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Development of a microwave sample preparation method for the determination of arsenic in humus and moss samples by graphite furnace atomic absorption spectrometry. 建立了用石墨炉原子吸收光谱法测定腐殖质和苔藓样品中砷的微波制样方法。
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000151
P. Perämäki, M. Pesonen, J. Piispanen
Two sample decomposition methods were optimized for the determination of arsenic by graphite furnace atomic absorption spectrometry (GFAAS) in moss and humus samples. In the first method, 5,0 ml of HNO 3 and 3,0 ml of H 2 O 2 were used for the decomposition of 500 mg of sample. When humus samples were decomposed in this way a slight, undissolved residue remained. Therefore, another sample decomposition method, including hydrofluoric acid, was also tested (5,0 ml HNO 3 ; 3,0 ml H 2 O 2 ; 0,4 ml HF; 2,5 ml H 3 BO 3 ). Pyrolytically coated graphite tubes, equipped with integrated or L'vov platfoms, were used in the determination of arsenic by GFAAS. Palladium-magnesium nitrate was used as a matrix modifier. Several reference materials (e.g. humus, moss, lichen, sea lettuce) were analyzed.
对石墨炉原子吸收光谱法测定苔藓和腐殖质样品中砷的两种分解方法进行了优化。在第一种方法中,用5,0ml的hno3和3,0ml的h2o2分解500mg的样品。当腐殖质样品以这种方式分解时,会留下少量未溶解的残留物。因此,还测试了另一种样品分解方法,包括氢氟酸(5,0 ml hno3;3,0 ml h2o2;0、4 ml HF;2,5 ml h3bo 3)。采用热包覆石墨管,配以集成或L’vov平台,采用原子吸收光谱法测定砷。采用硝酸钯镁作为基体改性剂。分析了几种参考物质(如腐殖质、苔藓、地衣、海莴苣)。
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引用次数: 17
Determination of glyphosate herbicide and aminomethylphosphonic acid in natural waters by liquid chromatography using pre-column fluorogenic labeling. Part I: Direct determination at the 0.1 μg/L level using FMOC 柱前荧光标记液相色谱法测定天然水中草甘膦、除草剂和氨基甲基膦酸。第一部分:用FMOC在0.1 μg/L水平下直接测定
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000148
E. L. Fur, R. Colin, C. Charreteur, C. Dufau, J. Peron
An analytical method has been developed for the determination of glyphosate herbicide and its metabolite aminomethylphosphonic acid (AMPA) in natural waters to a level of 0.10 µg/L with a good linearity in the range 0.10-2.00 µg/L and coefficients of variation under 20 % for each spiked level. The procedure involves a precolumn derivatization step with 9-fluorenylmethylchloroformate (FMOC-Cl) yielding highly fluorescent derivatives of the analytes which then can be determined by HPLC with fluorescence detection. The method is used for analysis of natural (surface and ground) and treated waters. Matric e effects have been pointed out, particularly the effects of hard ionic content and the effects of chlorine residues into treated waters.
