Analyses of phenolic compounds occurring in olive oil mill wastewaters by GC–MS

Phenolic compounds in olive oil mill wastewaters were analysed by HRGC–MS after extracting the acidified solution with ethyl acetate and derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide. Both simple and complex phenols were detected with the latter being the most abundant. 1,2-dihydroxybenzene (catechol), p-hydroxyphenyl ethanol (tyrosol), 3,4-dihydroxyphenyl ethanol (hydroxytyrosol) and 4-hydroxy-3-methoxyphenyl ethanol (homovanillyl alcohol) predominated among the simple phenols using a gas chromatograph coupled with a mass selective detector.     

Impacts of surfactants on the ecotoxicological effects of TiO2-NP and/or Cd contamination in sediments北大核心CSCD

Surfactants may alter the interaction between engineered nanoparticles (ENP) and coexisting pollutants, and further influence the ecotoxicity of these pollutants. This research aimed to evaluate the impacts of the surfactant sodium dodecyl benzene sulfonate (SDS) on the ecotoxicological effects of TiO2-NP and Cd combined contamination in freshwater sediments by deposit-feeding gastropoda Bellamya aeroginosa. We investigated the effects of TiO2-NP and/or Cd contamination in the presence of different concentrations of SDS on DNA damage, Na+, K+-ATPase activities, malondialdehyde (MDA) levels, and protein carbonyl (PCO) levels in the hepatopancreas of B. aeroginosa following 21-d chronic sediment bioassay. The results showed that low concentration (5 μg g-1) of Cd had no toxicity to B. aeroginosa, while relatively high concentration (25 μg g-1) displayed obvious toxicity, and that SDS could significantly enhance the toxicity of Cd to B. aeroginosa. TiO2-NP with nontoxic concentration could enhance the toxicity of Cd with low concentration to B. aeroginosa, but had no effects on the toxicity of Cd with high concentration. SDS could significantly enhance the toxicity of TiO2-NP and Cd combined contamination to B. aeroginosa in a SDS-concentration-dependent manner. When assessing the potential environmental risk of ENP, we should not only focus on the toxicity of ENP itself, or the interaction between ENP and coexisting contaminants, but also should consider the potential impacts of surfactants and other environmental factors.     

Influence of large-spectrum environmental contamination on the micro–meiobenthic assemblages in harbour sediments of the ligurian sea (W Mediterranean)

The concentration of a large spectrum of environmental contaminants (PCBs, PAHs, pesticides and metals) was assessed in surface sediments of two Ligurian harbours (Sanremo and Alassio, NW Mediterranean Sea, Italy) and their relative impact on micro–meiobenthic assemblages was analysed. Concentration, distribution and relative importance of the different contaminants varied considerably between harbours in relation to the different anthropic activities and contamination sources. Results from Principal Component Analysis indicated that high levels of contaminants were typically correlated with low micro–meiobenthic abundance in the sediment. Heavy metals and the organic enrichment were the main factors affecting the distribution and abundance of the bacterial and meiofaunal assemblages in Alassio harbour, whereas hydrocarbons and pesticides played a major role in Sanremo sediments. Neither the bacteria density nor the meiofauna abundance were dependent on sediment grain size, suggesting that micro–meiobenthic parameters may be under the influence of other variables. Our results suggest that high concentrations of contaminants independently from their source or typology are responsible for the impact observed on micro–meiobenthic assemblages in these harbours.     

A 1955�C2004 record of Hg contamination in Dianshan Lake sediments, Shanghai

Measuring Hg levels of water sediments is one of the primary routes to assess the trend of the contamination. Little work has been carried out in the Yangtze Delta to track the trend of mercury contamination caused by Shanghai, which is one of the fastest growing economies in the world today. The mercury concentration in the sedimentary cores from Dianshan Lake, Shanghai is studied here. Results show that mercury transported to Dianshan Lake from emissions of coal combustion and non-coal sources in the Yangtze Delta was greater after 1979. We found also that before 1979 mercury levels changed less with time than after 1979. Before 1967 Hg levels were more variable than in the 1970s. Moreover, the mercury dissolved in river water and bound to particles of water that flow past downtown Shanghai is different from that observed in Dianshan Lake, which is located in upper Shanghai. This indicates that atmospheric Hg deposition is probably the main source of mercury in Dianshan Lake. These results are important for the establishment of environmental protections and pollution treatment proposals for mercury in similar areas of the world, as well as in Shanghai.     

