Highlights
Assignment Task:
Practical 3. Soil chemical properties
Introduction
In this practical, spread over three weeks, you will examine several soil samples, measuring some key chemical properties. You will use soil from various places that we have collected previously. However, you are welcome to bring your own soil samples and analyse them instead if you wish.
By the end of this practical you will be able to:
Measure the following characteristics of a soil sample:
o field texture (ie. perfect your technique)
o organic matter content
o pH
o electrical conductivity
o cation exchange capacity
Understand how these parameters may be related to each other and to other characteristics of the soil and environment.


B. pH and electrical conductivity (EC)
Background
Soil pH can tell you a lot about the chemistry of a soil. Soil pH is a measure of the concentration of the hydrogen ion (H + ). It is determined by the net effect of all the acidic and alkali materials in soil. Because it is the net effect of the many reactive materials in soil, pH gives a good indication of many soil properties, especially the availability of various nutrients and toxic materials to plants. Soil pH influences the availability of nutrients directly by influencing the solubility of materials in soil, and indirectly by influencing biological activity. You have measured pH in the field using the indicator method. Now you will measure pH in the lab using a 1:5 soil:water suspension and a pH electrode (Rayment and Lyons 2011).
Soil electrical conductivity (EC), is related primarily to the amount of salt in the soil. Salts originate from rainfall, irrigation water, the sea, groundwater, weathering of minerals and mineralization of organic matter. In wet climates they are easily lost by leaching, but in places where evaporation exceeds precipitation they can accumulate. High levels of salinity limit plant growth, mostly due to osmotic effects. There are many salts in soil and water, having different composition and solubility. Sodium chloride is the most common salt in most Australian landscapes, and is also the most soluble. As most salt solutions have a similar relationship between concentration EC, and as EC is closely related to osmotic potential, EC is a useful way of measuring salinity. That is straightforward in water, but in soil we need to add pure water (drastically dilute the soil) to obtain enough solution to measure the EC. When measuring EC of soil it is critical to record the ratio of soil: water used. Common ratios are 1:5 soil:water (by weight), or a ‘saturated paste’. We will use a 1:5 ratio (the same suspension we use to measure pH). As a general rule of thumb, soils are considered saline (saline enough to adversely affect plant growth) if EC 1:5 is & 0.3 dS/m. Materials
Method
1. Weigh 5.0 g (±0.2 g) of each soil into each specimen jar.
2. Add 25 mL of deionised water to each and shake by hand for a few minutes.
3. Calibrate pH meter and EC meter and dip into suspension to measure pH and EC.
4. Record results in Table 3. The EC meters are labeled ?S (micro siemens), but the actual values are
S/cm (see label on calibration solution). Other commonly used units are mS/cm or dS/m (which are equal to each other). Divide ?S/cm by 1000 to obtain mS/cm or dS/m, which is the unit you should use for recording your results.

C. Soil organic matter content
Soil organic matter has many important functions: it is the main source of N, P and S for plants (via mineralization by microorganisms), has high cation exchange capacity, provides energy and nutrients for microorganisms and fauna, is an important pool of elements in global cycles, buffers against changes in
pH, alters the mobility and reactivity of pollutants, and influences soil physical properties. You will use the ‘Loss on ignition’ method to measure soil organic matter content. In this method the soil is heated to 400ºC, which burns off the organic matter (converted to gases), but leaves the mineral component remaining. The application of this technique to Australian soils has been discussed by Spain et al. (1982). Materials
Method (First week)
1. Record the engraved number on your 2 aluminium dishes in Table 2, then weigh them and record their masses.
2. Place approximately 8 teaspoons in the dishes and place in oven set at 105ºC, with lid off, to remove the water.
Method (Second week)
3. Replace the lids on the dishes, allow them to cool, and weigh them.
4. Place the dishes in a muffle furnace set at 400ºC for 16 hours (with lid off).
Method (Third week)
5. Remove the dishes from the oven, replace the lids, allow them to cool, and weigh them.
6. Calculate organic matter content of the soil as a % of oven-dried soil mass. % organic matter = 100 x (B-C)/(B-A).

