氮吹浓缩后用正己烷定容,最后通过气相色谱测定。结果表明,在2.0~100μg/L质量浓度范围内呈线性,相关系数r为0.9895~0.9991。空白样品在0.5,5和20μg/kg加标浓度下的回收率为75.3%~92.3%,相对标准偏差为3.2%~5.6%(n=5),方法检出限为0.053~0.064μg/kg,测定下限为0.21~0.26μg/kg。该方法操作简单、结果准确、有机试剂用量少、分析成本低,适用于土壤中有机氯农药的残留检测与分析。     

Women executives and off-the-job misconduct by high-profile employees: A study of National Football League team organizations

The risk of off-the-job misconduct by high-profile employees is a serious concern of top management in professional sport organizations, media and entertainment companies, and public-facing entities in the government and education sectors. Yet there is little research on how to prevent or mitigate this form of misconduct in organizations. Utilizing upper echelons theory and the literature on demographic composition, we examine the relationship between the gender composition of executives of team organizations in a men's professional sport league and subsequent misconduct by players on those teams. Specifically, we employed multilevel and logistic regression analyses to unique data on U.S. National Football League team organizations, and we found that firms with a critical mass of women executives experienced fewer player arrests. No support was found for executive power as a moderator of this relationship. We discuss the implications of our findings for the demographic composition literature. We also offer guidance for preventing and managing off-the-job misconduct by high-profile employees.     

Optimization of gas detector placement considering scenario probability and detector reliability in oil refinery installation

Gas detection system is a critical layer of protection in process safety. Leak scenario probability and detector reliability are two key factors in the optimization of gas detector placement. However, they are easily neglected in previous studies, which may lead to an inaccurate evaluation of the optimization solutions. In this study, a stochastic programming (SP) optimization method is proposed considering these two factors. In order to quantitatively represent the probability of leak scenarios, a complete accident scenario set (CASS) is built combining leak sources and wind fields. Then, the computational fluid dynamics (CFD) method is adopted for consequence modeling of gas dispersion. The Markov model is developed to predict the detector reliability. With the objective of minimal cumulative detection time (MCDT), the SP formulation considering scenario probability and detector reliability (MCDT-SPR) is proposed. By introducing the particle swarm optimization (PSO) algorithm, the optimization formulations can be solved. A case study is investigated on a diesel hydrogenation refining unit. Results validate this approach is promising to improve the detection efficiency. This method is more practical and matching with the actual industrial environment, where the leak scenarios and the detector reliability can change dynamically in real process setting.     

On the non-monotonic wind influence on flammable gas cloud from CFD simulations for hazardous area classification

Hazardous areas are defined as a result of a variety of variables as storage temperature, pressure, leak orifice size, physical properties of flammable substance, and wind characteristics. The potential formation of an explosive atmosphere must be accurately assessed to ensure process safety. Therefore, computational fluid dynamics (CFD) arises as an important tool for accurate predictions as recommended by the international standard IEC 60079-10-1 (2015). This study aims to analyze the influence of wind velocity magnitude and direction on the hazardous area classification. The authors evaluated the extent and volume for methane, propane, and hydrogen leakages from a CFD model. For each flammable gas, the wind velocity magnitude and direction were regularly varied. The outcomes show that the behavior of the plume size as the wind varies mainly depends on the gas concentration. Counter-flow wind directions lead to zero relative velocity closer to the release point, which concentrates the gas, and wind in the release direction promotes a higher dilution of the gas cloud increasing the hazardous extent while decreases the volume. As a consequence, the wind also influences the zone type, which was accurately predicted from CFD simulations and significant differences were found when compared to the standard analyses. These differences are, to some extent, related to the consideration of wind velocity effects on the gas jet release.     

基质固相分散-快速溶剂萃取-GC/MS法同时测定土壤中有机氯农药和多环芳烃

建立了基质固相分散-ASE提取-GC/MS法同时测定土壤中8种有机氯农药和16种多环芳烃的方法。对方法的线性、检出限、精密度、回收率及土壤质控样品进行了分析,结果表明,8种有机氯农药和16种多环芳烃线性良好,相关系数为0.997 5～0.999 8,方法检出限为0.39～1.57μg/kg,空白加标样品的相对标准偏差小于20%,实际土壤样品加标回收率为60.6%～125%,土壤质控样品结果均在范围内。该方法能够满足土壤中8种有机氯农药和16种多环芳烃的检测要求。     

固定污染源非甲烷总烃自动连续监测系统比对监测

对非甲烷总烃自动连续监测系统进行示值误差、响应时间、零点漂移和量程漂移等性能测试,对非甲烷总烃便携式分析仪进行检出限、精密度、准确度等性能测试。性能测试满足相关要求后同时利用便携式催化氧化-氢火焰离子化检测器法(催化氧化-FID)、便携式气相色谱-氢火焰离子化检测器法(GC-FID)和实验室气相色谱-氢火焰离子化检测器法(GC-FID)对固定污染源非甲烷总烃自动连续监测系统进行现场比对测试。测试结果表明,在工况变动较大的情况下,便携式FID法与实验室GC-FID法测试结果相对误差为19. 6%～35. 1%,具有很好的可比性。以实验室GC-FID法为参比方法时,自动连续监测系统相对准确度为64. 1%,不满足《固定污染源废气非甲烷总烃连续监测系统技术要求及检测方法》(HJ 1013—2018)的要求。以便携式FID为参比方法时,自动连续监测系统相对准确度分别为28. 6%和35. 3%,相对《固定污染源废气总烃、甲烷和非甲烷总烃的测定气相色谱法》(HJ 38—2017)方法一致性更好,均能满足《HJ 1013—2018》的要求。提出,应推进便携式方法在自动连续监测系统验收和质控比对中的应用。     

离子色谱-衍生-分光光度法同时测定水中三价铬和六价铬

本文建立了离子色谱法同时测定水中三价铬和六价铬的方法。样品中的三价铬经柱前衍生后,泵入分析柱,与样品中的六价铬分离,分离后的样品经在线柱后衍生,流入可变波长检测器,分别在365 nm和540 nm检测。利用正交实验找出最佳分析条件:水浴加热2 min,加热温度80℃,柱后衍生液流速1.1 ml/min。方法在10 min内完成水中三价铬和六价铬分析,三价铬和六价铬线性范围分别为0.05～10 mg/L和0.005～1 mg/L,方法检出限低,分别为18.1μg/L和0.267μg/L,精密度分别为1.16%(0.4 mg/L Cr3+,n=7)和3.07%(0.08 mg/L Cr6+,n=7),样品分析时的加标回收率在96%～102%之间。