MIL-DTL-11414F
4.5.7 Chromium (hexavalent) content. Determine the presence or absence of hexavalent
chromium by either of the following chemical reagent screening techniques. Nonconformance to
the 3.4.2 requirements shall constitute failure of this test.
a. Weigh approximately 250 mg of pigment into a small glass test tube. Add 5 ml of 25
percent aqueous KOH and shake vigorously for 1-2 minutes. Decant a one ml aliquot
into a plastic micro-centrifuge tube and centrifuge for five (5) minutes at 17,000 rpm,
balancing the centrifuge with a tube containing one ml of the KOH solution. The
resulting supernatant liquid shall be nearly colorless. Use the tube containing the KOH
solution as a reference. A distinct yellow color indicates the presence of hexavalent
chromium and therefore shall constitute failure of the test requirement.
b. Weigh approximately 50 mg of pigment into a small glass test tube. Add 5ml of 10
percent aqueous H2SO4 and shake vigorously for 1-2 minutes. Decant a one ml aliquot
into a plastic micro-centrifuge tube and centrifuge for five (5) minutes at 17,000 rpm,
balancing the centrifuge with a second tube containing one ml of the H2SO4 solution.
The solution in the second tube shall act as the test "blank". Immerse a chromate ion
(CrO42-) test strip into the supernatant from each tube. Shake off the excess liquid and
after approximately one minute compare the color change in the reaction zone of the
strips to the color scale (concentration levels) provided by the manufacturer. The
appearance of a purple/violet color from the "sample" strip is indicative of hexavalent
chrome and therefore shall constitute failure of the test requirement. If a color change
is apparent from the "blank" strip rerun the test using fresh, chromium-free reagents.
The appearance of a pronounced color change is indicative of hexavalent chrome and
therefore shall constitute failure of the test requirement.
4.5.8 Lead content. Determine the presence or absence of lead by weighing 50 mg of pigment
into a small glass test tube. Add 5 ml of dilute HNO3 and shake vigorously for 1-2 minutes.
Decant a one ml aliquot into a plastic micro centrifuge tube and centrifuge for five (5) minutes at
17,000 rpm, balancing the centrifuge with a second tube containing one ml of the dilute HNO3
solution. The solution in the second tube shall act as the test "blank". Immerse a lead ion test
strip into the supernatant from each tube. Shake off the excess liquid and after approximately one
minute compare the color change in the reaction zone of the strips to the color scale
(concentration levels) provided by the manufacturer. If a color change is apparent from the
"blank" strip rerun the test using fresh, lead-free reagents. Confirmation of the exact lead
concentration in the coating's solids shall be quantified using ASTM D3335. Nonconformance to
the 3.4.2 requirements shall constitute failure of this test.
4.5.9 Solvent analysis.
4.5.9.1 Solvent analysis for VOC content determination. Determine the VOC content in
accordance with ASTM D3960. Check for compliance with table II.
4.5.9.2 VOHAP content. Hazardous solvent content of the reduced enamel shall be determined
in accordance with ASTM D3271 or EPA Method 311, as applicable. Check for compliance with
table II.
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