ATHENS 2013 SOIL ANALYSIS REPORT

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1 FRAMME LIFE 08 NAT//GR// ATHENS 2013 SOIL ANALYSIS REPORT FRAMME - LIFE08 NAT/GR/ RHODES

2 FRAMME, Fire Restoration Methodology for Mediterranean Forests - environmental safety & sustainability of 4 interventions in the Rhodes NATURA 2000 site with contract number LIFE08 NAT/GR/ is a project co-financed by 50% by the European Commission s LIFE+ Programme and has a total budget of The management of the project is carried out by Elliniki Etairia Society for Environment & Cultural Heritage acting as Coordinating Beneficiary. Associate Beneficiaries to the Project are The Agricultural University of Athens and the Municipality of Rhodes. Contact Information Agricultural University of Athens 75 Iera Odos str, Votanikos Athens - Greece 1) Laboratory of Agricultural Chemistry and Soil Science Assist. Professor Ioannis Massas Tel: ) Laboratory of Ecology and Environmental Sciences Professor Gerassimos Arapis Tel:

3 Table of Contents 1. Introduction Soil Analysis methods :1 (V/V) soil/water mixture method Calcimeter Bernard method Walkley-Black method Kjeldahl method CH 3 COOΝΗ 4 1N method Results of the soil analysis References... 9

4 1. Introduction The soil analysis of the implementation area comes as a part of Action C5 of the project. Samples from each experimental segment were collected during the field visit of September 2012 offering a recent baseline of data for the comparative assessment of soil quality, before and after the application of sewage sludge. One of the biggest strains caused by fires to a forest area is the destruction of the top soil. This turns water to run off rather than soak in and causes a water balance deficit, as well as soil erosion etc. Consequently, the soil analysis is of big importance because it shows the effects of the fire on soil quality and especially on the change of the organic matter and the impact to the water dynamic of the soil. Moreover, soil analysis can be used to investigate the possibility of pollution caused by the interventions, using indicators such as the presence of heavy metals and the presence of organic pollutants. The absolute values given by these indicators, for each intervention alone as well as in every possible combination, will be available upon completion of the works conducted on the field requiring at least one additional year of monitoring (in order for an equilibrium to be achieved). The scope of this study is to show the soil analysis methods used for the analysis of specific soil properties, as well as the results in values, before and after the application of the intervention methods. Results presented in this report are of the soil quality before its fertilization with treated sewage sludge (refer to GCMS Sludge Analysis Report)

5 2. Soil Analysis methods In order to determine the texture of the soil in the study area, as well as the conciseness in organic matter, the CaCO 3, the ph level of the soil, the available Phosphorus, the total Nitrogen in soil materials, the exchangeable K, the total concentration and the available concentration of heavy metals such us Zn, Cu, Mn and Fe, the following methods have been applied. Table 1. List of the applied methods Property Particle size analysis ph Equivalent CaCO 3 Organic Matter Total Nitrogen Exchangeable Cations Available Phosphorus Total concentration of metals (Zn, Cu, Mn and Fe) Available concentration of metals (Zn, Cu, Mn and Fe) Method Bouyoucos, Hydrometer 1:1 (V/V) soil/water mixture Calcimeter Bernard Modified Walkley-Black method Kjeldahl CH 3 COOΝΗ 4 1N Olsen Aqua regia DTPA 2.1. Bouyoucos hydrometer method The percentage of sand, silt and clay in the inorganic fraction of soil is measured in this method. The method is based on Stoke s law governing the rate of sedimentation of particles suspended in water. The sample is treated with sodium hexametaphosphate to complex Ca++, Al3+, Fe3+, and other cations that bind clay and silt particles into aggregates. Organic matter is suspended in this solution. The density of the soil suspension is determined with a hydrometer calibrated to read in grams of solids per liter after the sand settles out and again after the silt settles. Corrections are made for the density and temperature of the dispersing solution. The apparatus and materials used in this method are the following: 1)Glass cylinders, 1000-ml capacity, 2)Thermometer, Fahrenheit, 3)Hydrometer, Bouyoucos (Fisherbrand Model # c) 4)Electric mixer with dispersing cup 5)Plunger 6)Balance sensitive to 0.01g. The reagents is: Dispersing solution, 5%: Dissolve 50 g of sodium hexametaphosphate, Na6(PO3)6 in deionized water and dilute to 1 liter.

