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1.
Determination of trace residues of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDDs and PCDFs) in various matrixes is carried out by a limited number of laboratories in the United States, Canada, and other countries. Current methods for analysis of foods and biological tissues include a combination of preparation, extraction, cleanup, isolation, determination, and identity confirmation procedures. Soxhlet, liquid/liquid, solid-phase, and column extraction procedures are used as well as treatment with acid or base before solvent extraction. Cleanup and isolation steps include sulfuric acid partitioning; adsorption chromatography on Florisil, silica gel, or alumina; gel permeation chromatography; multi-stage column chromatography on sulfuric acid silica and alkali silica; carbon column chromatography; and liquid chromatography fractionation with size exclusion, normal-phase, and reverse-phase columns. Activated carbon and multistage chromatographic columns are widely used in cleanup schemes. Isomer-specific identification and quantitation of PCDD and PCDF congeners at parts-per-trillion levels or lower are carried out by high resolution (capillary) gas chromatography (HRGC) and multiple ion detection mass spectrometry. In addition to chemical methods, bioassay procedures have been recommended (e.g., use of monoclonal antibodies, for immunoassay determination of PCDDs and PCDFs).  相似文献   

2.
A comprehensive review of the single and sequential extraction schemes for metal fractionation in environmental samples such as soil and industrially contaminated soils, sewage sludge and sludge amended soils, road dust and run off, waste and miscellaneous materials along with other approaches of sequential extraction methods are being presented. A discussion on the application of chemometric methods in sequential extraction analysis is also being given. The study of single and sequential extraction methods for various reference materials are also being looked into. The review covers several aspects of the single and sequential extraction methodologies. The use of each reagents involved in these schemes are also discussed briefly. Finally the present upto date information by different workers in various fields of environmental geochemistry along with the possible future developments are also being outlined.  相似文献   

3.
Soil organic matter (SOM) consists of various functional pools that are stabilized by specific mechanisms and have certain turnover rates. For the development of mechanistic models that predict changes in SOM storage, these pools have to be quantified and characterized. In the past, numerous fractionation schemes have been developed to separate and analyse such SOM fractions. In this review, the SOM fractions obtained with such operational fractionation procedures are described in terms of their pool sizes, chemical properties, and turnover rates. The main objective of this review is to evaluate these operationally defined fractions with respect to their suitability to describe functional SOM pools that could be used to parameterize SOM turnover models. Fractionation procedures include (1) physical separation of SOM into aggregate, particle size, and density fractions and fractions according to their magnetic susceptibility, and (2) various wet chemical procedures that fractionate SOM according to solubility, hydrolysability, and resistance to oxidation or by destruction of the mineral phase. Furthermore, combinations of fractionation methods are evaluated.The active SOM pool with turnover rates <10 years may best be represented by the soil microbial biomass and the light fraction (<1.6-2 g cm−3) obtained by density fractionation (if black carbon contents are considered). Most chemical and physical fractionations as well as combinations of methods yield SOM fractions that are not homogeneous in terms of turnover rates. It has proven to be particularly difficult to isolate functional fractions that represent the passive model pools in which the majority of soil SOM is stabilized. The available fractionation methods do not correspond to specific stabilization mechanisms and hence do not describe functional SOM pools. Another problem is that comprehensive data for turnover rates and data for whole soil profiles are only now becoming available, especially for new fractionation methods. Such information as well as the use of specific markers and compound-specific isotope analysis may be important for future differentiation and evaluation of functional SOM fractions.  相似文献   

4.
Abstract

In this study, a strong association between cobalt (Co) and manganese (Mn) in different geochemical soil phases (fractions) was evaluated using a continuous‐flow sequential extraction technique employing a modified Tessier extraction scheme. With the flow system, detailed extraction profiles of Co and Mn in soils could be obtained by plotting concentrations of the elements extracted against extraction time (plots referred to as extractograms). Extractograms may be used as an indicator of whether the elements dissolving in the same extraction step are closely associated, or are merely extractable with the same reagent. From the soil samples studied, the coincidence of Co and Mn peaks seems to indicate a close association of these elements in the exchangeable, reducible, and oxidizable fractions. Analysis of flow extraction data suggested that the association between Co and Fe is not as strong as reported in previous studies based on the statistical analysis of batch fractionation data.  相似文献   