Rapid liquid–liquid extraction for the reliable GC/MS analysis of volatile priority pollutants

Mass spectrometry is a powerful tool for the analysis of organic pollutants in the environment. Nevertheless, sample preparation for GC/MS analysis is often criticized for being too laborious and requiring expensive equipment. Thus, purge-and-trap or headspace devices are the most popular nowadays to investigate volatile organic pollutants. At the same time, modern commercial high-resolution mass spectrometers allow for the significant simplification of the sample preparation procedures due to better acquisition rate, accurate mass measurements, and improved sensitivity. Here, we used a time-of-flight high-resolution mass spectrometer Pegasus GC-HRT (LECO, USA) to identify and quantify 47 volatile priority organic pollutants in water. The developed accelerated water sample preparation approach requires just 1 mL of water and 1 mL of dichloromethane. The detection limits of the analytes are about 1 μg L^?1, while the quantification limits are approximately 5 μg L^?1. These limits correspond to those required by Method 8260C of the United States Environmental Protection Agency. Here, we demonstrate that sample preparation for the reliable and sensitive GC/MS analysis of volatile organic priority pollutants may be achieved in 5 min in 5-mL vials in the field or just prior to GC/MS analysis in the laboratory without the use of any expensive equipment.     

利用GC和GC/MS对溢油风化的鉴定

对重质燃料油泄漏两个月后现场采集的溢油样品进行分析,通过对比可见:各样品的风化程度不一,碳数较低的烷烃明显减少,特征比值C19 20/C21 22和Pr/Ph较为稳定,能很好地指示油样的来源;但C17/Pr和C18/Ph已明显降低.通过对1*油样与泄漏的重质燃料油中芳烃比较可知:芳烃CnB,C0N,C1N,C2N和C3N基本消失,油样与泄漏的重质燃料油中C3D(m/z 226)的分布几乎完全一致,说明C3D的分布对溢油鉴定有十分重要意义.     

Variations in heavy metal contamination of stream water and groundwater affected by an abandoned lead–zinc mine in Korea

This study evaluated variations in heavy metal contamination of stream waters and groundwaters affected by an abandoned lead–zinc mine, where a rockfill dam for water storage will be built 11 km downstream. For these purposes, a total of 10 rounds of stream and groundwater samplings and subsequent chemical analyses were performed during 2002–2003. Results of an exploratory investigation of stream waters in 2000 indicated substantial contamination with heavy metals including zinc (Zn), iron (Fe) and arsenic (As) for at least 6 km downstream from the mine. Stream waters near the mine showed metal contamination as high as arsenic (As) 8,923 μg L⁻¹, copper (Cu) 616 μg L⁻¹, cadmium (Cd) 223 μg L⁻¹ and lead (Pb) 10,590 μg L⁻¹, which greatly exceeded the Korean stream water guidelines. Remediation focused on the mine tailing piles largely improved the stream water qualities. However, there have still been quality problems for the waters containing relatively high concentrations of As (6–174 μg L⁻¹), Cd (1–46 μg L⁻¹) and Pb (2–26 μg L⁻¹). Rainfall infiltration into the mine tailing piles resulted in an increase of heavy metals in the stream waters due to direct discharge of waste effluent, while dilution of the contaminated stream waters improved the water quality due to mixing with metal free rain waters. Levels of As, Cu and chromium (Cr) largely decreased after heavy rain but that of Pb was rather elevated. The stream waters were characterized by high concentrations of calcium (Ca) and sulfate (SO₄), which were derived from dissolution and leaching of carbonate and sulfide minerals. It was observed that the proportions of Ca and SO₄ increased while those of bicarbonate (HCO₃) and sodium and potassium (Na+K) decreased after a light rainfall event. Most interestingly, the reverse was generally detected for the groundwaters. The zinc, being the metal mined, was the most dominant heavy metal in the groundwaters (1758–10,550 μg L⁻¹) near the mine, which far exceeded the Korean standard of 1000 μg L⁻¹ for drinking water. The decreases in the heavy metals contents in the groundwaters associated with reduced rainfall were quite different from the increases observed for the stream waters, which is not clearly understood at this time and warrants further investigation.     

GC/MS/MS分析复杂基体中痕量组分的优越性

在现代实验室中,GC/MS用于痕量分析极为普遍,要求更低的检测限而被分析样品的基体越来越复杂的情况由来已久.……     

沃特世QUATTRO MICRO GC对水中多环芳烃(PAHs)的快速GC/MS/MS分析

GC/MS分析多环芳烃(PAHs)被认为是分析这些持久性有机污染物最灵敏的方法之一.PAHs使用标准的GC色谱柱很容易分离且无需衍生化.使用一根长30m,内径0.25 mm,膜厚0.25μ肌的5%苯基聚甲基硅烷固定相的色谱柱,可以在不到30min内分离所有的PAHs.使用细内径、薄膜厚的色谱柱能够提高分离能力,并减少分析时间.     

