MIL-DTL-14067C
4.5.11.2 Procedure.
a.
An accurately weighed sample of 0.7700 plus or minus 0.0300 grams of Type III alloy
shall be transferred to a 250 milliliter beaker.
b.
Ten milliliters of distilled water shall be added to the sample beaker.
c.
The beaker shall be covered with a watch glass and 20 milliliters of concentrated HCl
shall be added dropwise through the opening at the lip of the beaker.
d.
After the reaction in the beaker has subsided, the solution shall be heated to boiling to
assure complete solution.
e.
The watch glass shall be washed thoroughly with distilled water and the washings
drained back into the beaker.
f.
The solution shall be filtered through a No. 41 Whatman, or equivalent, filter paper with
the filtrate caught in an accurately calibrated, 1 liter volumetric flask.
g.
The filter paper shall be washed thoroughly with hot distilled water and the solution made
up to the 1 liter volume with the distilled water.
h.
A 100 milliliter aliquot shall be transferred to a 250 milliliter beaker using an accurately
calibrated buret or pipet.
i.
Three drops of bromphenol blue indicator shall be added to the solution neutralized by
adding dropwise and with constant stirring, a filtered 1:1 NH4OH solution until the
yellow color turns to blue.
j.
Two drops of NH4OH shall then be added to the excess solution.
k.
The solution shall be heated to boiling and 18 milliliters of the 8-hydroxyquinoline
solution added in small portions, stirring after each addition to dissolve the precipitate
that forms. Any precipitate remaining after the completion of the addition of the reagent
shall be disregarded.
l.
The solution shall be heated to boiling and 40 milliliters of 2 molar (M) ammonium
acetate solution (154 grams per liter) added dropwise with vigorous stirring and then
placed in a steam bath for 30 minutes.
m.
The solution shall be filtered with a suction through a tared, fine porosity, fritted glass
bottomed crucible.
n.
The precipitate shall be washed eight times with 15 milliliter portion of distilled water,
releasing the suction before each addition and allowing the precipitate to remain in
contact with the wash water for at least one minute prior to the application of suction.
The precipitate shall be dried for 3 hours in an oven at 120o to 140oC, cooled in a
o.
desiccator and weighed as aluminum hydroxyquinoline, Al(C9H6ON)3.
The percent aluminum shall be calculated as follows:
Percent aluminum =
Where:
A = grams of precipitate.
B = percent iron.
W = grams of sample contained in the aliquot.
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