5.
Trace Elements in Soils of Urban Areas   总被引：2，自引：0，他引：2  
Urban soils are an essential element of the city environment. However, studies on urban soils are scattered in terms of geographical distribution, sampling pattern, analytical dataset, etc. One of the major issues arising from the studies on this ecosystem is the diffusion of its contamination. In cities, in fact, the proximity to humans may cause a serious danger for citizens. In the present study, results from the literature about trace elements in urban soils are presented to compare methodologies and results and to offer a basis for the harmonization of investigation approaches and establishment of remediation thresholds. A total of 153 studies on the urban ecosystem published in the last 10 years were collected and data on trace elements in soils of 94 world cities were compared and discussed. Data highlights the discrepancies among different studies (sampling strategies, analytical procedures) and the extreme variability of urban soils. Most cities are contaminated by one or more trace elements, revealing the environmental relevance of the urban soil system. While Pb is still one of the major concerns in many locations, new contaminants are on the rise and would deserve more attention from the researchers. While in fact some contaminants are almost ubiquitous in world cities and could be used as tracers for urban contamination, some traffic-related elements such as platinum, rhodium, and palladium, whose reactivity and toxicity is still unknown, are becoming of concern. Collation of literature data highlights the need for the harmonization of sampling, analytical, and rendering procedures for regulatory purposes and provides a useful dataset for environmental scientists dealing with the urban ecosystem and for city planners. A sampling design adapted to local urban patterns, a prescribed sampling depth, and a minimum set of elements that deserve to be measured could be the core of a common methodology.  相似文献   

6.
SMS may be obtained from a number of locations and from crops produced in different ways. Consequently such material may be variable in terms of physical structure and chemical analysis. This is important when choosing blends of material for subsequent reuse, including recomposting. Ranges for maximum and minimum values of plant nutrient properties of fresh SMS are outlined. In particular, pH (8.2-7.3), conductivity (2,380-1,410 μS cm?1) and C:N ratio (9-15:1) each vary from sample to sample. Nitrogen availability varies both in terms of organic- and inorganic-N and in the ratio of nitrate-N to ammonium-N. This appears to be a function of duration of cropping and subsequent storage conditions.

Methods for determination and interpretation of plant nutrient content of SMS are discussed. The need for greater standardisation of salt extraction procedures and presentation of published data is discussed.

Changes in composting procedures and Agaricus bisporus substrate recipes demand continuing research into the biology, potential uses and economics of SMS.  相似文献   

7.

Purpose

Analyzing organic pollutants in forest soil is challenging because they are strongly physical and chemical bound to soil organic matter (SOM). Within the framework of a forest soil inventory, an analytical protocol for the determination of polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), and organochlorine pesticides (OCP) should be established and validated using one and the same extraction and cleanup procedure. The protocol should be applicable for reliable analysis of a high number of samples in a short timeframe.

Materials and methods

Two different soil samples representative for the humic layer from a typical mixed and coniferous forest soil had been used for the analysis. Three solvents of different polarity, namely cyclohexane (CH), ethylacetate (EA)/CH (1/1, v/v), and acetone (AC)/CH (2/1, v/v), and the six standard extraction techniques (pressurized liquid extraction (PLE), soxhlet extraction, fluidized bed extraction, sonication, shaking, and one-step extraction recommended for analyzing agricultural soil in Germany (VDLUFA 2008)) were compared concerning their extraction efficiency. For additional matrix separation, two different cleanup procedures (gel permeation chromatography (GPC) and solid-phase extraction (SPE) with different sorbents) were tested. Quantification was carried out using gas chromatography combined with mass spectrometry (GC–MS) and two different injection systems (split/splitless injection and programmable temperature vaporizer (PTV) injection). Labeled internal standards, added prior to extraction, were used for method evaluation.

Results and discussion

For the simultaneous extraction of PAH, PCB, and OCP from organic forest soil PLE with acetone/cyclohexane (2/1, v/v) provided the highest extraction efficiency. A two-step cleanup procedure consisting of GPC followed by SPE with silica gel was entirely sufficient for the separation of humic substances without discrimination of analytes. Recovery rates for the different extraction and cleanup steps ranged between 89% and 106%. For quantification, a GC–MS method was developed using two different injection systems and two capillary columns of different selectivity.

