An overview of the present state of standardization of soil sampling in Spain

There are no national standard soil sampling guidelines at present in Spain, although a strong need for standardization of sampling activities is evident. Some relevant publications dealing with sampling subjects are cited, and common practices in sampling and sample pre-treatment carried out in Spain for basic soil maps, soil fertility and soil contamination are briefly described. The need to standardize sampling protocols and guidelines in Spain and to harmonize them with those of the EU countries is emphasized.     

The Austrian soil sampling procedure tested in a field study (CEEM-project)

The Austrian soil sampling procedure requires sampling from representative, uniform areas. For chemical analyses a composite sampling procedure is proposed in which 15-25 single samples should be distributed evenly over the area. Sampling depth for top soils varies between 5 and 30 cm depending on land use. In a field experiment, the suitability and reliability of this sampling method for the determination of trace elements in soil was tested. A high degree of accordance with the results of the extensive and systematic CEEM-Reference Sampling Method was found; therefore the Austrian sampling procedure is recognized as a simple but valid method which can be also proposed as a basis for corresponding ISO- or CEN-Standards.     

Objectives, concept and design of the CEEM soil project

Within the member countries of the European Union, different strategies and guidelines for the sampling and the preparation of soils are used to investigate soil contamination. As a consequence, there is reasonable doubt that the results gained by applying these different strategies and methods are comparable. In general, the relative contribution of sampling and sample preparation to the total uncertainty in soil contamination studies is a subject of speculation than of knowledge. For this purpose, the first European soil sampling inter-comparison test was organised as a project under the Standards, Measurement and Testing Programme of the European Commission. The aim of this project was to analyse and to compare the existing guidelines, the degree and the state of standardisation in this field in the European countries, and to compare their results when applied on the same test area under comparable conditions by representative sampling teams. The results of the project in general demonstrate that sampling and sample preparation errors reach about the same order of magnitude as errors caused in the chemical analysis. However, there are great differences depending on the elements investigated and their concentration ranges, as well as on pedological and land-use conditions in the test area. Consequently, sampling and sample preparation require the same attentiveness and equivalent measures for quality assurance (QA) and quality control (QC) as the chemical analysis, which has not been the case up to now. Insufficient comparability of the results is illustrated by the fact that different participants arrive at different conclusions for up to 61% of tested soil quality criteria (e.g. threshold levels). The methods and results of the project are presented in detail in the six following papers within this volume. The following 13 papers present some key studies and specific contributions of the participants, as well as synoptical papers of the invited experts in standardisation and accreditation.     

Quantitative evaluation of the CEEM soil sampling intercomparison

The aim of the CEEM soil project was to compare and to test the soil sampling and sample preparation guidelines used in the member states of the European Union and Switzerland for investigations of background and large-scale contamination of soils, soil monitoring and environmental risk assessments. The results of the comparative evaluation of the sampling guidelines demonstrated that, in soil contamination studies carried out with different sampling strategies and methods, comparable results can hardly be expected. Therefore, a reference database (RDB) was established by the organisers, which acted as a basis for the quantitative comparison of the participants' results. The detected deviations were related to the methodological details of the individual strategies. The comparative evaluation concept consisted of three steps: The first step was a comparison of the participants' samples (which were both centrally and individually analysed) between each other, as well as with the reference data base (RDB) and some given soil quality standards on the level of concentrations present. The comparison was made using the example of the metals cadmium, copper, lead and zinc. As a second step, the absolute and relative deviations between the reference database and the participants' results (both centrally analysed under repeatability conditions) were calculated. The comparability of the samples with the RDB was categorised on four levels. Methods of exploratory statistical analysis were applied to estimate the differential method bias among the participants. The levels of error caused by sampling and sample preparation were compared with those caused by the analytical procedures. As a third step, the methodological profiles of the participants were compiled to concisely describe the different procedures used. They were related to the results to find out the main factors leading to their incomparability. The outcome of this evaluation process was a list of strategies and methods, which are problematic with respect to comparability, and should be standardised and/or specified in order to arrive at representative and comparable results in soil contamination studies throughout Europe. Pre-normative recommendations for harmonising European soil sampling guidelines and standard operating procedures have been outlined in Wagner G, Desules A, Muntau H, Theocharopoulos S. Comparative Evaluation of European Methods for Sampling and Sample Preparation of Soils for Inorganic Analysis (CEEM Soil). Final Report of the Contract SMT4-CT96-2085, Sci Total Environ 2001;264:181-186. Wagner G, Desaules A, Munatu H. Theocharopolous S, Quevauvaller Ph. Suggestions for harmonising sampling and sample pre-treatment procedures and improving quality assurance in pre-analytical steps of soil contamination studies. Paper 1.7 Sci Total Environ 2001b;264:103-118.     