建立了测定天然水体中草甘膦除草剂及其代谢物氨甲基膦酸(AMPA)含量至0.10 μ g/L的分析方法,在0.10 ~ 2.00 μ g/L范围内具有良好的线性关系,每个加标水平的变异系数小于20%。该过程包括柱前衍生化步骤,与9-氟酰甲基氯甲酸酯(FMOC-Cl)产生高荧光衍生物,然后可以用荧光检测的高效液相色谱法测定。该方法用于分析自然(地表水和地下水)和处理过的水。指出了基质效应,特别是硬离子含量的影响和氯残留对处理水的影响。
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引用次数: 25
■ An investigation of the incidence of intersex fish in Seine-Maritime and Sussex regions 塞纳-海地区和苏塞克斯地区双性鱼发生率调查
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000280801
C. Minier, G. Caltot, F. Leboulanger, E. Hill
The incidence of intersex was examined in freshwater fish in one English and three French rivers. Over 331 fish, mainly roach, were sampled above and below the major sewage treatment works (STW) on each river and the incidence of intersex was recorded by histological examination of fish gonads. No intersex conditions were observed in male fish collected either above or below the major STW on the River Ouse in Sussex. In contrast, roach showing primary oocytes in their testes were found in all three French rivers with the incidence ranging from 9 to 21 % of the males. An intersex chubb and gudgeon were also caught, showing that other species can suffer from this pathology. In addition, roach in the River Seine were heavily parasitised with the tapeworm Ligula intestinalis which may impair the reproductive capabilities of the fish. Introduction
研究了一条英国河流和三条法国河流中淡水鱼的双性人发生率。在各条河流的主要污水处理厂上下取样331余条鱼类,主要为蟑螂,并通过对鱼类性腺的组织学检查记录双性虫的发生情况。在苏塞克斯乌斯河主要污水处理厂上方或下方收集的雄性鱼没有观察到双性现象。相比之下,在法国的三条河流中都发现了睾丸中有原始卵母细胞的蟑螂,其发病率从9%到21%不等。雌雄同体的丘贝和雌雄同体的吉吉翁也被捕获,这表明其他物种也可能患有这种疾病。此外,塞纳河的蟑螂被肠尾绦虫严重寄生,这可能会损害鱼的繁殖能力。介绍
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引用次数: 72
Alkylphenol ethoxylates and their degradation products in abiotic and biological samples from the environment. 环境中非生物和生物样品中的烷基酚聚氧基酯及其降解产物。
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000280776
P. Voogt, O. Kwast, R. Hendriks, N. Jonkers
Analytical procedures were optimized for the analysis of surfactants and their degradation products in abiotic and biological samples. The procedures include filtration of water samples and Soxhlet extraction of sediment or sludge samples, followed by automated SPE (C-18 cartridge) and cleanup (Al 2 O 3) . For biological materials a matrix dispersed solid phase extraction method was used. Using these methods, information was obtained about the efficiency of the sewage treatment plants, the changes in oligomer ratios of APEO between influent and effluent, the formation and occurrence of metabolites, and the internal concentrations that may occur when mussels are exposed to APEO in the field.
优化了分析非生物和生物样品中表面活性剂及其降解产物的分析方法。程序包括过滤水样和索氏提取沉淀物或污泥样品,然后是自动SPE (C-18滤筒)和清理(a2o3)。对于生物材料,采用基质分散固相萃取法。利用这些方法,获得了有关污水处理厂效率、进水和出水间APEO低聚物比例的变化、代谢物的形成和发生以及贻贝在野外暴露于APEO时可能产生的内部浓度的信息。
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引用次数: 26
Endocrine disruptors: Analytical and toxicological aspects 内分泌干扰物:分析和毒理学方面
Pub Date : 2000-11-01 DOI: 10.1051/analusis:2000280761
P. Garrigues
http://www.edpsciences.org Endocrine disruptors: Analytical and toxicological aspects Over the last 5 years, concerns have increased about chemicals in the environment, which influence the reproductive capabilities of human and animals. Reproductive hormone-receptor systems appear to be especially vulnerable. Hormonal disturbances in wildlife include sex changes in riverine fish and marine snails, reproductive failure in birds, genital tract malformations in mammals. These effects may be attributed to various classes of chemicals such as chlorinated pesticides (DDT, endrin, pentachlorophenol) or chlorinated aromatic compounds (PCBs, dioxins), metals (cadmium, selenium, zinc, mercury, tributyltin), alkylphenols (nonylphenol, pentylphenol, bisphenol), phytooestrogens. The identification of the chemicals responsible of these reproductive alterations is difficult and demands the development of specific procedures to analyse these compounds in complex environmental mixtures. Moreover the causal relationships between the exposure to these substances by wildlife organisms and the adverse effects on reproduction in the environment are not yet clear evidence.
