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Introduction to Soil Chemistry

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kjeldahl—organic nitrogen 121<br />

Nitrogen in soil organic matter is mostly in the form of proteins and amino<br />

acids. Although the specific analysis for these important and interesting<br />

compounds can and is done, it is more often the case that the <strong>to</strong>tal inorganic<br />

and organic nitrogen in soil is determined. This is because inorganic nitrogen<br />

compounds are used by plants and are of environmental concern. Decomposition<br />

of organic nitrogen containing compounds results in the release of<br />

ammonia in<strong>to</strong> the soil solution, where it immediately reacts <strong>to</strong> form ammonium.<br />

Once in this form, it is readily oxidized by soil bacteria <strong>to</strong> nitrite and<br />

finally in<strong>to</strong> nitrate. Because of the ready conversion of organic nitrogen in<strong>to</strong><br />

inorganic forms and the ready interconversion of inorganic nitrogen in soil, its<br />

<strong>to</strong>tal concentration, both inorganic and organic, is important. Kjeldahl is the<br />

basic and most commonly used method for determination of <strong>to</strong>tal nitrogen in<br />

soil.<br />

In a <strong>to</strong>tal soil nitrogen analysis a soil sample is first digested in a kjeldahl<br />

flask <strong>to</strong> convert all organic nitrogen in<strong>to</strong> inorganic ammonium. Two kjeldahl<br />

flasks are shown on the left-hand side in Figure 6.7; the flask with the bulb at<br />

the bot<strong>to</strong>m is an older-type kjeldahl flask, while the large test tube is a newerdesign<br />

digestion tube. Digestion is accomplished using concentrated sulfuric<br />

acid and a catalyst. A salt such as potassium sulfate is added <strong>to</strong> increase the<br />

boiling point of sulfuric acid such that decomposition of organic matter occurs<br />

more readily. This mixture plus soil is heated until all organic matter has<br />

been destroyed. In Figure 6.6 a heating block for heating the kjeldahl flask is<br />

shown next <strong>to</strong> the distillation unit. After digestion the solution is cooled and<br />

a concentrated basic solution, usually 50% NaOH, is added and the released<br />

ammonia steam-distilled in<strong>to</strong> a receiving flask containing a standard acid<br />

that reacts with the ammonia. On completion of the steam distillation, the<br />

unreacted acid is titrated and the amount of ammonia distilled is calculated<br />

by difference.<br />

The kjeldahl procedure has been used for many years <strong>to</strong> determine the<br />

nitrogen in human tissues and in both animal and human foodstuffs. For these<br />

materials, the procedure works well and is straightforward. For soil, such is not<br />

the case. All soils naturally contain some ammonium, and when the steam<br />

distillation is carried, out this distills along with the ammonium produced by<br />

the decomposition of organic matter. This then gives a measurement of the<br />

<strong>to</strong>tal ammonium in soil after digestion. It cannot distinguish between ammonium<br />

derived from organic matter and from the soil itself.<br />

If a soil kjeldahl organic nitrogen determination as described above has<br />

been carried out, then this can be used along with simple ammonia steam<br />

distillation, <strong>to</strong> measure the amount of nitrogen from each source, that is, inorganic<br />

ammonium and organic matter. However, this still does not provide a<br />

measurement of the <strong>to</strong>tal nitrogen in soil because it does not account for that<br />

present as either nitrite or nitrate. See Figure 6.7 for a flow diagram for determining<br />

all nitrogen in soil using a kjeldahl apparatus.

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