RESULTS AND DISCUSSION

In this exercise, soil organic matter analysis was performed utilizing what is known as Walkley-
Black procedure. Prior to this exercise, the necessary soil samples, Macolod Clay and Cavinti Soil, were
subjected to sieving (0.5mm non-ferrous sieve) to obtain the fine portion of the said samples which is
necessary so that the sample mixes readily with the potassium dichromate used in the experiment.
Furthermore, in a reduction-oxidation titrimetric procedure such as Walkley-Black method, precautionary
measures were taken regarding the reagents used. It is necessary that the ferrous sulfate to be used is
freshly prepared or prepared not more than 2 weeks prior (no formation of oxidized crystals) as iron to
be used in this exercise should be in its reduced state. Also, Fe2+, MnO2 and Cl- if abundant in the sample
can interfere with the analysis (Hesse, 1972).

The experiment started with the oxidation of the organic matter. To do this, fine soil samples
placed in a 500mL conical flask (reaction vessel is the same for all samples to obtain uniform heats of
dilution for the same period of time) was added with 1:2 proportion of 1N potassium dichromate and
concentrated sulfuric acid. The reaction produces a dichromate ion which oxidizes the oxidizable matter
and at the same time generates heat necessary to facilitate the reaction (see overall reaction below).

(INSERT EQUATION 3-1 HERE)

Given the nature of the reaction involved in this analysis, several assumptions were made. Organic carbon
in soils has an average oxidation state of zero and an equivalent weight of 3g/equivalent when reacted
with the dichromate ion, such that;

(INSERT EQUATION 3-2 HERE)

Another assumption is that the heat of the reaction oxidizes only 75% of organic carbon in the soil hence,
a correction factor f=100/75=1.33 is to be used during calculation (Walkley and Black, 1934).

After oxidation of the organic matter, the excess dichromate ion is determined by titration with
standard ferrous sulfate using diphenylamine in concentrated sulfuric acid as indicator. The endpoint is a
blue green color which is sharpened by the addition of phosphoric acid.

(INSERT EQUATION 3-3 HERE)

Though not performed there are other methods of determining the excess dichromate. One of which is
colorimetric methods to be specific Graham colorimetric method which makes use of the reduced
chromium 3+ as the direct measure of carbon oxidized. Another method is potentiometric method which
makes use of an autotitrator relying on the principle of the reduction-oxidation nature of the analysis. In
this method, during endpoint, a voltage shift of around 300 to 400mV is obtained for about 0.01 to 0.02mL
of the ferrous sulfate titrant (Hesse, 1972).

After oxidation and titration, the collected data were used to calculate for the organic carbon
content of the samples. First off, the meq potassium dichromate was computed for all the samples and
since it was the same all throughout meq potassium dichromate has a value of 10 for all the samples.
Then, the concentration of the ferrous sulfate titrant is first calculated given meq potassium dichromate