1、United Nations Economic Commission for Europe(UNECE)Convention on Long-range Transboundary Air Pollution(CLRTAP)International Co-operative Programme on Assessment and Monitoring of Air Pollution Effects on Forests(ICP Forests)MANUAL on methods and criteria for harmonized sampling,assessment,monitori
2、ng and analysis of the effects of air pollution on forests Part XI Soil Solution Collection and Analysis Version 05/2016 Prepared by:ICP Forests Expert Panel on Soil and Soil Solution(Tiina M.Nieminen,Bruno De Vos,Nathalie Cools,Nils Knig,Richard Fischer,Susanne Iost,Henning Meesenburg,Manuel Nicola
3、s,Philip ODea,Guia Cecchini,Marco Ferretti,Ana De La Cruz,Kirsti Derome,Antti-Jussi Lindroos,Elisabeth Graf Pannatier)Nieminen TM,De Vos B,Cools N,Knig N,Fischer R,Iost S,Meesenburg H,Nicolas M,ODea P,Cecchini G,Ferretti M,De La Cruz A,Derome K,Lindroos AJ,Graf Pannatier E,2016:Part XI:Soil Solution
4、 Collection and Analysis.In:UNECE ICP Forests Programme Co-ordinating Centre(ed.):Manual on methods and criteria for harmonized sampling,assessment,monitoring and analysis of the effects of air pollution on forests.Thnen Institute of Forest Ecosystems,Eberswalde,Germany,20 p.+Annex http:/www.icp-for
5、ests.org/manual.htm ISBN:978-3-86576-162-0 Bruno De Vos,Nathalie Cools,Nils Knig,Richard Fischer,Susanne Iost,Henning Meesenburg,Manuel Nicolas,Philip ODea,Guia Cecchini,Marco Ferretti,Ana De La Cruz,Kirsti Derome,Antti-Jussi Lindroos,Elisabeth Graf Pannatier contributed to the elaboration of this r
6、evised manual.The work was co-financed by the European Commission under the LIFE Regulation.All rights reserved.Reproduction and dissemination of material in this information product for educational or other non-commercial purposes are authorized without any prior written permission from the copyrig
7、ht holders provided the source is fully acknowledged.Reproduction of material in this information product for resale or other commercial purposes is prohibited without written permission of the copyright holder.Application for such permission should be addressed to:Programme Co-ordinating Centre of
8、ICP Forests Thnen Institute of Forest Ecosystems Alfred-Mller-Str.1,Haus 41/42 16225 Eberswalde Germany Email:pcc-icpforeststhuenen.de Eberswalde,2016Soil Solution Collection and Analysis Part XI Version 05/2016 CONTENTS 1 INTRODUCTION.3 2 SCOPE AND APPLICATION.3 3 OBJECTIVES.3 4 LOCATION OF MEASURE
9、MENTS AND SAMPLING.4 4.1 SOIL SOLUTION SAMPLING TECHNIQUES.4 4.2 SAMPLING DESIGN AT PLOT SCALE.4 4.2.1 Location of the soil solution sampling points.4 4.2.2 Sampling depths.4 4.2.3 Location and number of replicates.5 4.3 SAMPLING EQUIPMENT AND INSTALLATION.7 4.3.1 Tension lysimetry.7 4.3.2 Zero-tens
10、ion lysimetry.7 4.3.3 Materials suitable for use in lysimeter systems.8 4.3.4 Installation.9 4.4 SAMPLE COLLECTION.10 4.4.1 Determination of the soil solution volume.10 4.4.2 Sampling frequency.11 4.4.3 Protection from spoilage.11 4.4.4 Replacement of collecting vessels.11 4.4.5 Transport.11 5 MEASU
11、REMENTS.12 5.1 MEASUREMENTS AND REPORTING UNITS.12 5.1.1 Selected variables.12 5.1.2 Analysis.15 5.1.3 Reception at the laboratory,initial checks and temporary storage.15 5.1.4 Pre-treatment of the samples.15 5.2 QUALITY ASSURANCE AND QUALITY CONTROL.16 5.2.1 Quality Assurance in the field.16 5.2.2
12、Quality Assurance in the laboratory.16 6 DATA HANDLING.18 6.1 DATA SUBMISSION PROCEDURES AND FORMS.18 6.2 DATA VALIDATION.18 6.3 TRANSMISSION TO CO-ORDINATING CENTRES.18 6.4 DATA PROCESSING GUIDELINES.18 6.4.1 Calculation of leaching fluxes.19 6.5 DATA REPORTING.19 7 REFERENCES.19 ANNEX I THE SOIL W
13、ATER FRACTIONS SAMPLED BY ZERO-TENSION LYSIMETRY,TENSION LYSIMETRY AND CENTRIFUGE DRAINAGE.22 ANNEX II MATERIALS USED FOR THE CONSTRUCTION OF TENSION SOIL WATER SAMPLERS.23 ANNEX III OVERVIEW OF ANALYTICAL EN/ISO METHODS FOR DIFFERENT PARAMETERS IN WATER,SOIL OR PLANT SAMPLES AND EXTRACTS AND DIGEST
14、ION SOLUTIONS.24 Part XI Soil Solution Collection and Analysis ANNEX IV MINOR CHANGES AFTER 2016.27 Soil Solution Collection and Analysis Part XI Version 05/2016 Page 3 1 Introduction In addition to the direct effects of stress factors on the forest canopy,forest condition is also influenced by soil
15、-mediated effects via the tree root system.In this respect,soil solution is the matrix mediating between the solid soil and the roots because all nutrients,as well as toxic compounds,pass into the roots via the soil solution.Thus,soil solution chemistry is a valuable indicator for monitoring the eff
16、ects of air pollution and other stress factors on forest ecosystems.The chemical composition of the soil solution is governed by a range of biogeochemical processes that comprise the input of atmospheric deposition into the soil,interactions between the soil solid and liquid phases and the soil gas
17、phase,soil biological processes,and chemical equilibrium reactions.Determination of the chemical composition of the soil solution provides real-time,continuous information about nutrient availability and the possible inhibition of nutrient uptake caused by the effects of toxic elements(e.g.Al3+)on p
