微波-亚临界水萃取底泥中两种多氯联苯的研究

微波亚临界水萃取模拟土样中的2,3-二氯联苯和3,3′-二氯联苯,用气相色谱进行分析。与亚临界水萃取方法相比,该法缩短了萃取时间,分析物的萃取回收率有所提高。对微波亚临界水的萃取条件进行优化,确定了最佳萃取条件为时间20min、温度区段为210℃～225℃。方法对长江镇江段内江的底泥中的多氯联苯进行分析,测定结果与索氏提取-GC分析结果吻合,且不受底泥中腐殖质等有机物影响。     

Extraction and clean-up methods for organochlorine pesticides determination in milk

Organochlorine pesticides (OCPs) can cause environmental damage and human health risks since they are lipophilic compounds with high resistance to degradation and long half-lives in humans. As most persistent OCPs have been banned years ago, it is expected to find these compounds at trace levels in environment. Therefore, increasingly sensitive and reliable analytical techniques are required to ensure effective monitoring of these compounds. The aim of this review is to discuss extraction and clean-up methods used to monitor OCP residues in milk, reported in the last 20 years. To carry out this review, an exhaustive bibliographic review was conducted. Despite the disadvantages of conventional extraction and clean-up methods, such as liquid–liquid, solid-phase or Soxhlet extractions, these procedures are still used due to their reliability. New extraction methods, like solid-phase microextraction, matrix solid-phase dispersion or QuEChERS, have not been thoroughly evaluated for OCP determination in milk. Almost all the methodologies analyzed in this review presented good performance characteristics according to the performance acceptability criteria set in SANCO’s procedure. Comparison between limits of quantification (LOQ) and detection (LOD), for the reported methodologies, is not always possible due to the heterogeneity of the units. Thus, researchers should take into account an homogenization of LOD and LOQ units, according to the international regulations and MRLs established. Finally, more research is necessary to obtain the ideal methodology for OCPs determination in milk, which comprises the environmentally friendly characteristics of the new techniques and the reliability of the traditional methodologies.     

Assessment of organochlorine pesticide residues in Atlantic Rain Forest fragments, Rio de Janeiro, Brazil

A superficial water quality survey in a watershed of the Paraíba do Sul River, the main water supply for the most populated cities of southeastern Brazil, was held in order to assess the impact of the expansion of agricultural activity in the near border of the Atlantic Rain Forest. The aim of this study was to investigate the presence of priority organochlorine pollutants in soils and superficial waters of Atlantic rainforest fragments in Teresópolis, Rio de Janeiro State. Soil sample preparations were compared by using ultrasound, microwave assisted extraction and Soxhlet extraction. Recoveries of matrix spiked samples ranged from 70 to 130%. Analysis of a certified soil material showed recoveries ranging from 71 to 234%. Although low concentrations of organochlorine residues were found in water and soil samples, this area is of environmental importance and concern, thus demanding a monitoring program of its compartments.     

Comparison of Three Extraction Methods for 17 β-Estradiol in Sand,Bentonite, and Organic-Rich Silt Loam

Extraction is an important procedure for samples that contain soil because other compounds in soil may affect analysis of estrogens. This study was conducted to evaluate three different extraction methods for 17β-estradiol in soil. Sand, bentonite, and organic-rich silt loam were spiked with 1 mg kg^{? 1} of 17β-estradiol as a model compound of estrogens. 17β-estradiol and its metabolites, estrone and estriol, were extracted using (i) a modified Bligh and Dyer extraction, (ii) a pressurized fluid extraction, and (iii) a diethyl ether extraction, and measured by liquid chromatography tandem mass spectrometry. There were significant differences in the extraction efficiency for 17β-estradiol among the extraction methods and the soils: the efficiencies ranged from 10% to 97%. Overall, the diethyl ether extraction method had the largest efficiency of 17β-estradiol with 45% and 57% for bentonite and silt loam, respectively. Transformation of 17β-estradiol to estrone and estriol in the different extraction methods was less than 3.6% during the extraction procedures. This study underlined the importance of sample preparation for estrogen analysis in soil samples.     

