MIL-DTL-382E
manufacturer recommendations. Alternately, stock solutions may be prepared in-house from high
purity metals or their salts. The maximum recommended shelf life is one year from date of
initial preparation.
a.
Certified Fe stock solution shall contain 100.00 µ g/mL Fe in 5.00 % 1:1 HNO3 (v/v).
b.
Certified Mg stock solution shall contain 20,000.00 µ g/mL Mg in 0.10 % 1:1 HNO3 (v/v)
Nitric Acid (HNO3), concentrated, 67 70 %.
c.
d.
Distilled water.
4.5.3.4.2 Procedure.
4.5.3.4.2.1 Sample Dissolution.
a. Weigh one gram of sample, as "M", to the nearest 1 milligram and transfer into 400
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.
d. Cover with watch glass and heat on hot plate at approximately 180oC to completely
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.
4.5.3.4.2.2 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 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.
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