Conclusions

By comparing six standard extraction techniques for PAH, PCB, and OCP from forest soil, we obtained the highest extraction efficiency when using PLE with AC/CH (2/1). For sample injection, we achieved best results using an optimized PTV injection system as it highly reduced the breakdown of thermolabile pesticides. Using this combination of technical equipment, it is possible to determine a concentration of the analytes in the trace level range of 1–2 μg kg?1 in humic soil.  相似文献   

8.
The analysis of literature sources and a database on soil physical properties collected by the Department of Soil Physics and Amelioration of Soils of the Faculty of Soil Science of Moscow State University made it possible to compare three major constituents of the particle-size distribution analysis (PSDA): (a) the classification of soil separates with respect to their sizes and the classification of soil textures, (b) the procedures used to prepare soil samples for the PSDA, and (c) the specificity of the determination of the particle-size distribution by different methods. It was shown that there are good physical and statistical grounds for the conversion of data on the particle-size distribution from the Russian classification system into other systems. Much larger problems are related to the pretreatment of soil samples for the PSDA. The diversity of existing methods, classification schemes, and technical devices based on different physical principles (sedimentation and laser diffractometry) should be taken into account in the analysis and quantitative conversion of particle-size distribution data from a given classification system into another system. The Russian classification of soil textures and soil particle-size groups developed by N.A. Kachinskii has certain advantages and can be easily converted into other systems. In the choice of a particular system, it is important to take into account the goals of the study. Agreement between soil scientists concerning the major constituents of the PSDA has to be reached.  相似文献   

9.

Background, aim, and scope  

Despite the contribution of many sequential P fractionation schemes to the study of P transformations in agricultural soils, the nature of P in each fraction remains qualitative rather than mechanistic. This study used the sequential extraction and isotopic dilution techniques to assess the recovery of a tracer (32P) in soil P fractions and to elucidate the transformation of soil P in different P pools and its lability.  相似文献   

10.
We compared Cr, Cu, Ni and Zn fractionation patterns in four typical soils naturally containing high levels of these elements on the tropical volcanic island of Réunion. Two sequential chemical extraction procedures were used: the modified four-stage BCR procedure (subsequently called mBCR) and the modified six-stage Geological Survey of Canada procedure (subsequently called mGSC). The results obtained by these two procedures highlighted some similarities. With both approaches, exchangeable fractions were the smallest fractions with respect to the four heavy metal (HM) distributions (< 5% of the total HM quantity), and residual fractions had the highest Cr, Cu, Ni and Zn contents (39.1–97.9%) in the four soils. In contrast, we noted differences in HM fractions bound to organic matter. These differences could be explained by the different reagents and extraction sequences implemented in the two procedures. However, the most marked difference in the results obtained by the two procedures concerned the HM fraction bound to oxyhydroxides, despite the fact that the same reagent was used (hydroxylammonium chloride). Our results revealed that the mBCR procedure underestimated the proportion of HM bound to this fraction. The mGSC procedure therefore seems more suitable for analysing tropical soils which typically contain high levels of Fe and Mn oxyhydroxides.  相似文献   

11.
General concepts of tectology—the universal organization science—are discussed. It is shown that some of them can be applied for the formal analysis of visual images of soil systems obtained at different levels of their organization—from photos of thin sections to soil maps—and the corresponding attribute data. The structure of visual and attribute data at the level of thin sections and the methods of their analysis do not differ from those applied upon the analysis of soil cartographic materials. In particular, this concerns the procedures for data classification—the universal tool to analyze empirical data and to generate various hypotheses. These procedures include the methods of multivariate statistics and data convolution, the development of systems of information indices, the development of hierarchical and/or ordinate structures of soil objects, etc. Modern information technologies, including data bases and geographic information systems with solid mathematical support, make it possible to advance the ideas of tectology with the aim to improve the efficiency of theoretical and applied studies in soil science.  相似文献   

