M. Haldimann et B. Zimmerli, EVALUATION OF ASHING PROCEDURES FOR THE GAS-CHROMATOGRAPHIC DETERMINATION OF FLUORIDE IN BIOLOGICAL-MATERIAL, Analytica chimica acta, 282(3), 1993, pp. 589-601
Fluoride in acidic aqueous solution was extracted with chlorodimethylp
henylsilane in cyclohexane and converted to fluorodimethylphenylsilane
, which was quantified by gas-liquid chromatography (GC) with flame io
nization detection. The potential of GC, combined with different ashin
g procedures, including high pressure closed vessel acid digestion, to
determine trace amounts of fluoride was evaluated with different biol
ogical standard reference materials. Major constituent elements such a
s Ca, Mg, Al and Si were also measured, but no correlation was apparen
t as to their effect on fluoride yields. Cluster analysis of fluoride
yields with the various ashing methods revealed a difference between p
lant- and non-plant materials. Using alkaline fusion (KOH) for plant m
aterials and a retaining agent (CaO) for non-plant materials good agre
ement with either certified or published values was obtained. The comb
ination of both ashing aids gave satisfactory results regardless of th
e sample type. Application of this ashing method to Swiss total diet s
amples from the year 1983 and comparison with an ion-selective procedu
re in another laboratory yielded consistent results and identical mean
values of 1.9 mu g F g(-1) (dry matter), corresponding to a daily die
tary intake of 0.9 mg F per adult.