Introduction to Soil Chemistry
Introduction to Soil Chemistry
Introduction to Soil Chemistry
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160 spectroscopy<br />
<strong>to</strong> scratch them. When using cuvettes that have not been used before, they<br />
should be tested <strong>to</strong> make sure that they are all the same. This is accomplished<br />
by inserting them in<strong>to</strong> the spectropho<strong>to</strong>meter and noting their absorbence.All<br />
should be the same. Keep in mind that empty cuvettes will have a higher<br />
absorbence than when filled with water. This is because light is refracted at<br />
each surface and when filled with water there is less refraction at the surfaces.<br />
8.8.1. Zeroing and Blanks<br />
When using a spectropho<strong>to</strong>meter for a colorimetric analysis, both the 0 (•A)<br />
and 100% (0A) readings must be set. Once the instrument has warmed up,<br />
with nothing in the sample compartment, the readout is set <strong>to</strong> 0. A blank, a<br />
solution containing all the components used in the analysis except the analyte<br />
being measured, is placed in a cuvette and placed in the sample compartment,<br />
and the instrument is adjusted <strong>to</strong> 100%. This procedure is intended <strong>to</strong> account<br />
for all interferences that may be introduced in<strong>to</strong> the measurement by components<br />
other than the analyte of interest. Once the instrument is adjusted,<br />
determination of the absorbence of standards and samples can be made.<br />
8.8.2. Relating Component Concentration <strong>to</strong> the Original Sample<br />
Performing an analysis requires the preparation of a standard or calibration<br />
curve. A series of standard solutions, a minimum of three, containing known<br />
amounts of the component of interest are prepared. There are two primary<br />
restrictions on these solutions: (1) they should be over the range of the<br />
expected concentrations of the component of interest and (2) all results for<br />
the extracted component must be higher than the lowest standard solution and<br />
lower than the highest standard. If a result is beyond these limits, its concentration<br />
cannot be determined. In the table of data for Figure 8.9, Unk1<br />
(unknown 1) is 0.05, which is below the lowest standard, specifically, 0.15, and<br />
so its value cannot be determined. Likewise, the Unk2 value is 0.97, which is<br />
above the highest standard and also cannot be determined.<br />
If, as with Unk 2, the value is above the highest standard, then the sample<br />
may be diluted and retested. In this case the concentration must be corrected<br />
for the amount of dilution. Similarly, in some cases when the concentration of<br />
an unknown is lower than the lowest standard, the solution can be concentrated<br />
and reanalyzed.<br />
Furthermore, standards must be over a range where there is a direct or<br />
straight-line relationship between the amount of color produced and the<br />
amount of component present. It is common for data points beyond the standard<br />
curve <strong>to</strong> be part of a different straight line or simply not measurable<br />
because the solution is <strong>to</strong>o light or <strong>to</strong>o dark. In Figure 8.9 the distance between<br />
points 0,0 and 10,0.15 may form a line very different from the one shown in<br />
the graph. We know nothing about this region. The same can be said about the<br />
region above points 90,0.95. With many instruments very low absorbances are