MIL-DTL-11309J
4.5.1.2.2 Reagents - hyamine 1662.
a. Hyamine 1622 crystals (benzethonium chloride).
b. Sodium hydroxide, 50 percent solution, reagent grade.
c. Sodium lauryl sulfate (dodecyl sulfate, sodium salt) crystals.
4.5.1.2.3 Reagents - methylene blue indicator.
a. Methylene blue chloride (652).
b. Sulfuric acid, concentrated, reagent grade.
c. Sodium sulfate, anhydrous, reagent grade.
4.5.1.2.4 Preparation of hyamine 0.018 N. Fill a one-liter volumetric flask half full with
distilled water. Then carefully add 3.20 grams of 50 percent sodium hydroxide and mix. Then
add 7.36 grams of hyamine crystals and fill to volume with distilled water. Stir until dissolved.
Do not dry the hyamine. The weight should be adjusted, if necessary, to provide a solution close
to 0.018 N.
4.5.1.2.5 Standardization of hyamine. Sodium lauryl sulfate (SLS) active solution; (by
weight), 0.003 N: weigh approximately 0.873 grams of SLS to the nearest 0.1 mg (use standard
as received, do not dry). Transfer to a one-liter volumetric flask, dissolve in distilled water,
dilute to volume, and mix. Calculate the normality of SLS solution to six decimal places. When
not being used, store the SLS in a tightly stoppered container. Label with normality, date and
technician's initials. Discard after one year. To standardize hyamine, pipette a 20-mL aliquot
from the 0.003 N standard active SLS solution and add it to a 250-mL stoppered graduated
cylinder already containing:
25 mL methylene blue indicator
25 mL chloroform
30 mL distilled water
Titrate with the 0.002 N hyamine solution using a 50-mL burette containing as large a volume as
possible without risk of over-titrating. Stopper the graduated cylinder and shake vigorously at
least 30 times. To speed up the separation, hold the graduated cylinder in a horizontal position
until most of the chloroform has separated, then return the graduated cylinder to the vertical
position and swirl gently. After the mixture has separated, note color difference between the two
layers. Using the degree of color difference as a guide, continue adding hyamine in successively
smaller increments, shaking the graduated cylinder 20 times after each addition. When colors of
the two layers are close, add the hyamine in 0.5-mL amounts until the end point at which both
layers will be an aqua blue color. The end point is when the colors of the two match when the
graduated cylinder is observed at eye level against a white background. The comparison should
be made as soon as the layers separate completely.
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