Harmonisation and quality assurance in pre-analytical steps of soil contamination studies--conclusions and recommendations of the CEEM Soil project

The paper summarises the project's results and consequences including expert's statements. Based on sampling strategies and methodological details which have been recognised to be critical for the comparability of the results of soil contamination studies, recommendations are given towards harmonisation of soil sampling guidelines, improvement of quality assurance of pre-analytical steps and inclusion of soil sampling into accreditation systems. Recommended approaches to improve QA and QC in soil sampling are: harmonised guidelines; specified SOPs; written sampling (strategy) plans; defined qualification and experience of sampling personnel; sampling records; regular interlaboratory comparisons (proficency tests) for sampling; and inclusion of sampling and sample preparation into accreditation procedures. Needs for further research in the field of pre-analytical phases of soil contamination studies are outlined and further R&D projects are encouraged.     

A soil sampling strategy for mapping trace element concentrations in a test area

A sampling strategy, based on previous knowledge of a test area, was compared with a Reference Sampling in the frame of the EU-funded CEEM project. The aim was a comparison of sampling strategies for the drafting of concentration maps for a set of trace elements (Cd, Pb, Cu and Zn), with three-dimension information that can be used for risk assessment. The main constraint was that only 15 soil samples were to be analysed. The test area (in Dornach, Switzerland) included different soil types and land uses (forest, arable land and permanent grasslands). The sampling strategy proposed defined strata on the basis of land use, then applying a systematic regular sampling within each stratum. A composite sample was formed from each individual sample. In forests, H and Ah horizons were taken separately. In arable lands, a depth within the ploughed layer (0-15 cm) was analysed. In grasslands, samples were taken at two depths (0-10 and 10-20 cm) to provide information on the vertical variability. The comparison of the results obtained with those derived from the Reference Sampling allowed us to estimate if the information obtained from the proposed sampling strategy was sufficiently representative for an assessment of the level of elements considered. It was concluded that recommendations on sampling strategy depend on the interaction pattern of the element. In this case, for mobile trace elements, such as Cd, the information derived from sampling of two soil layers was not as important as that for the rest of metals studied that accumulated in the upper layer. If the H horizons in forests was not considered this led to unreliable predictions of the concentration levels, since the concentrations in H and Ah horizons differed irrespective of whether they were expressed in mg kg(-1) (the H horizon was enriched in those trace elements, except for Cd) and in mg m(-2) (the low bulk density of the H horizon led to a lower trace element level than in Ah horizon). Finally, in undisturbed systems such as grasslands, sampling 0-10 cm instead of 0-20 cm is recommended to prevent dilution of the concentration of trace elements.     

Implications of soil complexity for environmental monitoring

International proposals for national soil and environmental monitoring lack adequate awareness of the diversity and complexity of soils. These need to be considered in sampling and reporting. This paper provides examples of the diversity and complexity of soil and environmental conditions in Bangladesh and Ghana, including differences between physiographic regions, within soil toposequences, between and within neighbouring fields, and in areas of shifting cultivation. These examples show that large numbers of sites would need to be sampled and monitored to provide the information required for the national environmental accounting envisaged. Detailed studies are needed in countries with relevant soil monitoring capacities to determine the scale of sampling required and the feasibility of conducting national monitoring. Where the latter is considered infeasible, the contribution that more limited measures could make to environmental monitoring needs to be examined. There is scope for useful academic studies to be made of environmental variability and practical monitoring techniques.     

