MIL-DTL-46162E
APPENDIX A
A.5. REAGENTS
A.5.1 Saponification mixture (1N). Prepare by mixing 6.5 grams (g) (0.23 oz) of potassium
hydroxide (KOH), (ACS reagent grade) with 100 mL (3.34 oz) of absolute 1-butanol
(ACS reagent grade) and heat to dissolve the KOH. After the solution cools, filter the mixture
through the glass-fiber filter paper.
A.5.2 Diphenylamine (l percent solution). Prepare by dissolving 0.250 g (8.8 oz) of
diphenylamine (ACS indicator grade in 25 mL of sulfuric acid (specific gravity (gr) 1.834)).
A.5.3 Toluene (ACS reagent grade).
WARNING
Toluene is flammable and toxic. Avoid
breathing vapors or contact with skin.
A.6 PROCEDURE
A.6.1 Pipette 10 mL of the sample into the reaction bottle and add 5 mL (0.2 oz) of toluene
followed by 10 mL of the saponification mixture.
WARNING
Oral pipetting techniques should not be used because of the toxicity
of the substance involved. A pipetting bulb or assembly similar to
one of those described in A.3.3 should be used.
A.6.2 Affix cap to the reaction bottle tightly and, after mixing the contents, place it in an
oven maintained at 110°C (230°F) for four hours.
A.6.3 Remove the reaction bottle from the oven and allow it to cool to 25 ± 3°C
(77 ± 5.4°F).
A.6.4 Filter the contents of the reaction bottle through the 60 mL glass-fitted crucible fitted
with the glass filter disc.
A.6.5 Wash the reaction bottle with 25 mL of toluene and transfer it to the glass-fitted
crucible.
A.6.6 Carefully remove the glass fiber filter disc and dry it in oven at 110°C (230°F) for
15 minutes.
A.6.7 Remove the filter disc and cool it to 25 ± 3°C.
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