12.
土壤磷形态组分分级及31P-NMR 技术应用研究进展   总被引：4，自引：1，他引：3  
农田生态系统中土壤磷形态转化,影响土壤磷对作物的有效供应。土壤磷分为无机磷和有机磷两大部分。化学连续提取法 (chemical sequential fractionation,CSF) 研究土壤磷形态分级,采用不同的化学提取剂,分级提取土壤中组成或分解能力接近的有机无机含磷化合物,是目前表征土壤磷素形态的重要方法。但该方法虽历经改进,仍难以确切反映土壤磷的实际组成,提取的不同磷形态间存在重叠,有机磷和无机磷组分分级存在一定的误差;不同分级磷组分对作物的有效性,需谨慎评估。核磁共振波谱技术 (nuclear magnetic resonance,NMR) 根据核磁共振波谱图上共振峰的位置、强度和精细结构来研究土壤中含磷化合物的分子结构。液相31P-NMR 可以同吋检测出土壤中多种磷组分,如正磷酸盐、磷酸单酯、磷酸二酯、膦酸脂、焦磷酸盐和多聚磷酸盐,识别土壤提取物磷形态,可将有机磷与无机磷分开。本文综述了应用31P-NMR 技术研究土壤磷形态组分的一些进展,总结了样品制备过程、NMR 测试参数及在土壤磷形态转化研究中的应用。二维31P-NMR 技术发展为鉴定分析土壤中更多种类的含磷化合物提供了契机。  相似文献   

13.

Introduction  

Sequential fractionation procedures have been an important tool in the study of phosphorus (P) dynamics in soils and sediments for over 50 years. Throughout this period, the various methodologies have been thoroughly reviewed, and several limitations are widely acknowledged, but there are also aspects of P fractionation that have received little or no discussion. As there are few alternatives to fractionation procedures, in order to advance the usefulness of these techniques, we need to explore the undisclosed variables that may falsely bias our interpretation.  相似文献   

14.
Trace species in atmospheric particles have frequently been used to apportion pollutants in acid rain to their sources by comparing the relative concentrations of trace species at the source and receptor sites. Another approach is to use the trace species in precipitation directly in a source apportionment. This has rarely been done due to the paucity of data on trace species in precipitation and the unknown fractionation of the species during the scavenging process. A study was undertaken to analyze precipitation for a large number of trace species and to compare the concentrations with those in atmospheric particles. Precipitation was collected in Lenox, MA during the summer of 1984. Extreme measures were taken to avoid contamination during collection and analysis. Using five analytical methods, including the novel method of freeze-drying the precipitation followed by neutron-activation analysis, 31 species were analyzed in the rain. The trace concentrations measured in this study were lower than those found in earlier studies, where contamination was believed to be a problem. Concentrations of trace species in the precipitation were compared with those in atmospheric particles. A few species were enriched in precipitation relative to particles, including some large-particle species (Ca, Ti, Fe) and species with gaseous precursors (SO4, NO3, Br). Due to this enrichment, these species should be carefully considered before using them in source apportionment calculations. However, most species showed similar enrichments in precipitation and in atmospheric particles, suggesting that negligible fractionation had taken place during the scavenging process. These species could be used effectively in the future to apportion the pollutants in precipitation to their various sources.  相似文献   

15.
Changes in land use alter the natural cycling of phosphorus (P) in soil. Understanding the chemical nature of these changes is important when developing sustainable management practices for cultivated soils. In this study, we evaluated the ability of commonly used laboratory methods to characterize land use–induced changes in various P pools. Also, the characteristics of soil P revealed by different methods are discussed. Soil samples were taken from three differently managed field plots of the same clay soil: uncultivated grassland and organic and conventional crop rotations. Soil P reserves were characterized using Chang and Jackson and Hedley sequential fractionation procedures and by sodium hydroxide (NaOH)–ethylenediaminetetraacetic acid (EDTA) extraction followed by 31P NMR spectroscopy. Both of the tested fractionation methods identified differences in the P pools and provided evidence regarding land use–induced changes. However, the 31P NMR analysis suggests that the quality of organic P in this soil was not affected by the change in land use.  相似文献   

16.
Gas chromatography coupled with mass spectrometry (GC-MS) using both electron impact and chemical ionization detection modes led to the determination of the volatile composition of two samples of freshly distilled Cognac and two samples of freshly distilled Calvados. A total of 169 volatile compounds were directly identified in dichloromethane extracts obtained by liquid-liquid extraction. Trace compounds present in both spirits were characterized with the help of preparative separations. In a first step, groups of compounds were separated by preparative GC, and the fractions were analyzed on a polar stationary phase by GC-MS. In a second step, silica gel fractionation was used to separate them by polarity. In this study, 331 compounds, of which 162 can be considered as trace compounds, were characterized in both freshly distilled Cognac and Calvados. Of these, 39 are common to both spirits; 30 are specific to Cognac with numerous hexenyl esters and norisoprenoidic derivatives, whereas 93 are specific to Calvados with compounds such as unsaturated alcohols, phenolic derivatives, and unsaturated aldehydes.  相似文献   