6 As far as the procedure 100 ml of the 5% dispersing solution and 880 ml of deionized water are mixed in a 1000 ml cylinder. This mixture is the blank. (Note: 100 ml ml = 980 ml. This blank is not diluted to 1000 ml; the other 20 ml is the volume occupied by 50 g of soil.). 7.2 Weigh g of soil and transfer to a dispersing cup. The weight is recorded to 0.01g. 100-ml of 5% dispersing solution is then added. A dispersing cup is attached to a mixer and the sample is mixed for sec. The suspension is transferred quantitatively from the dispersing cup to a 100 ml cylinder and filled to the ml mark with deionized water equilibrated to room temperature, or allowed to stand overnight to equilibrate. At the beginning of each set, the temperature is recorded, and the hydrometer reading of the blank, using the procedure described below. To determine the density a plunger is inserted into suspension, and carefully mixed for 30 sec. until a uniform suspension is obtained. The plunger is afterwards removed (begin 40 second timer) and gently inserted the hydrometer into the suspension. The hydrometer should be recorded to reading at 40 sec. This is the amount of silt plus clay suspended. The sand has settled to the bottom of the cylinder by this time. (Repeat for each sample). The hydrometer should be recorded reading again after 6 hours, 52 minutes. This is the amount of clay in suspension. The silt has settled to the bottom of the cylinder by this time :1 (V/V) soil/water mixture method This method determines the ph on a 1:1 (V/V) soil/water mixture (5 g NCR-13 soil scoop/5 ml DI water). Samples are stirred both before and after a 15 minute equilibration period. ph is measured on a Beckman ph meter with glass and calomel reference electrodes calibrated to buffers ph 4 and Calcimeter Bernard method Percentage of calcium carbonate, CaCO (%), is defined as the total carbonates which is contained in 100 g of dry soil. Total carbonates, (CaCO 3, MgCO 3,etc ) are expressed as CaCO 3. The determination of CaCO3 equivalent (%) is based on the volumetric analysis of the carbon dioxide CO2, which is liberated during the application of hydrochloric acid solution HCl 4 N in soil s carbonates and is described with the following reaction: (CaCO3 + MgCO3 etc.) + 2 HCl (CaCl2 + MgCl2 etc.) + H2O + CO2 During the application of the acid into the soil sample a characteristic foaming is observed, evidence of carbon dioxide s liberation and the existence of carbonate salts consequently. The reagents of the method are the Methylorange indicator, the Calcimeter Bernard filling solution, the Solution of HCl 4 Ν and the instrument is the calcimeter Bernard. As far as the procedure is considered 2,00 g of prepared soil sample transferred into the Bernard apparatus conical flask. Afterwards the glass of the apparatus is filled with HCl 4 Ν solution till the ¾ of its height and placed into the conical flask attentively. We should pay

7 attention, that the tubule stays upright with the acid (Solution of HCl 4 Ν) inside. The conical flask is tapped with its particular plug and then the level of the filling solution is set to zero Walkley-Black method The Walkley-Black method is one of the best known of the rapid dichromate oxidation methods. In this procedure, potassium dichromate (K 2 Cr 2 O 2 ) and concentrated H 2 SO 4 are added to between 0.5g and 1.0g (although the range may be up to 1.0g depending on organic carbon content) of soil or sediment. The solution is swirled and allowed to cool prior to adding water to halt the reaction. The addition of H 3 PO 4 to the digestive mix after the sample has cooled has been used to help eliminate interferences from the ferric (Fe 3+ ) iron that may be present in the sample although in most cases, this step is not necessary (Tiessen and Moir, 1993). The chemistry of this extraction procedure is as follows: 2Cr 2 O C H + = 4Cr CO2 + 8H 2 0. (3) It should be noted that the concentrations of the reactants and volumes of solutions are not presented in this text due to the numerous variants available in the published literature, all of which are based upon the Walkely-Black procedure Kjeldahl method According to Kjeldahl method Nitrogen is determined by converting the various nitrogen forms to NH 4 +. To accomplish this, g (depending on the OM level) of air dry soil is digested in 3.5 ml conc. H 2 SO 4 with 1.5 g K 2 SO 4 and 7.5 mg Selenium. This mixture is slowly ramped to 400 C in an electrically heated aluminum block and digested for 2½ hours. The ammonium thus formed is determined colorimetrically by reaction with salicylate in the presence of hypochlorite and nitroprusside to form and emerald green complex. Color intensity is measured on a Technicon AutoAnalyzer at 660 nm. This method only partially converts nitrate, thus samples with high nitrate levels must be pretreated with salicylic acid to ensure complete conversion CH 3 COOΝΗ 4 1N method 5.0 g of air dried soil (<2.0 mm) are placed in a 50 ml centrifuge tube and 25 ml of 1N CH 3 COONH 4 are added and the mixture is shaked for 30 min. Afterwards, the tube is placed in the centrifuge and spined at 2,000 rpm for 10 min. The supernatant is poured to a 50-ml volumetric flask. The procedure is repeated with an additional 25 ml 1N CH 3 COONH 4 and finally the volume is brought up to 50 ml with CH 3 COONH 4. Potassium and sodium