A 1-dodecanethiol-based phase transfer protocol for the highly efficient extraction of noble metal ions from aqueous phase

A 1-dodecanethiol-based phase-transfer protocol is developed for the extraction of noble metal ions from aqueous solution to a hydrocarbon phase, which calls for first mixing the aqueous metal ion solution with an ethanolic solution of 1-dodecanethiol, and then extracting the coordination compounds formed between noble metal ions and 1-dodecanethiol into a non-polar organic solvent. A number of characterization techniques, including inductively coupled plasma atomic emission spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis demonstrate that this protocol could be applied to extract a wide variety of noble metal ions from water to dichloromethane with an efficiency of >96%, and has high selectivity for the separation of the noble metal ions from other transition metals. It is therefore an attractive alternative for the extraction of noble metals from water, soil, or waste printed circuit boards.     

PERCOLATION OF LEAD(II) AND CADMIUM(II) THROUGH TWO BENTONITES USED AS LANDFILL LINER

In order to prevent contamination of subsoil and groundwater by leachates containing heavy metals, montmorillonite linings are used on landfill bottoms. It is therefore important to understand ion uptake by this clay. In this study we have performed percolation of lead(II) and cadmium(II) through columns filled firstly with a technical bentonite and then with a reference bentonite. Elution curves provide an evaluation of metals retention. After the percolation step, columns are cut and metal ions are extracted to evaluate influence of side effects and soil depth on metal uptake. Moreover retentions of lead(II) and cadmium(II) are compared.     

Set-up costs and the existence of competitive equilibrium when extraction capacity is limited

Although set-up costs are prevalent and substantial in natural resource extraction, it is known that a Walrasian competitive equilibrium cannot exist in simple extraction models with set-up costs. This paper demonstrates that this result is sensitive to the assumption of unlimited extraction capacity and derives sufficient conditions for existence. An equilibrium exists if extraction is limited such that each firm earns sufficient surplus to cover its set-up costs or if firms choose extraction capacity subject to non-increasing returns. The resulting competitive equilibrium price either grows at the rate of interest when total extraction is below industry capacity or is constant when industry capacity is fully utilized. In the equilibrium, identical deposits are opened simultaneously, and set-up costs for new deposits are incurred when the industry has excess capacity rather than when capacity is fully utilized.     

几种螯合剂对污染土壤的重金属提取效率的研究

在Cd,Pb污染的土壤上,采用批提取实验(batchexperiment),研究了几种螯合剂和不同的水土比对重金属提取效率的影响。结果表明:螯合剂对Cd的提取效率随着各淋洗剂浓度的提高而逐渐提高,相同浓度下各淋洗剂的提取效率大小顺序依次为EDTA>DTPA>NTA>PA>CA>CD>HCl。随水土比提高,相应的提取效率也提高。几种淋洗剂中只有EDTA对Pb和Cd都能达到理想的淋洗效果。     

Influence of soil moisture on the sequestration of organic compounds in soil

A study was conducted as a part of continuing investigation of the effect of soil moisture on the sequestration of organic compounds aged in the soil. Here, experiments focused on the effects of moisture changes within the soil before, during, and after contaminant addition. The extractability of aged (68 d) phenanthrene was greater from soil that had been subjected to wetting and drying cycles prior to solute addition as compared to soil initially maintained at constant moisture. The recovery of phenanthrene added to moist soil was increased relative to extractability from soil that was air-dried at the time of the contaminant addition. Repeated wetting and drying of soil after the addition of atrazine or phenanthrene resulted in decreased extractability of the compounds as compared to samples maintained at constant moisture. A method for rapidly sequestering contaminants is proposed and may be useful in limiting the time required for laboratory studies involving “aged” contaminants. These data build upon the findings of earlier work from our laboratory and indicate that changes in the moisture conditions of soil can affect the availability of sequestered contaminants possibly through alterations in the structure of the natural solid.     

超临界态二氧化碳再生活性炭法治理甲苯废气

制鞋业产生的含甲苯、苯和二甲苯废气的治理大多采用活性炭吸附法。该课题提出以压缩二氧化碳为脱附剂,采用超临界流体萃取技术再生活性炭及回收甲苯工艺。实验表明,以液态或超临界态的压缩二氧化碳作萃取剂,采用萃取法可完全再生活性炭,其采用液态优于超临界态;压缩二氧化碳对活性炭具有扩孔作用,可增加活性炭的吸附容量,多次再生的活性炭吸附容量几乎不变;萃取剂的用量和密度显著影响着活性炭的再生效率;活性炭捆包填充在脱附塔中,不会显著增加脱附的阻力。