顶空-气相色谱法测定地表水中6种乙酸酯类化合物

采用顶空-气相色谱法测定地表水中乙酸酯类化合物,并对顶空瓶的加热温度、平衡时间进行优化。优化后,方法在6种乙酸酯类化合物质量浓度0.05~1.00 mg/L范围内线性良好,检出限为4.49~58.5μg/L,RSD为0.61%~2.51%,加标回收率为96.5%~104%,方法便捷、环保、经济,适用于地表水中乙酸酯类的检测。     

Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry

A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg^?1 (square regression) and 250.0 and 2000.0 μg kg^?1 (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg^?1, respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.     

中国环保产业调查方案设计研究

结合中国目前环保产业调查的现状及其存在问题,设计了以普查为基础、以抽样调查为主体的环保产业调查方案,并采用按产值规模的分层抽样以及与其等样本量的重点抽样、按行业分类的分层抽样以及与其等样本量的重点抽样4种方法对2004年中国环保产业调查进行了实证.结果表明,重点抽样的误差小于分层抽样,且按产值分层抽样的误差小于按行业分类抽样;抽样实践中应考虑以重点抽样为主,而样本量则可以按产值分类的分层抽样所需的样本量来确定,这样得到的误差会更小.抽样调查能够以更低的成本实现对总体情况的较好估计,也更具实践可操作性,能够为环保产业发展形势的连续观测提供可靠的依据.     

Sources of Volatile Organic Compounds in a University Building

A total of 34 volatile organic compounds (VOCs) were measured in the indoor of laboratories, offices and classrooms of the Chemical Engineering Department of Hacettepe University in Ankara in 2 week-day passive sampling campaigns. The average concentrations ranged from 0.77 to 265 μg m^?3 at the different indoor sites, with the most abundant VOC found to be toluene (119.6 μg m^?3), followed by styrene (21.24 μg m^?3), 2-ethyltoluene (17.11 μg m^?3), n-hexane (10.21 μg m^?3) and benzene (9.42 μg m^?3). According to the factor analysis, the evaporation of solvents used in the laboratories was found to be the dominant source.     

兰州市生活垃圾物理成分及含水特性分析

通过冬夏两季现场采样和分析,得出兰州市生活垃圾物理成分、含水率的测定值,根据垃圾日产量调查数据得出市郊4区6个填埋场的加权平均值。分析了垃圾物理成分、含水率季节变化特点及原因,与国内其他城市的差别及原因。分析数据可作为兰州市生活垃圾基础资料的一部分,结论和建议可供政府制定垃圾处理技术政策和方案选择时参考。     

Dilution sampling and analysis of particulate matter in biomass-derived syngas

Thermochemical biomass gasification, followed by conversion of the produced syngas to fuels and electrical power, is a promising energy alternative. Real-world characterization of particulate matter (PM) and other contaminants in the syngas is important to minimize damage and ensure efficient operation of the engines it powers and the fuels created from it. A dilution sampling system is demonstrated to quantify PM in syngas generated from two gasification plants utilizing different biomass feedstocks: a BioMax^?15 Biopower System that uses raw and torrefied woodchips as feedstocks, and an integrated biorefinery (IBR) that uses rice hulls and woodchips as feedstocks. PM_2.5 mass concentrations in syngas from the IBR downstream of the purification system were 12.8–13.7 μg·m^-3, which were significantly lower than the maximum level for catalyst protection (500 μg·m^-3) and were 2–3 orders of magnitude lower than those in BioMax^?15 syngas (2247–4835 μg·m^-3). Ultrafine particle number concentration and PM_2.5 chemical constituents were also much lower in the IBR syngas than in the BioMax^?15. The dilution sampling system enabled reliable measurements over a wide range of concentrations: the use of high sensitivity instruments allowed measurement at very low concentrations (~1 μg·m^-3), while the flexibility of dilution minimized sampling problems that are commonly encountered due to high levels of tars in raw syngas (~1 g·m^-3).     