8 concentrations were determined by a flamephotometer while calcium and magnesium concentrations were determined by an Atomic Absorption Spectrometer. According to this method Phosphorus is extracted by shaking 1 g of air dried soil in 20 ml of 0.5 M NaHCO 3, ph 8.5, for 30 minutes. Phosphorus is determined on the filtrate by the molybdate-blue method using ascorbic acid as a reductant. Color development is measured at 880 nm on a Brinkmann PC 600D probe colorimeter Aqua regia method Aqua regia is called the mixture of concentrated nitric (HNO 3 ) and hydrochloric acids (HCL). Metals are extracted by shaking 3 g of air dried soil in 30 ml of 1 N HNO 3 for 1 hour. After centrifugation, the supernatant analyzed for Fe, Al, Mn, Cu, Zn, Cd, Ni, Pb, and Cr by ICP-AES DTPA extraction for Fe, Zn, Cu, Mn These metals are extracted by shaking 10 g of air dried soil for 2 hours in 20 ml of 0.005MDTPA (diethylenetriaminepentaacetic acid). The filtrate is analyzed for Cu, Zn, Fe, Mn, Cr, Cd, Ni, and Pb by ICP-AES. A soil to solution ratio of 1:5 or 1:10 is used for peats and mucks. 3. Results of the soil analysis The results of the soil analysis are concentrated on the following table: Table 2. Table of results Particle size analysis Property Organic Matter 4.35 CaCO 3 (%) 18.6 ph 7.56 Available P(ppm) K (ppm) 250 Total N (%) Total concentration of metals (Zn, Fe, Mn, Cu) Available concentration of metals (Zn, Fe, Mn, Cu) Value Soil Sand(%) Silt(%) Clay(%) Symbol L To be evaluated To be evaluated

9 4. References Bouyoucos, G. H. (1951). A Recalibration of the Hydrometer for making Mechanical Analysis of Soils, Agronomy J. 43: 438. Bremner, J.M. & Mulvaney C.S. (1982). Nitrogen Total. In: Methods of Soil Analysis. Part 2: Chemical and Microbiological Propertie. A.L. Page, R.H. Miller & D.R. Keeney (Eds). Madison, Wisconsin: American Society of Agronomy, Gasparatos, D. & Haidouti, C. (2001). A comparison of wet oxidation methods for determination of total phosphorus in soils. Journal of Plant Nutrition and Soil Science, 164, Lindsay, W.L & Norvell, W.A. (1978). Development of a DTPA soil test for zinc, iron, manganese and copper. Soil Sci. Soc. Am. J., 42, Nelson D.W. and Sommers L.E. (1982). Total carbon, organic carbon and organic matter, In: Methods of Soil Analysis. Part 2: Chemical and Microbiological Propertie. A.L. Page, R.H. Miller & D.R. Keeney (Eds). Madison, Wisconsin: American Society of Agronomy, Mc Lean E.O. (1982). Soil ph and lime requirement, In: Methods of Soil Analysis. Part 2: Chemical and Microbiological Propertie. A.L. Page, R.H. Miller & D.R. Keeney (Eds). Madison, Wisconsin: American Society of Agronomy, Olsen S.R. and Sommers L.E. (1982). Phosphorus, In: Methods of Soil Analysis. Part 2: Chemical and Microbiological Propertie. A.L. Page, R.H. Miller & D.R. Keeney (Eds). Madison, Wisconsin: American Society of Agronomy, Thomas G.W. (1982). Exchangeable cations, In: Methods of Soil Analysis. Part 2: Chemical and Microbiological Propertie. A.L. Page, R.H. Miller & D.R. Keeney (Eds). Madison, Wisconsin: American Society of Agronomy,

SOIL SURVEY STANDARD TEST METHOD PARTICLE SIZE ANALYSIS

Department of Sustainable Natural Resources SOIL SURVEY STANDARD TEST METHOD PARTICLE SIZE ANALYSIS ABBREVIATED NAME PSA TEST NUMBER P7 TEST METHOD TYPE B VERSION NUMBER 3 RECORD OF AMENDMENTS Version