Determination of cobalt by air-assisted liquid–liquid microextraction

Abstract

A rapid and selective technique for extraction, preconcentration and determination of trace amounts of cobalt in water and pharmaceutical samples by air-assisted liquid–liquid microextraction combined with flame atomic absorption spectrometry is proposed. 1-Nitroso-2-naphthol is used as a complexing agent and 1-octanol as an extraction solvent. Parameters relevant for analytical effectivity, i.e. pH of sample solution, concentration of complexing agent, volume of extraction solvent, and number of extraction cycles are optimized using a Box–Behnken design. At optimum conditions, a dynamic linear range of 5–600?µg L^?1 is obtained, with a limit of detection of 1.2?µg L^?1. The method is used for determination of Co(II) in environmental water and pharmaceutical samples.     

Hazardous halogenated substances formed during combustion processes

The results of the emissions from combustion processes and/or from fire accidents show the risk to man and his environment and thus the need for strict legislation and critical analysis of unwanted compounds. These substances or their thermolysis products are often due to incomplete combustion or may result from the interaction of various substances.

In the following we report the formation of octachlorostyrene (OCS) and of high‐toxic substances such as polybrominated dioxins (PBrDD's), dibenzofurans (PBrDF's) by the combustion.

In order to determine a possible source of the non‐manufactured compound OCS, we conducted several model experiments in a combustion chamber at various temperatures from 400 °C to 800 °C. The thermolysis of chlorinated solvents like chloroform or of chlorinated aromatice like pentachlorobenzene produced—among other chlorinated substances—OCS as one of the major products.

Analogous combustion experiments with polyester plastics containing decabromodiphenylether as flame retardant and antimony trioxide as Synergist led to PBrDD's and PBrDF's. Here antimony trioxide seems to play an important role because in absence of this oxide, PBrDD's and PBrDF's were not found in our experimental conditions.     

水体和甘蓝及土壤中毒死蜱残留检测方法

研究运用不同的样品前处理方式,在装配火焰光度检测器的气相色谱(GC-FPD)上检测,建立了有机磷杀虫剂毒死蜱在水样、土壤和甘蓝中的残留测定方法.研究表明,不同样品中的毒死蜱残留采用本文中介绍的前处理方法是可行的,用石油醚盐析提取和净化水样中毒死蜱,采用丙酮振荡提取甘蓝中毒死蜱,选用索氏提取法提取土壤中毒死蜱,并经液液分配净化后,采用OV-101大口径毛细管柱(30 m×0.53 mm×1.0μm),在装配火焰光度检测器(FPD和磷滤光片)的气相色谱上测定.该分析方法下,毒死蜱的保留时间为1.74 min,线性范围在1.0×10-11—1.0×10-8g之间,其线性相关系数为0.9998,最小检出量为2.0×10-12g.在设定的较低添加浓度的条件下,毒死蜱在水样、土壤与甘蓝上的添加回收率为80%—120%,变异系数均小于5%.该分析方法灵敏、准确、操作简便,适合水样、甘蓝和土壤中低浓度毒死蜱的残留检测.     

溴代阻燃剂在土壤中的迁移转化研究进展

BFRs（溴代阻燃剂）是一种重要的持久性有机污染物,各种传统和新型的BFRs（PBDEs、TBBPA、DBDPE、BTBPE等）在全球环境中被广泛检出,其持久性、生物蓄积性以及对环境和人类健康的潜在毒性引起了人们的极大关注.在归纳和总结国内外关于BFRs在土壤中的迁移转化行为规律研究动态的基础上,重点讨论了吸附/解吸、光降解的机理和影响因素以及厌氧、好氧微生物降解和植物代谢的特点和降解途径.结果表明:吸附/解吸是BFRs在土壤中迁移转化的关键过程,土壤有机质含量和pH是影响其在土壤中迁移的主要影响因素.光解、微生物降解是BFRs在土壤中的主要转化途径,光解是表层土壤中BFRs的主要转化过程,逐步脱溴产生低溴化产物,溴化程度、土壤有机质和矿物质会直接影响其光解速率;厌氧脱溴和好氧微生物降解是BFRs在深层土壤中的主要降解过程,溴化程度与微生物降解密切相关.土壤中BFRs被植物吸收的过程中可能被代谢为低溴化产物,在食物链中积累,危害人体健康.尽管多年来在BFRs方面的研究取得了进展,但对这类污染物的环境行为和归趋的全面了解仍然很难,随着越来越多的新型BFRs被作为传统BFRs的替代品推向市场,建议对这些新兴替代化学品在土壤介质中的迁移转化过程,特别是生物降解进行更多的调查.      

