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Figure5.9. (a) Freezing microtome: (1) tissue sample; (2) stretcher with a thin section; (3) scalpel.
(b) A thin section of mussel tissue is placed on a quartz-glass carrier. Figure from Ref. [98],
reproduced with permission. Copyright1989, Elsevier.
absolutely recommended for cooling down to room temperature and condi-
tioning of the section.
Finally, the individual sections are analyzed by TXRF within a counting time
of 100-1000 s. Afterward, the dry mass of the section has to be determined. For
this purpose, a difference weighing is carried out by means of a microbalance
with a precision of 0.1 μ g. Every carrier is weighed twice, first with the deposited
section and then without the section, after it was scraped off with a scalpel. The
carriers must not be touched by hand, and gloves must be used in order to
precisely determine dry masses of only 100 μ g or so. The mass fractions are
finally determined by Equation 4.12.
The reliability of the method was checked by the analysis of different
reference materials [98]: NIST 1573“Tomato Leaves”; NIST 1566“Oyster
Tissue”; NIST 1577“Bovine Liver”; and NIES 2 No. 6“Mussel Tissue”.
Because these materials are only available as powders, 100 mg was first mixed
with several μ l of ultrapure water and then this powder mash was freeze-cut and
analyzed by TXRF. The detection limits were found to be about 1 μ g/g. The
relative deviations between certified and measured values were about 10% for
elements with a mass fraction > 10 μ g/g. A possible Fe contamination by the
iron scalpel was precluded by control tests.
The freeze-cut technique can be applied to the analysis of human tissues, for
example, of kidney, liver, and lung. Within a project on occupational hazards,
Wiecken and colleagues studied the dust stress caused by the inhalation of
heavy-metal particles [96]. A first group of 12 persons with exposure to normal
dust stress was examined. The spectra obtained from their lung tissue differed
2 NIES stands for the National Institute for Environmental Studies (Tsukuba, Japan).
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