17.
Density fractionation along with ultrasonic dispersion is widely applied in soil science to obtain distinct fractions of soil organic matter. Density cut‐off and dispersion energy are crucial parameters to yield fractions closely corresponding to their conceptual definitions. Our literature review revealed methodological discrepancies in the utilization of density‐fractionation schemes. Strikingly, reasons for the selection of specific density or dispersion energy were rarely explained. Thus, it is not known how results of different approaches relate to each other. We therefore recommend testing and reporting effects of fractionation parameters on chemical and physical properties of fractions, to achieve agreement and coherence on parameters to be used and facilitate comparability in future studies.  相似文献   

18.
Abstract. The hierarchial concept of land use planning becomes less relevant in a society with continuous interactions between stakeholders, researchers, planners and politicians. In this context, land use negotiation rather than land use planning appears to be the most appropriate concept. In the negotiation process, good quality data about the land is important as land properties are, obviously, key elements to be considered. Case studies at farm and regional level have been analysed to explore answers to a number of questions. How can soil data be presented most effectively? What are the research needs? How can the large existing body of data be mobilized most effectively? Studies on regional land use in Costa Rica used methods in a logical sequence including projections, explorations and predictions of land use patterns. The work involved upscaling of data, obtained at farm level, to the regional level. Work at farm level focussed on prototyping procedures in which farming systems were ‘designed’ by close interaction between farmers and scientists, including applications of precision agriculture. Soil data demands were analysed, emphasizing the effects of using data with different degrees of detail together with the application of pedotransfer functions which effectively transform existing data into parameters that are difficult or expensive to measure directly. This not only facilitated interactions with stakeholders but also with colleague scientists in interdisciplinary teams. In addition, use of Geographical Information Systems allowed visual presentations of alternative geographical land use patterns that were associated with various scenarios, thereby facilitating the interaction processes. A plea is made to increase interaction of stakeholders and researchers by considering research programmes as vehicles for joint learning.  相似文献   

19.
The objectives of this research study were to isolate, evaluate, and compare the fine structures of starch fractions obtained from a wild‐type (normal) corn starch and amylose‐extender25, dull39, sugary2, and sugary1 corn mutants in the same genetic background using three different fractionation procedures based on gel‐permeation chromatography or alcohol‐precipitation methods. Starch fractions obtained from each of the three methods were enzymatically debranched and analyzed using high‐performance anion‐exchange chromatography with a postcolumn amyloglucosidase reactor and a pulsed amperometric detector. The separations were performed by fractionation on a GPC column, by precipitation with 1‐butanol, and by preferential precipitation with 1‐butanol and isoamyl alcohol. Using any of these methods, no apparent differences in the molecular weight distributions of amylopectin or of amylose among the different starches were observed. The proportions of branch chain lengths of the starch components obtained by the various fractionation methods were very similar among methods for each of the starch types analyzed, such as the predominance of long branch chains in ae25 corn and that of the short branch chains in su2 corn. Overall, the effect of the corn mutations was more important to the differences observed among the starch types than was the method of fractionation used.  相似文献   

20.
In recent years, lanthanides (Ln) have become an object of active studies by soil scientists and geologists, which is favored by the development of instrumental equipment. It has become possible to obtain reliable soil clarkes of lanthanides. The study of lanthanides in soils is important not only from the theoretical and pedogenetic viewpoints but also because of its applied value, as Ln-containing substances and wastes are used as microfertilizers. The established fact of the geochemical fractionation of lanthanides in soils and rocks appears to be one of the latest significant achievements. The tetrad-effect in lanthanides was revealed and theoretically substantiated. Strong positive anomalies of the Ce content and weak anomalies of the Eu content were found in soils (unlike many rocks). Ferromanganese soil concretions are depleted in Y as compared with light-weight lanthanides. The type of lanthanide fractionation in the course of soil formation in different zones depends on the content of Ln-minerals in the parent rock. In the zone of supergenesis, Mn oxides are among the most important Ln-bearing phases, many of which (Ce, in particular) are classified as manganophilic. In calcite, Ca2+ may be replaced by lanthanides, including Y. Humus acids stabilize Ce3+ and prevent positive cerium anomalies in the newly formed bodies. Microorganisms favor Ln accumulation in biogenic bodies, such as Fe-Mn nodules and Fe-ocher.  相似文献   

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