http://www.edpsciences.org内分泌干扰物:分析和毒理学方面在过去5年中,对环境中影响人类和动物生殖能力的化学品的关注有所增加。生殖激素受体系统似乎特别脆弱。野生动物的荷尔蒙紊乱包括河鱼和海螺的性别改变,鸟类的生殖失败,哺乳动物的生殖道畸形。这些影响可归因于各种化学物质,如氯化农药(滴滴涕、内啡肽、五氯苯酚)或氯化芳香族化合物(多氯联苯、二恶英)、金属(镉、硒、锌、汞、三丁基锡)、烷基酚(壬基酚、戊基酚、双酚)、植物雌激素。鉴定导致这些生殖变化的化学物质是困难的,需要开发特定的程序来分析复杂环境混合物中的这些化合物。此外,野生生物接触这些物质与环境中对生殖的不利影响之间的因果关系尚未有明确的证据。
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引用次数: 1
Optimization of the degradation of sewage sludge by wet air oxidation. Study of the reaction mechanism on a cellulose model compound 湿式空气氧化法降解污泥的优化研究。纤维素模型化合物的反应机理研究
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000159
N. Ricq, S. Barbati, M. Ambrosio
The aim of this work is to optimize the degradation yield of an activated sludge and to study the reaction mechanism on a cellulose model compound. This optimization is performed with a Simplex design with four parameters: reaction temperature (280- 350 °C), injected air pressure (40-60 MPa), reaction time (10-45 minutes) and COD concentration (0.5-5 g L -1). The better yield obtained on TOC concentration is 82 5% at 330 °C. Over this temperature, the yield substantially decreases. The use of cellulose a s a model compound for activated sludge confirms optimization results and leads to the identification of by-products and free rad ical species participating in the reaction. Two major organic compounds have been detected: 4-oxo pentanoic acid and 3-oxo butanoic acid, and three types of radicals: HO°, CO 2° -and °CH(OH)CH3.
本工作的目的是优化活性污泥的降解率,并研究纤维素模型化合物的反应机理。该优化采用Simplex设计,包括四个参数:反应温度(280- 350°C),注入空气压力(40-60 MPa),反应时间(10-45分钟)和COD浓度(0.5-5 g L -1)。在330℃条件下,TOC的收率为82.5%。超过这个温度,产率就大大降低。纤维素作为活性污泥的模型化合物的使用证实了优化结果,并导致了参与反应的副产物和自由基的鉴定。检测到两种主要的有机化合物:4-氧戊酸和3-氧丁酸,以及三种自由基:HO°、CO 2°和CH(OH)CH3。
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引用次数: 9
Use of high surface area TiO$_2$ for preconcentration and following determination of Cr species by on-line flow injection inductively coupled plasma atomic emission spectrometry 在线流动注射电感耦合等离子体原子发射光谱法,利用高比表面积tio_2进行预富集和后续测定
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000160
E. Vassileva
A flow-injection analysis (FIA) system incorporating two microcolumns of TiO 2 was used for the developing of an on- line method for preconcentration and sequential determination of Cr 3+ and Cr6+ species by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimal conditions for both analytes have been obtained. With a sample volume of 10-50 ml and an elution volume of 500 µl, a signal was 20-100 times higher than the signal given by a continuous aspiration system. The method gave good reproducibility with precisions less than 7 % RSD for 5 replicates at the 10 ng/ml level for both Cr- species. Recoveries between 95 and 98 % were obtained for Cr 3+ and Cr6+. The preconcentration system and the methodology proposed were validated on several natural water samples, on reference water samples as well as on synthetic seawater. It was found that the on-line detection using ICP-AES allows sequential Cr speciation analysis at the low concentration levels (ng/l) usually encountered in these media.