高层建筑水箱浸出有机物的GC/MS分析

采用高分子大网状吸附树脂(XAD)富集技术和GC/MS方法,对国内七种材料的水箱浸出有机物进行了分析,共计检出有机物百余种.根据测定结果可以判定,作为水箱的材质和涂料,水泥、SHZ-90瓷釉和玻璃钢是比较好的,其次为环氧树脂;聚胺酯和“青凝”涂料配方中都存在较大问题,应进一步改进;防锈漆问题最多,效果最差,应逐步淘汰.这一工作为合理地选择水箱材料和二次加压高层建筑供水设施的卫生学评价提供了科学依据.     

GC/MS/MS法测定水果中10种甲氧基丙烯酸酯类杀菌剂残留量

本文使用岛津GCMS-TQ8050 NX三重四极杆气相色谱质谱联用仪建立了测定水果中10种甲氧基丙烯酸酯类杀菌剂残留量的测定方法.水果样品由乙腈简单提取,经分散固相萃取试剂净化后上GC/MS/MS分析,大大减少了样品前处理过程.在0.5—200μg·L~(-1)浓度范围内10种甲氧基丙烯酸酯类杀菌剂线性关系良好,相关系数均达到0.998以上.5.0μg·L~(-1)标准品溶液连续进样6针,峰面积RSD%小于8%.实际样品加标回收率为93.5%—104.3%.该方法快速、简便、灵敏度高,完全满足食品安全分析对甲氧基丙烯酸酯类杀菌剂的检测要求.     

GC/MS/MS法结合SPME进样测定饮用水中亚硝胺类化合物

本文利用岛津公司GCMS-TQ8050 NX三重四极杆气质联用仪以及AOC-6000自动进样器的SPME Arrow功能,建立了一种饮用水中亚硝胺类化合物的测定方法.水样经固相微萃取方式萃取后采用多反应监测模式(MRM)进行检测.11种亚硝胺类化合物在线性范围内线性关系良好,标准曲线相关系数(R) ＞0.999,检出限...     

Assessing heavy-metal contamination and sources by GIS-based approach and multivariate analysis of urban–rural topsoils in Wuhan,central China

Nine potentially harmful heavy metals (Cd, Co, Cr, Cu, Hg, Mn, Pb, Ni, and Zn) were measured in 477 topsoil samples collected from urban–rural areas in the city of Wuhan in order to identify their concentrations and possible sources, and characterize their spatial variability for risk assessment. Results showed that in most rural areas heavy-metal concentrations in soil were similar to their natural background values, but Cd, Cu, Hg, Pb, and Zn concentrations were relatively higher in densely populated districts and around industrial facilities. Multivariate analyses (correlation matrix, principal component analysis, and cluster analysis) indicated that Cd, Cu, Hg, Pb, and Zn were mainly derived from anthropogenic inputs, and Co, Cr, and Mn were controlled by natural source, whereas Ni appeared to be affected by both anthropogenic and natural sources. The result of risk assessment indicated that nearly 48% of the study area suffered from moderate to severe contamination.     

单极四杆GC/MS分析VOCs的最新进展

根据美国环境保护署(EPA)方法,采用赛默飞世尔公司ISQ单四极杆气质联用仪建立了挥发性有机物(VOCs)的分析检测方法.整个方法所需的仪器包括进样器、气相色谱、质谱、数据处理软件等.为了满足法规中日益严格的检出限要求及新型污染物的加入,我们对实验方案进行了改进,以提高检测灵敏度及提高样品通量.     

安捷伦科技于2011年ASMS大会推出新型LC/MS和GC/MS系统

2011年6月6日,安捷伦科技公司在2011年度美国质谱大会（ASMS）上推出了新的质谱系统,将生物分析和化学分析的性能标准提高到一个新的水平.     

Speciation of particulate trace metals in sediments of Anarbe reservoir∗

Total concentration and chemical forms of heavy metals in samples of sediment from a drinking water reservoir have been analysed. The result of total metal contest shows Fe and Mn concentration increase along the reservoir, from 4.4% in Fe and 0.07% in Mn in the end part to 6.4% Fe and 0.22% Mn at the dam. However, a decrease in organic matter along the reservoir is observed. In order to test the accuracy of the digestion methods used, a standard reference material was also analysed.