温拌阻燃沥青混合料阻燃效果评价

通过氧指数、质量损失率及路用性能试验,研究EC130温拌剂、FRMAX型阻燃剂对沥青混合料阻燃效果的影响。试验结果显示,相比普通沥青混合料,阻燃沥青混合料、温拌阻燃沥青混合料氧指数分别增加23.3%、25.6%,质量损失率减小28.0%、32.0%,残留动稳定度增加14.0%、16.1%,残留最大弯拉应变增加14.1%、17.1%,冻融劈裂强度比增加5.3%、9.0%。相比普通沥青路面,阻燃沥青路面、温拌阻燃沥青路面发生火灾时能够减少34.0%、41.1%的毒害气体生成,并减少路面修补所需的混合料质量。其次得出普通沥青路面、阻燃沥青路面及温拌阻燃沥青路面的质量损失率、残留动稳定度、残留最大弯拉应变、残留冻融劈裂强度比与燃烧时间的关系模型。结果表明:阻燃剂对沥青混合料的阻燃效果显著;温拌剂有助于阻燃剂更好地发挥阻燃作用,降低火灾对道路的破坏,降低隧道火灾发生时有害气体的生成,提升隧道安全性。     

监控完全遮挡场景下火焰特征分析方法*

为解决监控完全遮挡场景下火灾原因认定面临的问题,探究火焰的视频特征分析方法。利用油盘火、垃圾桶火焰和短路火花3种实体火焰模拟室内火灾,布置普通彩色CCD监控摄像头使之被完全遮挡,收集火灾视频进行预处理,利用视频分析技术提取、对比、分析油盘火焰、垃圾桶火焰和短路火花的HSV颜色、火焰面积增长、质心变化、Harris角点变化、火焰频闪等特征,并总结对应特征变化规律。结果表明:在监控完全遮挡场景下,提出的火焰视频特征分析方法可以较为精确地定量表征火焰动静态特征,为火灾调查工作的顺利开展提供有力的工具。     

The effect of barriers on reducing thermal heat fluxes from a hydrocarbon pool fire

The radiant heat flux from a pool fire is frequently calculated using the solid flame model, where the flame envelope is approximated as a stationary cylinder whose surface emits thermal radiation at a constant rate. Radiant heat flux calculations using the solid flame model assume the target to be at a given elevation, typically at ground level, and to have an unobstructed view of the fire. The presence of obstacles (e.g., walls, buildings, etc.) or terrain features that would create shaded areas and provide shielding of a target from the fire is typically neglected in these calculations: this is a conservative approach, but it is not accurate. This paper presents a methodology to utilize the solid flame model to calculate the heat flux to a target while taking into account the presence of an obstruction between the target and the fire. The shielded solid flame method can quantitatively account for the presence of obstacles as a passive mitigation measure and allows project developers or designers to optimize their facility layout to meet safety requirements. The methodology presented in this paper uses the same correlations found in currently used solid flame models (e.g., LNGFIRE3), therefore, it remains consistent with current regulatory requirements for LNG facilities in the U.S.     

爆炸形成过程中火焰加速的试验研究

为预防和控制工业爆炸事故,并为脉冲爆轰发动机的研究提供理论指导,分析火焰加速导致的燃烧转爆轰过程的影响因素。采用爆轰管探讨障碍物的阻塞比、混合物的组成、初始压力和点火能等4个因素对爆炸性气体火焰速度和爆轰压力的影响规律。试验结果表明:障碍物的存在能大大提高火焰速度和爆轰压力;爆轰压力随管内障碍物阻塞比的增大先变大后减小,并在阻塞比为0.498,燃料种类为天然气,化学当量比为1时达到最大;爆轰压力还随混合气体初始压力的增大和点火能的提高而增大。选择适宜的条件可大大提高火焰加速速率,促进燃烧向爆轰过程转变。     

典型木材燃料层流扩散火焰碳黑生成特性研究

为了对木材燃料层流扩散火焰碳黑生成特性进行研究,搭建了基于消光法原理的轴对称层流火焰碳黑浓度测量平台, 选用马尾松针、柚木以及红橡木三种典型木材燃料粉碎成针状试样,并堆成直径3.5 cm堆垛,利用酒精引燃后可获得稳定的层流扩散火焰,同时通过电热丝辅助加热延长稳定燃烧。通过对三种典型木材燃料层流燃烧过程的质量损失和火焰碳黑浓度的测量和对比分析,结果显示三种燃料中马尾松针碳黑生成能力最大,这说明木材的碳黑生成能力可能与其碳元素和氧元素的含量有关。     

泄爆口参数对氢气火焰传播过程影响的数值模拟*

为了减少管内气体爆炸造成的损失与破坏,基于大涡模拟LES模型和Zimont燃烧模型,研究泄爆尺寸(直径为40,60,80 mm)和泄爆位置(侧方距点火端1,3,5 m)等泄爆条件对受限空间中氢气燃爆特性的影响。研究结果表明:大孔径泄爆口更好的排放效果造成火焰锋面在通过泄爆口时发生严重畸变,而泄爆口与点火端距离的增加则会削弱火焰锋面畸变的程度,且不同尺寸泄爆口产生的泄压效果差异较大。因此,应考虑将合适尺寸的泄爆口设置于靠近易燃点处。通过探索不同泄爆孔径与泄爆口位置对氢气火焰传播的影响规律,可为实际应用中的安全泄爆起到指导性作用。