The distribution of
fillers, pigments and other materials on the surface of modern
papers is of major importance in regards to their ultimate performance.
Determining the distributions of these materials however is not
possible with standard bulk chemical techniques. One technique
which is well suited to this task is digital mapping by WDS (Wavelength
Dispersive Spectroscopy) x-ray spectroscopy. By scanning an electron
beam at discrete intervals across a sample and recording the intensity
of the resultant x-rays, a detailed digital map of element distribution
in two dimensions can be constructed. This technique allows rapid
simultaneous determination of multiple element distributions with
a minimal processing required in most cases. Distributions may
be determined with both EDS and WDS, but the greater resolving
power and lower detection limits of WDS makes it the essential
for determining the distribution of starch1, one of
the major constituents on paper surfaces.
This procedure was
used to determine the distribution of starch , silicon and calcium
in several papers. The papers were prepared by carbon coating
and were attached to glass slides using carbon tape. Inorganic
constituents such as SiO2 and CaCO3 generally
produce sufficient x-rays (Ca K1 and Si K1) to be determined directly,
with the finished map ready for image processing. Starch (composed
mainly of carbon, hydrogen and oxygen), however does not produce
sufficient X-rays to allow direct measurement. To allow visualization
of starch it must be first complexed with iodine, which produces
enough x-rays to allow mapping2. A complication in
starch determination is the presence of a calcium peak (Ca K1,3
) near the iodine peak (I L1) which necessitates the removal
of the calcium produced background. The simplest method of removing
this background is to detune the spectrometer to a position above
and below the iodine peak and linearly interpolate the background
at the position of the Iodine peak. This procedure triples the
amount of time required for map acquisition, but in some cases
it may be possible to collect background signals at the same
time as peak signals3,4.
Once the element distribution
images are acquired, they may be analyzed with image processing
software. Examples of the determination of overall coverage are
given.