MIL-DTL-14067C
4.5.5.2.1 Sample Dissolution.
Weigh one gram of sample, as "M", to the nearest 1 milligram and transfer into 400
a.
milliliter beaker.
b.
Add 10 milliliters of distilled water to the beaker followed by 2 milliliters of 1:1 HNO3.
(Slowly add acid and allow reaction to subside.)
c.
Gradually add 16 milliliters of 1:1 HNO3 to the sample solution, approximately 1
milliliter at a time. Reaction may become overly vigorous by adding reagent too quickly.
Cover with watch glass and heat on hot plate at approximately 180oC to completely
d.
decompose sample.
e.
Allow sample to cool to ambient temperature and transfer into 100 milliliter volumetric
flask.
f.
Rinse lower surface of watch glass and inner walls of beaker with distilled water into
flask.
g.
Dilute the sample solution with distilled water to 100 milliliters.
4.5.5.2.2 Preparation of calibration curve.
a. Dispense 50 milliliters of Mg stock solution into each of two 100 milliliter volumetric
flasks.
b. Add stepwise 20.0 milliliters, and 30.0 milliliters of Fe stock solution separately to the
two volumetric flasks and dilute with distilled water to 100 milliliters. These solutions
will represent the mid and high standards respectively.
c. Prepare blank by pipetting 50 milliliters of Mg stock solution into a third 100 milliliter
volumetric flask and dilute with distilled water to the 100 milliliter mark.
Mid standard shall contain: 20 µ g/mL Fe and 10,000 µ g/mL Mg.
High standard shall contain: 30 µ g/mL Fe and 10,000 µ g/mL Mg.
Blank shall contain 10,000 µ g/mL Mg.
d. Aspirate standard solutions into ICP spectrometer in order of increasing concentration.
Take emission measurements for iron and generate a calibration curve utilizing the
instrument s software. Fe emission intensity shall be measured using radial view at the
259.940 nm wavelength. The calibration shall be forced through the origin. Repeat the
calibration if the correlation determination (R2) for Fe is < 0.9999.
4.5.5.2.3 Sample Analysis.
a. Aspirate sample solution into ICP spectrometer and record Fe emission measurement.
Software generated concentrations for Fe shall be inserted into the formula below as A1.
b. Aspirate blank solution containing 10,000 µ g/mL Mg and insert into formula below as
A2.
4.5.5.2.4 Sample Calculation.
Where:
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