采用两微柱的流动注射分析(FIA)系统,建立了电感耦合等离子体原子发射光谱(ICP-AES)在线预富集和序列测定cr3 +和Cr6+的方法。得到了两种分析物的最佳条件。当样品体积为10-50 ml,洗脱体积为500µl时,信号比连续抽吸系统高20-100倍。在10 ng/ml浓度下,该方法重复性好,精密度小于7% RSD,重复5次。cr3 +和Cr6+的回收率在95 ~ 98%之间。在几种天然水样、参考水样和合成海水中对预富集系统和方法进行了验证。发现使用ICP-AES在线检测可以在这些介质中通常遇到的低浓度水平(ng/l)下进行顺序的Cr形态分析。
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引用次数: 10
Evidence of butyl benzyl phtalate induced modifications in a model system developed in vitro 在体外开发的模型系统中,邻苯二甲酸丁苯酯诱导修饰的证据
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000153
M. Sabbieti, L. Marchetti, R. Curini, G. Menghi, A. Roda, M. V. Russo, C. Nugnes, S. Materazzi
The phtalate induced modifications on osteoblastic cells have been monitored in a model system in vitro: preliminary encouraging results, independently obtained by calorimetry (DSC), confocal laser scanning microscopy (CLSM) and coupled gas chromatography-mass spectrometry (GC-MS), show the possibility to relate kinetic data and immunofluorescence images, that are very useful to show the entry and the localization of phtalate into the cells. The calorimetric data were obtained by a cellula r liv- ing system growth and reacting into the aluminium pans.
在体外模型系统中监测了邻苯二甲酸盐对成骨细胞的诱导修饰:通过量热法(DSC)、共聚焦激光扫描显微镜(CLSM)和耦合气相色谱-质谱法(GC-MS)独立获得的初步令人鼓舞的结果显示,将动力学数据和免疫荧光图像联系起来的可能性,这对显示邻苯二甲酸盐进入细胞和定位非常有用。量热数据是通过细胞活系统生长和与铝锅反应得到的。
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引用次数: 7
Determination of glyphosate herbicide and (aminomethyl)phosphonic acid (AMPA) in water by liquid chromatography and fluorescence detection. Part II: Direct determination using pre-column derivatization with NBD-Cl. 液相色谱法和荧光检测法测定水中草甘膦除草剂和(氨基甲基)膦酸。第二部分:用NBD-Cl柱前衍生直接测定。
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000149
R. Colin, E. L. Fur, C. Charreteur, C. Dufau, J. Peron
An analytical method was developed for the determination of glyphosate and AMPA in water. This method involves derivatization in situ with NBD-Cl reagent at 60 °C. The quantification is performed using liquid chromatography with fluores- cence detection after a separation on an amino column. The limit of quantification was estimated at 1 µg/L level for glyphosate and at 0.1 µg/L level for AMPA.
建立了测定水中草甘膦和AMPA的分析方法。该方法包括在60°C下用NBD-Cl试剂原位衍生化。定量是在氨基柱分离后用荧光检测的液相色谱法进行的。草甘膦的定量限为1µg/L, AMPA的定量限为0.1µg/L。
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引用次数: 8
Pyrolysis-mass spectrometry for rapid classification of oysters according to rearing area. 牡蛎养殖区热裂解-质谱法快速分类。
Pub Date : 2000-11-01 DOI: 10.1051/ANALUSIS:2000150
M. Cardinal, C. Viallon, C. Thonat, J. Berdagué
Current concern for the safety and traceability of food, as well as the desire of oyster farmers, for marketing reason, to emphasise the geographical origin of their production, requires new methods to make possible a real product identification. I n this study, 181 oyster samples were analysed to determine their origin area. These samples were collected in nine French rear- ing areas at four different times of the year (spring, summer, and the beginning and end of autumn) and from four to eight sites in each area to provide a variability parameter. Analysis of fingerprints after Curie point pyrolysis-mass spectrometry, by an a rti- ficial neural network gave a mean classification rate of 89 %. Although the technique requires further improvements, it appears to be a useful discriminative tool for rapid identification of an oyster production area.
目前对食品安全和可追溯性的关注,以及牡蛎养殖者出于市场原因强调其生产的地理来源的愿望,需要新的方法来实现真正的产品识别。在这项研究中,对181个牡蛎样本进行了分析,以确定它们的原产地。这些样本是在一年中的四个不同时间(春季、夏季、秋初和秋末)从法国九个后方地区的4到8个地点收集的,以提供变异性参数。利用人工神经网络对居里点热解-质谱分析后的指纹进行分类,平均分类率为89%。虽然该技术需要进一步改进,但它似乎是一种有用的判别工具,可以快速识别牡蛎产地。
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引用次数: 9
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Analusis
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