18、lant roots and mycorrhizas.The continuous monitoring of soil solution also provides a direct insight into the relationships between forest condition and environmental stress factors,specifically air pollution(e.g.acidifying deposition)and short-term climatic events,and facilitates the prediction of
19、future trends in soil condition.In addition,determination of the composition of the soil solution,together with the estimation of soil water fluxes,can be used to calculate element fluxes through the soil and the output of compounds from the soil into the groundwater and other ecosystems.Together wi
20、th the assessment of other element fluxes(e.g.litterfall),it is possible to determine input-output budgets of forest ecosystems in relation to deposition,climate change,as well as of forestry management practices.2 Scope and application This part of the Manual aims at providing a consistent methodol
21、ogy for collecting high quality,harmonized and comparable forest soil solution data at selected ICP Forests Level II intensive monitoring plots.Soil solution is assessed at level II and level II core plots,but not at level I.Harmonization of the procedures employed in the collection of soil solution
22、 samples and in the chemical analyses is essential to ensure full comparability of the chemical soil solution data.In order to ensure that the national data is acceptable in the international database,as well as for use in evaluations,the National Focal Centers and their scientific partners particip
23、ating in the ICP Forests programme should follow the methods and procedures outlined in this manual.3 Objectives The harmonised collection and analysis of soil solution at the Level II plots across Europe have the following objectives:1 to determine and monitor long-term trends in soil solution chem
24、istry in response to natural and anthropogenic stress factors(e.g.acidifying deposition,climate change).2 to determine input-output budgets of elements from forest ecosystems in relation to deposition and forestry management practices.3 to quantify the temporal and spatial variability of soil soluti
25、on parameters for the major forest soil types in order to improve the adequacy and precision of soil solution assessment and to understand its dynamics and spatial patterns.Part XI Soil Solution Collection and Analysis Page 4 http:/icp-forests.org/manual.htm The third objective can be obtained only
26、by using a limited selection of intensive monitoring plots equipped with an adequate number of lysimeters.The overall sampling design(e.g.number of replicate samples and sampling depths)should enable the estimation of plot-based averages of element concentrations,variation and precision level requir
27、ed for the statistical verification of differences between plots and of changes over time.4 Location of measurements and sampling 4.1 Soil solution sampling techniques Soil solution can be collected by 1)non-destructive or 2)“semi-destructive”methods.Non-destructive methods involve the installation
28、of a soil solution collector(tension lysimeters)that samples the soil solution at the same point over time.Disturbance to the soil/site associated with the installation of this type of lysimeter is normally relatively minimal and of only short duration.Semi-destructive sampling mainly concerns zero-
29、tension lysimeters,the installation of which can cause major,long-term changes to the soil hydrology and aeration of the sampling point.The most common method used in the ICP Forests soil solution monitoring programme is tension lysimetry.In 2006,72%of all samplers were tension lysimeters.The sampli
30、ng techniques differ considerably with respect to the soil solution fraction sampled,the effects of sampling on the site,as well as the extent to which they provide information about temporal and spatial variation in the properties of soil solution(Haines et al.,1982;Hendershot and Courchesne,1991;M
31、arques et al.1996).The different soil solution fractions sampled by the r techniques are shown in Annex 1.4.2 Sampling design at plot scale 4.2.1 Location of the soil solution sampling points Soil solution sampling with non-destructive and semi-destructive methods(lysimetry)should be carried out on
32、the plots so that soil solution sampling can be integrated with throughfall and litterfall sampling,as well as with soil moisture measurements,i.e.implemented on the same location.If it is not possible to install the lysimeters on the plot they can be placed in the buffer zone surrounding the plot.4
33、.2.2 Sampling depths It is mandatory to sample soil solution at fixed depths because the evaluations to be carried out on soil solution and other ecosystem components will primarily be based on fixed depths(e.g.water and element fluxes and budgets).In addition to the fixed depth interval,the genetic
