MIL-PRF-23236D
4.5.4.6.2 Materials and reagents. The following materials and reagents shall be required:
a.
Dry ice and acetone for cooling
b.
Drierite or equal
c.
Ammonia
d.
Sodium
e.
Alcohol
f.
Sodium hydroxide pellets
g.
Ammonium persulfate
h.
Sodium arsenite, 10 percent
Nitric acid (HNO3) approximately 20 percent
i.
Silver nitrate (AgNO3), 0.05N
j.
4.5.4.6.3 Procedure for the analysis of gasolines. The procedure for the analysis of decomposition of bromides
shall be as follows:
a. Cool the flask with a dry-ice, acetone slurry and introduce 15 grams of ammonia (see note 2). Replace the
rubber stopper carrying the delivery tube by the one fitted only with a protected vent. Add a cube of freshly cut
sodium, having an edge dimension of 5 millimeters (0.25 inch). Rotate the stirrer slowly by hand to partially
dissolve the metal. Add exactly 50 milliliters of the gasoline under test (see notes 3 and 4), remove the cooling bath,
and start the stirrer. As soon as the ammonia starts to evolve, disconnect the drying tube from the vent (see note 5).
Continue the stirring until the ammonia has evaporated (about 20 minutes for a 15-gram charge). If the
characteristic blue color of sodium in liquid ammonia should disappear during the earlier stages of the evaporation,
add another piece of sodium.
b. Upon evaporation of the ammonia, add 5 milliliters of alcohol to the mixture to decompose the excess
sodium. Next, add 30 milliliters of water and stir to aid in the extraction of inorganic salts. Remove the reaction
flask from the stirrer, wash down the stirrer with water, and transfer the contents to a separatory funnel. Separate the
aqueous layer and extract the organic layer with two additional 30-milliliter portions of water. Combine the three
aqueous extracts, evaporate to 50 milliliters, and cool slightly. If, at this point, the mixture is not clear and contains
a precipitate, filter and wash the paper several times with small portions of hot water. Evaporate the combined
filtrate and washings to 50 milliliters and cool slightly. Add 2 grams of sodium hydroxide pellets, followed by 2
grams of ammonium persulfate. After the solids have dissolved, boil the solution for 15 minutes (see notes 6 and 7).
Cool the solution slightly, add 10 milliliters of a 10 percent solution of sodium arsenite, boil for 10 minutes, and cool
to room temperature. Make the solution acid to phenolphthalein by adding HNO3 (20 percent) and determine the
bromides as given below (see note 8).
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