Trace metal concentrations, with exception of Cadmium, Pb and Mn, found in fraction 5 are higher than those observed in the others extractions, Fe, Ni, Zn, Cr and Cu content in non‐residual fraction is found mainly in moderately reducible fraction, but the percentage of this fraction in each metal is very different.     

Seasonal AVS–SEM relationship in sediments and potential bioavailability of metals in industrialized estuary, southeastern Brazil

In anoxic sediments, as those found in estuaries, the mobility of metals can be controlled by the formation of stable sulfide complexes. The potential bioavailability of a metal can then be predicted on the basis of the acid volatile sulfide (AVS) and simultaneously extracted metals (SEM) criterion. Distributions of AVS and SEM (Hg, Cu, Pb, Cd, Zn, and Ni) along the sediment profiles were determined seasonally for three rivers that constitute the Santos-Cubat?o estuarine system (SE Brazil), which is located in one of the most industrialized areas of Latin America. AVS and SEM concentrations varied significantly, from 0.04 to 31.9 μmol g⁻¹ and 0.086–6.659 μmol g⁻¹, respectively. The highest AVS levels in sediments were detected in the winter, whereas high SEM values predominated in the summer. Considering SEM–AVS molar differences as a parameter to evaluate potential bioavailability, sediments nearest to the industrial area represent higher risk to biota, especially during the summer. It is due to relatively low AVS values and not necessarily high concentrations of metals.     

Effects of dissolved organic matter on the desorption of Cd in freeze–thaw treated Cd-contaminated soils

Lab-scale experiments were conducted to investigate the effects of dissolved organic matter (DOM) on the desorption of Cd in freeze–thaw treated Cd-contaminated soils. The results indicated that DOM significantly facilitated the desorption of Cd from freeze–thaw treated soils when comparing with that of non-frozen soils. Effects of DOM on the Cd desorption were highly dependent on the soil type and contamination concentration. The maximum desorption ratios of Cd by DOM generated from straw and sludge were 15.6% and 13.65%, respectively, in brown soils, and the maximum desorption ratios reached 14.7% and 9.3%, respectively, when using black soils through the same treatment. The higher the Cd contamination concentration in soils, the higher the ratio of Cd desorption by DOM. This was because of the integrated effects of the soil properties changed by the freeze–thaw treatment and the species transformation of Cd. The characteristics of DOM, such as its concentration and properties, had shown obvious impacts on the Cd desorption by DOM. The desorption was promoted with the increased DOM concentration and the hydrophilic fraction, and lowered pH and the low-molecular-weight of DOM.     

Trends of chemical speciation profiles of anthropogenic volatile organic compounds emissions in China, 2005–2020

This study estimates the detailed chemical profiles of China＇s anthropogenic volatile organic com- pounds （VOCs） emissions for the period of 2005-2020. The chemical profiles of VOCs for seven activity sectors are calculated, based on which the Photochemical Ozone Creation Potential （POCP） of VOCs for these sectors is evaluated. At the national level, the VOCs species emitted in 2005 include alkanes, alkenes and alkynes, aromatic compounds, alcohols, ketones, aldehydes, esters, ethers and halocarbons, accounting for 26.4wt.%, 29.2wt.%, 21.3 wt.%, 4.7 wt.%, 5.4 wt.%, 1.7 wt.%, 2.1 wt.%, 0.7 wt. % and 2.2wt.% of total emissions, respectively. And during 2005-2020, their mass proportions would respec- tively grow or decrease by - 34.7%, -48.6%, 108.5%, 6.9%, -32.7%, 7.3%, 65.3%, 100.5%, and 55.4%. This change would bring about a 13% reduction of POCP for national VOCs emissions in the future. Thus, although the national VOCs emissions are expected to increase by 33% over the whole period, its ozone formation potential is estimated to rise only by 14%. Large discrepancies are found in VOCs speciation emissions among provinces. Compared to western provinces, the eastern provinces with a more developed economy would emit unsaturated hydrocarbons and benzene with lower mix ratios, and aromatic compounds except benzene, oxidized hydrocar- bons and halocarbons with higher mix ratios. Such differences lead to lower POCP of VOCs emitted in eastern provinces, and higher POCP of VOCs emitted in western provinces. However, due to the large VOCs emissions from Chinese eastern region, the ozone forma- tion potential of VOCs emission in eastern provinces would be much higher than those in western provinces by about 156%-235%.