34、 horizon(s)in which the lysimeters have been installed,should also be reported.The same horizon designations should be used as in the profile description of the plot(see submanual X).The reference point for depth determination is the center(mid-point)of the active sampling zone of the soil solution
35、collector,whatever its type.Tension lysimeters should be installed at three depths(Table 1)at least:1)in the midpoint of the 0-20 cm mineral soil layer(0 cm line=interface between the organic layer and underlying mineral soil)in order to sample the soil solution passing through the organic layer,2)w
36、ithin the rooting zone(mid-point of the lysimeter at 20-40 cm in order to be able to monitor the concentrations of nutrients and toxic elements near the fine roots,and 3)below the rooting zone(mid-point of the lysimeter 40-80 cm layer)in order to be able to Soil Solution Collection and Analysis Part
37、 XI Version 05/2016 Page 5 estimate the output of elements.Note that the sample obtained from these fixed depths represents soil solution from both above and below the fixed depth;during dry periods the volume of soil sampled will be much greater than that during wet periods,i.e.the actual layer of
38、soil sampled can vary considerably.Zero-tension lysimeters should be installed immediately below the organic layer at 0 cm depth,at 20-40 cm and at 40-80 cm.The reason why lysimeters should be installed at fixed depths is because these are the depths of the mandatory soil sampling procedure and the
39、soil moisture probes.In order to sample all relevant pedogenetic horizons,soil solution may be sampled optionally below 80 cm in addition to the mandatory depth intervals.Table 1:Depth agreements of soil solution measurements with other soil assessments Layer type Soil Soil Solution Soil properties
40、Moisture probe Zero-tension Tension lysimeter OFH,Forest floor OL,OF,OH 5 cm thick-(M05,M51,M01,H01)0-5/5-10 0-10 0-20 cm 0-5 cm 0-20 cm(M12,H12)10-20-(M24,H24)20-40 20-40 cm 20-40 cm 20-40 cm(M48,H48)40-80 40-80 cm 40-80 cm 40-80 cm 4.2.3 Location and number of replicates 4.2.3.1 Number of replicat
41、es The number of samples at the same sampling depth required to obtain a plot mean that is within 20%of the population mean,with a confidence level of 95%,is at least 10 for most elements(Grossmann and Kloss,1994,de Vries and Leeters,1994,Manderscheid and Matzner,1995).However,the number of samples
42、required to meet this criterion also varies according to the element/ion in question.The spatial variation of element/ion concentrations in soil solution collected by 20 replicate tension lysimeters and expressed by coefficients of variance as percentages have been reported to range from 12%to 79%(G
43、rossmann and Kloss,1994)and from 5%to 128%(Manderscheid and Matzner,1995).Flster et al.(2003)were able to achieve statistically reliable temporal trends for sulphate and base cations by the use of 3 to 7 replicate lysimeters.Three replicates per depth are mandatory.It is also strongly advised that t
44、wo extra lysimeters are installed at each depth in order to ensure that at least 3 samples are obtained at each sampling.It should be noted that 3 replicate samples provide information on the trends in soil solution chemistry at specific points of the plot,rather than a fully representative estimate
45、 of the site.If soil solution monitoring is being used in input-output budget studies,then it is strongly advised to install at least 10 replicates(see also Bille-Hansen,2002).It is strongly recommended to analyze at least three samples separately from each sampling depth on each sampling occasion.T
46、he soil solution samples have to be stored in a refrigerator/cold room(+5oC).Pooling of soil solution samples from one depth should be avoided because otherwise no information is obtained about the spatial variation(variance)of the results for the depth in question.This information is essential when
47、 investigating time trends at the national or European level.The volume of the soil solution sample should always be recorded.If pooling has to be carried out for financial reasons or in order to obtain sufficient volume for the chemical analyses,then this should be done by combining the whole sampl
48、es or by volume weighting in the laboratory.Pooling to only one sample precludes the estimation of spatial Part XI Soil Solution Collection and Analysis Page 6 http:/icp-forests.org/manual.htm variation and missing values can result in biased means if the spatial variation between the individual lys
49、imeters is high.This problem can be avoided to some extent if the spatial variation between the lysimeters has been quantified in a pilot study or for earlier sampling periods during the soil solution monitoring.The values of missing samples can then be estimated using regression equations.In that c
50、ase these estimated values should be flagged as such in the database.4.2.3.2 Selection of sites for replicates The lysimeters should be randomly or systematically located on the plot or buffer zone in order to obtain a representative sample,although this may be limited by the presence of stones or t