Guidelines for sampling in Flanders (Belgium)

In Flanders, sampling guidelines for investigations on contamination of soils are in development. One detailed sampling guideline is currently available with respect to the prospective investigation in the frame of the decree related to soil sanitation. Four strategies for sampling may be followed as a function of available information about pollution sources. Guidelines indicate what has to be sampled (top soil, deeper soil, soil water), how sampling points must be determined, how the number of samples and analyses is determined and what parameters need to be analysed. The example given shows that sampling guidelines will strongly depend on the ultimate goal of a particular sampling. A sampling procedure should be developed with close consideration of practical aspects and limitations, in order to be practical, realistic and cost-effective.     

Application of phytotoxicity data to a new Australian soil quality guideline framework for biosolids

To protect terrestrial ecosystems and humans from contaminants many countries and jurisdictions have developed soil quality guidelines (SQGs). This study proposes a new framework to derive SQGs and guidelines for amended soils and uses a case study based on phytotoxicity data of copper (Cu) and zinc (Zn) from field studies to illustrate how the framework could be applied. The proposed framework uses normalisation relationships to account for the effects of soil properties on toxicity data followed by a species sensitivity distribution (SSD) method to calculate a soil added contaminant limit (soil ACL) for a standard soil. The normalisation equations are then used to calculate soil ACLs for other soils. A soil amendment availability factor (SAAF) is then calculated as the toxicity and bioavailability of pure contaminants and contaminants in amendments can be different. The SAAF is used to modify soil ACLs to ACLs for amended soils.The framework was then used to calculate soil ACLs for copper (Cu) and zinc (Zn). For soils with pH of 4-8 and OC content of 1-6%, the ACLs range from 8 mg/kg to 970 mg/kg added Cu. The SAAF for Cu was pH dependant and varied from 1.44 at pH 4 to 2.15 at pH 8. For soils with pH of 4-8 and OC content of 1-6%, the ACLs for amended soils range from 11 mg/kg to 2080 mg/kg added Cu. For soils with pH of 4-8 and a CEC from 5-60, the ACLs for Zn ranged from 21 to 1470 mg/kg added Zn. A SAAF of one was used for Zn as it concentrations in plant tissue and soil to water partitioning showed no difference between biosolids and soluble Zn salt treatments, indicating that Zn from biosolids and Zn salts are equally bioavailable to plants.     

Applied bearing pressure beneath a reinforced soil foundation used in a geosynthetic reinforced soil integrated bridge system

Geosynthetic reinforced soil integrated bridge system (GRS-IBS) design guidelines recommend the use of a reinforced soil foundation (RSF) to support the dead loads that are applied by the reinforced soil abutment and bridge superstructure, as well as any live loads that are applied by traffic on the bridge or abutment. The RSF is composed of high-quality granular fill material that is compacted and encapsulated within a geotextile fabric. Current GRS-IBS interim implementation design guidelines recommend the use of design methodologies for bearing capacity that are based around rigid foundation behavior, which yield a trapezoidal applied pressure distribution that is converted to a uniform applied pressure that acts over a reduced footing width for purposes of analysis. Recommended methods for determining the applied pressure distribution beneath the RSF for settlement analyses follow conventional methodologies for assessing the settlement of spread footings, which typically assume uniformly applied pressures beneath the base of the foundation that are distributed to the underlying soil layers in a fashion that can reasonably be modeled with an elastic-theory approach. Field data collected from an instrumented GRS-IBS that was constructed over a fine-grained soil foundation indicates that the RSF actually behaves in a fairly flexible way under load, yielding an applied pressure distribution that is not uniform or trapezoidal, and which is significantly different than what conventional GRS-IBS design methodologies assume. This paper consequently presents an empirical approach to determining the applied pressure distribution beneath the RSF in GRS-IBS construction. This empirical approach is a useful first step for researchers, as it draws important attention to this issue, and provides a framework for collecting meaningful field data on future projects which accurately capture real GRS-IBS foundation behavior.     