基于高密度采样的土壤重金属分布特征及迁移速率

重金属在土壤剖面中的垂直分布特征是土壤自身理化性质和外界条件影响下重金属迁移和积累的综合反映,也是了解土壤重金属污染程度和修复治理的基础.传统的用于农业土壤研究的层次采样技术和方法,只能粗略了解重金属在土壤层次中的分布状况,不足以确定污染物的垂直迁移距离和速度.本研究通过对钢铁厂周边3种不同利用类型土壤进行垂直方向的高密度采样分析,即在0～40cm深度内以2cm间隔,在40～80cm以5cm间隔,80cm以下以10cm间隔采样,对重金属元素Cu、Zn、Pb、Cr、Cd的剖面垂直分布进行了研究.结果表明,在几乎未受人为干扰的林地土壤中,可见重金属在土壤表层明显富集,证实其来源是大气沉降,其中Zn、Pb向下迁移的距离很小,Cu、Cd迁移稍快,Cr向下淋溶迁移的深度没有明显的界限;在受人为影响的旱地和水稻田中,重金属在耕层土壤中被人为扰动混合,但在耕层界面以下仍然有明显的向下迁移.研究表明,垂直方向高密度采样可以比较精确地理解重金属在土壤中的分布模式,通过重金属元素含量与稳定元素Ti含量的比值及其变化,还可以估计在特定时间内污染物的迁移距离和迁移速度,各种重金属具有不同的迁移能力,其相对顺序为Cd>Cu>Zn>Pb.     

固定源PM_(2.5)稀释采样器的研制

为研究固定源PM2.5的排放特征,研制开发了一套紧凑型稀释采样器,能模拟高温烟气排放到大气中的冷却、稀释、凝结等物理化学过程,采集固定源排放的一次PM2.5.稀释采样器主要的技术参数如下:稀释比在20∶1~50∶1范围内,在稀释器里的停留时间为10 s,稀释后的烟气温度和相对湿度分别小于42℃和50%,满足ISO 25597:2013的要求.稀释采样器的性能评价实验表明,稀释器气密性良好,稀释空气中颗粒物浓度低,气流混合均匀性良好,细颗粒在采样器内的损失小,表明稀释采样器可靠性高,适合于对固定源排放PM2.5的采集.     

海洋痕量元素采样技术和分析方法的发展及展望:厦门大学痕量元素平台建设进展

海洋中的痕量元素通常是指质量摩尔浓度在10 μmol ·kg^-1以下的元素,是海水的重要化学组分,其中既有铁和锌等海洋生物新陈代谢所必需的微量营养元素,对海洋初级生产力具有重要的调控作用,因而也与碳氮等元素的生物地球化学循环密切相关,进而影响地球环境演化与全球气候变迁;也有铅等源于人类活动的污染物.痕量元素及其同位素还可作为许多海洋学过程的示踪物和古海洋学研究的指标.然而,海水的高盐基底和痕量元素极低的浓度,加之在样品采集、处理与分析过程中极易受到科考船、采样设备和周围环境的沾污,在相当长的一段历史时期限制了科学家获得可靠的海洋痕量元素含量数据.因此,获取无沾污的样品并加以准确定量成为研究海洋痕量元素生物地球化学与环境行为的先决条件.通过回顾国际海洋学界海洋痕量元素采样技术和分析方法的发展历程,介绍了厦门大学在该领域的研究历史和平台建设进展,重点比较了不同采样技术和分析方法的优缺点及其适用性,并展望了未来的发展趋势.     

Environmental sampling of volatile organic compounds during the 2018 Camp Fire in Northern California

Trace analysis of volatile organic compounds (VOCs) during wildfires is imperative for environmental and health risk assessment. The use of gas sampling devices mounted on unmanned aerial vehicles (UAVs) to chemically sample air during wildfires is of great interest because these devices move freely about their environment, allowing for more representative air samples and the ability to sample areas dangerous or unreachable by humans. This work presents chemical data from air samples obtained in Davis, CA during the most destructive wildfire in California's history - the 2018 Camp Fire – as well as the deployment of our sampling device during a controlled experimental fire while fixed to a UAV. The sampling mechanism was an in-house manufactured micro-gas preconcentrator (µPC) embedded onto a compact battery-operated sampler that was returned to the laboratory for chemical analysis. Compounds commonly observed in wildfires were detected during the Camp Fire using gas chromatography mass spectrometry (GC–MS), including BTEX (benzene, toluene, ethylbenzene, m+p-xylene, and o-xylene), benzaldehyde, 1,4-dichlorobenzene, naphthalene, 1,2,3-trimethylbenzene and 1-ethyl-3-methylbenzene. Concentrations of BTEX were calculated and we observed that benzene and toluene were highest with average concentrations of 4.7 and 15.1 µg/m³, respectively. Numerous fire-related compounds including BTEX and aldehydes such as octanal and nonanal were detected upon experimental fire ignition, even at a much smaller sampling time compared to samples taken during the Camp Fire. Analysis of the air samples taken both stationary during the Camp Fire and mobile during an experimental fire show the successful operation of our sampler in a fire environment.