D. Cation exchange capacity (CEC)
Cation exchange capacity (CEC) is a measure of the negative charge of soil, which is the same as its ability to retain cations in ‘exchangeable’ form. Exchangeable cations are held electrostatically, are in equilibrium with ions in solution, and are available to plants but are not easily lost by leaching. Many of the elements that are essential for plants, including calcium, potassium and magnesium, behave as cations in soil, so CEC is important for soil fertility. In this practical you will measure the
Materials
Method
1. weigh 0.2 g (±0.01 g) soil into a 50-mL tube, add 20 mL of 5 mM MB solution using the 10-mL pipette
2. shake on end-over-end shaker for 15 minutes, then centrifuge at 3000 rpm for 5 minutes
3. Using a pipette, remove 0.2 mL of supernatant and place into a 20 mL test tube. Then add 9.8 mL deionized water (final volume of 10 mL).
4. Prepare samples for a ‘standard curve’ by pipetting 0.2 mL of each of the 6 primary standards into a 20 mL test tube and adding 9.8 mL deionized water to each (final volume of 10 mL).
5. Pour the prepared standard samples into spectrophotometer cuvettes, filling them to about 5 mm below the top. Take care never to touch the clear sides of the cuvettes. Before measuring absorbance, wide the clear sides with a tissue to ensure they’re spotless.
6. Using the spectrophotometer, measure and record (in Table 4) the absorbance of the diluted standards (at 550 nm). Draw a graph of absorbance against known MB
concentrations, on the next page or in Excel. On the graph, label the concentration axis using the primary standard concentrations, because the sample will be diluted by the same amount. Draw a line of best fit, which is called the ‘standard curve’ or ‘calibration curve’. The line of best fit may be drawn by eye and hand or using regression (‘trend line’) in Excel. The graph must have an explanatory caption
7. Using the spectrophotometer, measure and record the absorbance of the diluted supernatant and determine the concentration of the MB (mM MB) in the supernatant
solution by reading the value off the standard curve. Record results in Table 5.
8. Calculate CEC, using the formula CEC = [(5 – c)/10] * [extractant volume/mass soil], where CEC is in cmol(+)/kg, c is the concentration of MB in the supernatant solution (mM), extractant volume is 20 (mL), and mass of soil is 0.2 (g).

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6. Using the spectrophotometer, measure and record (in Table 4) the absorbance of the
diluted standards (at 550 nm). Draw a graph of absorbance against known MB
concentrations, on the next page or in Excel. On the graph, label the concentration axis
using the primary standard concentrations, because the sample will be diluted by the
same amount. Draw a line of best fit, which is called the ‘standard curve’ or ‘calibration
curve’. The line of best fit may be drawn by eye and hand or using regression (‘trend
line’) in Excel. The graph must have an explanatory caption
7. Using the spectrophotometer, measure and record the absorbance of the diluted
supernatant and determine the concentration of the MB (mM MB) in the supernatant
solution by reading the value off the standard curve. Record results in Table 5.
8. Calculate CEC, using the formula CEC = [(5 – c)/10] * [extractant volume/mass soil],
where CEC is in cmol(+)/kg, c is the concentration of MB in the supernatant solution
(mM), extractant volume is 20 (mL), and mass of soil is 0.2 (g).
Table 4. Data for standard curve.
MB conc. (mM) 0 1 2 3 4 5
Absorbance at 550 nm
Table 5. Cation exchange capacity results
Soil:
Absorbance at 550 nm
MB conc. (mM)
CEC (cmol(+)/kg)
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E. Acid sulfate soils
Acid sulfate soils are very important in coastal areas and also in waterlogged saline areas inland. They need to be identified and managed carefully (Dear et al. 2014). We will demonstrate the field test for acid sulfate soils, in which the pH of a soil sample is measured before (pH F ) and after oxidation using hydrogen peroxide (pH FOX ), according to the method of Ahern et al. (2004). The hydrogen peroxide oxidation is a rapid simulation of the oxidation that occurs when potential acid sulfate soils (PASS) are exposed to air and become actual acid sulfate soils (AASS). PASS may have neutral pH, whereas AASS have pH<4. Laboratory analysis is required
for confirmation and for estimation of the amount of potential acidity and internal neutralizing capacity (calcium carbonate).
PASS contains iron sulfides and high concentrations of potentially toxic elements in sulphide form (e.g. Fe, Al, As, Co, Cu, Ni, and Pb). Oxidation of the PASS releases sulphuric acid and high concentrations of the potentially toxic elements, which are soluble in acid conditions. Environmental impacts of oxidised ASS occur in the disturbed soils and downstream. In addition to toxic concentrations of metals and metalloids, when the water’s pH is raised (eg. due to mixing with seawater), oxidation of the Fe 2+ to Fe 3+ consumes all the oxygen in the water, leading to asphyxiation of animals.
This activity is not included in your report. Materials (for lecturer/tutor)
Method (for lecturer/tutor)
Put 6-10 g soil in each of 4 tubes. Add water to two of them and H 2 O 2 to the other two. Be careful, as fumes, heat and bubbles may be generated. Allow to react and then measure pH of all.
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