Analytical investigation of disturbance of seabed-sampled soil specimens and its influence on unconfined strength

In view of the need to utilize ocean space and to develop seabed resources, the assessment of the stability of deep seabed soil has emerged as an important challenge in the field of geomechanics. To study seabed stability, the strength and stiffness of the natural ground must be ascertained. Accordingly, it is necessary either to conduct laboratory testing on soil specimens sampled from the seabed or to estimate the strength and stiffness by in-situ tests. While in the future it may be reasonable to conduct in-situ tests to estimate the stiffness and strength of seabed soil, it will still be necessary to compare the physical properties measured by in-situ testing with those measured by laboratory testing in advance of these determinations. In short, soil specimens must be sampled from the actual deep seabed, and laboratory mechanical tests must be conducted on the sampled soil specimens. However, soil sampled from the ocean bottom is subject to effects that differ from those exerted on soil sampled from the earth. More specifically, the non-negligible effects of disturbance are expected with soil sampled from the ocean bottom. The effects of disturbance occur during the sampling process due to the vaporization of dissolved gases, as these soil specimens are under relatively higher pressure and contain pore water with a high amount of dissolved gases. Therefore, numerical simulations were conducted in the present study to investigate the effects of vaporized dissolved gases on the mechanical behavior of soil specimens during sampling and on the undrained shear strength as determined by laboratory tests. The analyses revealed that the combination of the decreasing effective stress caused by the sampling and factors such as overconsolidation and unsaturation is attributable to the difference between the soil strength ascertained by laboratory testing and the in-situ soil strength.     

Cryptosporidium parvum oocyst inactivation in field soil and its relation to soil characteristics: analyses using the geographic information systems

The need exists to understand the environmental parameters that affect inactivation of Cryptosporidium parvum oocysts in soil under field conditions. The inactivation of C. parvum oocysts placed in the natural environment was studied at a dairy farm in western New York State, USA. Seventy sampling points were arranged in a grid with points 150 m apart using the Geographic Information System. The sampling points were distributed among three distinct areas: woodland, corn field and pasture. Purified oocysts were inoculated into chambers filled with soil from each sampling point, and buried in the surface of each respective sampling point. To compare C. parvum oocyst survival with another organism known to survive environmental stresses, Ascaris suum eggs were also placed in soil contained in chambers and buried at the same sampling points as the oocysts. As controls oocysts and eggs in distilled water were also placed at each sampling point. Oocyst and egg viability, soil pH and percent gravimetric water content were measured at all sampling points at 0, 60 and 120 day sampling periods. Soil organic content was determined for each sampling point. At 120 days after placement, mean viability of C. parvum oocysts was 10% although at a few sampling points, 30% of oocysts were still potentially infective; whereas 90% of A. suum eggs were viable at all sampling points. Statistically significant differences were not observed among the three different sampling areas, and no statistically significant predictors were found by regression analysis. Results exemplified the heterogeneity of soil parameters and oocyst viability across a landscape; such results make predictive models for C. parvum inactivation problematical. The long-term survival of C. parvum oocysts in soil under field conditions, as this study demonstrated, emphasizes their potential as a risk to contaminate surface waters.     

Comparative evaluation of European methods for sampling and sample preparation of soils--the Portuguese contribution

The main purpose of this work was to prepare a Portuguese sampling strategy, according to the existing Portuguese recommendations, for the soil sampling exercise at Dornach in the framework of the CEEM soil project of the SMT Programme of the EU. Within this project, the results obtained from the Dornach study were compared with the results obtained by other European participants and also with the reference sampling. The objective of this comparison was to validate the method used and to evaluate possible factors of uncertainty that may arise from the application of our national guideline as well as possible advantages. Another objective, also important, was to provide information regarding the need for a harmonised procedure within the European Union related to soil sampling and sample preparation of soils. The results obtained were consistent with the results obtained by other participants, however, in the Portuguese recommendations there is a general lack of specific information that may complicate its application to polluted scenarios. In fact, those guidelines are valuable to detect the average contamination of the soil, but they are not useful to identify hot spots or the edge influence in a contaminated land. As a conclusion, the results obtained by the CEEM soil project helped to evaluate the Portuguese sampling plan. This may provide a basis for further standardisation of soil sampling for specific purposes, e.g. contaminated land, and to establish a technical support for criteria used in the accreditation of laboratories for soil sampling.     

轻质土技术在土木工程中的应用

对轻质土材料的制作工艺及其在土木工程中的应用进行了论述,指出了轻质土技术的研究趋势及WEPS混合轻质土及气泡混合轻质土在土木工程中将有广泛的应用前景。     

Retention of organophosphorous insecticides on a calcareous soil modified by organic amendments and a surfactant

Pesticides may affect soil quality since they are applied either directly to the soil or transported from the treated crops. Although the soil is able to partially retain environmental contaminants, the use of organic amendments, such as sewage sludge, peat or surfactants, may increase the retention in the upper soil layers, where the contaminants can be degraded and thus diminish their environmental fate. The effect of adding sewage sludge, peat and humic acids, together with a cationic surfactant to the soil, on the adsorption and desorption of organophosphorous insecticides has been studied. The results indicate that humic acids induce an adsorption increment of the pesticides, while peat and sewage sludge do not significantly affect pesticide adsorption at the dosage applied. The use of a cationic surfactant considerably enhances the insecticide retention. The increase was highest for the combined application of the surfactant and the humic acids. Desorption isotherms are inversely related to the adsorption behaviour, being higher for only soil, lower for soil added with carbon-rich amendments, and drastically reduced when the cationic surfactant is present. Concerning the insecticides, adsorption and desorption are related to their physicochemical properties.     

Analytical aspects of the CEEM soil project

In the past, exercises aiming at an assessment of data uncertainty in environmental analysis were usually restricted to the analysis step, while sampling and pre-analytical sample treatment was largely ignored. Collaborative studies on the quantification of sampling errors require, besides a suitable and well characterized test site, the availability of a reference laboratory for the analysis of all of the samples taken in the context of the study by all participants and also test methods which do not contribute large and variable uncertainties due to long and complex analytical methodologies. Here we summarize the major analytical aspects of a European project on the identification and quantification of sampling influences on the determination of lead, cadmium, copper and zinc in soil. The participant group included the leading soil analysis laboratories in Europe; the test site at Dornach (CH) was well suited for the purpose and showed high metal gradients and differentiated land use. The analytical methods (wavelength-dispersive X-ray fluorescence spectrometry and solid-state Zeeman AAS) used in the study showed stable performance characteristics within the confidence interval of the certified reference materials used for the measurement quality control over the entire project period. Additionally, double-blind tests on split samples showed agreement of data in very narrow limits thus demonstrating the reliability of the reference database.     

软土地基的处理

阐述了软土的概念及特征，分析了软土地基中可能出现的问题，介绍了在国内外应用较广的几种方法，如粉体搅拌法、排水固结、路堤堆压等，以供借鉴。     

土的击实试验影响因素

击实试验是土木工程中不可缺少的试验项目,对击实标准、试样制备、润滑剂、余土高度及土的重复使用5个影响击实成果的因素做了对比试验;同时,对试验结果进行了分析.通过土的击实影响因素对比试验,得出如下结论：随着击实功的增加,最大干密度增大,最优含水量反而减小;土样应采用未使用过的天然土或风干土制备,不允许采用使用过的土进行击实试验;余土高度应控制在4 mm之内;在击实试验中,应在击实筒及护筒内壁均匀地抹上一薄层凡士林,这些研究成果对击实原理的研究及击实试验均有一定的指导作用.     

Biodegradation of endosulfan isomers in broth culture and soil microcosm by Pseudomonas fluorescens isolated from soil

Bacterial isolates from endosulfan-contaminated soil were grown in minimal medium and screened for endosulfan degradation. The isolate which used endosulfan and showed maximum growth was selected for detailed study. Maximum degradation in shake flask culture by Pseudomonas fluorescens was 92.80% of α and 79.35% of β endosulfan isomers in 15?days at 20?mg/L concentration, followed by 50 and 100?mg/L, while the corresponding values in static condition were 69.15 and 51.39%, respectively. Endosulfan concentration degradation declined significantly at 50 and 100?mg/L. Concomitant to degradation, release of chloride ion exhibited positive relation, while pH decreased from 7.0 to 4.53 in agitating and 7.0–5.18 in static condition. The soil microcosm study revealed maximum endosulfan degradation in sterilized soil amended with P. fluorescens. Endosulfan diol and endosulfan ether were among the products of endosulfan metabolism in broth culture, but only endosulfan ether was detected in the soil microcosm. Endosulfan sulphate, a persistent and toxic metabolite of endosulfan, was not detected in either case. The study showed that P. fluorescens could be used effectively for bioremediation of the pesticide contaminated sites.