MIL-DTL-38741A
a. Load the specimen as illustrated in figure 1 by flashing liquid into a suitable apparatus or
bag. The vaporized sample may have a very slight positive pressure with respect to atmosphere,
but should not exceed 10 psig. To assure the analytical integrity of the result, the entire aliquot of
bromochlorodifluoromethane must be vaporized.
b. Using a vacuum manifold, evacuate the sample loop and interconnecting tubing to the
sample apparatus valve. Close the valve to the vacuum pump and load the sample loop with the
specimen bromochlorodifluoromethane.
c. Analyze the specimen bromochlorodifluoromethane. The most frequently encountered
impurities in bromochlorodifluoromethane are listed in table III and will be available in the
calibration standard. Use component spiking and/or GC/MS to identify and quantify any
unknown peaks which appear in the analysis.
d. The weight percentage of bromochlorodifluoromethane is calculated as follows:
100 × AB × RRFB
WB =
∑ 1 to i ( Ai × RRFi )
Where WB
=
Weight percentage of bromochlorodifluoromethane.
=
Peak area of bromochlorodifluoromethane.
AB
=
Relative response factor for bromochlorodifluoromethane.
RRFB
Σ1 to i
=
Sum of all component peak areas times their respective response factors.
4.4.2 Acid halides. A large sample of the specimen bromochlorodifluoromethane shall be
evaporated in the presence of a small amount of crushed ice-distilled water slurry. The solution is
titrated for acid halides with standardized sodium hydroxides.
4.4.2.1 Reagents.
a. Sodium hydroxide, 0.01N solution: Dissolve 0.40 grams of carbonate-free sodium
hydroxide in recently boiled distilled water in a 1,000 mL volumetric flask. Cool and dilute to the
mark. This solution shall be standardized against reagent grade potassium acid phthalate.
b. Methyl red indicator, 0.1% solution.
CAUTION - Perform this procedure in a hood.
4.4.2.2 Procedure. Place 10 mL of a crushed ice-distilled water slurry in a 250 mL glass
stoppered Erlenmeyer flask and add 50 grams of bromochlorodifluoromethane to the slurry.
Place the stopper in the flask loosely and swirl the flask gently from time to time until the ice is
completely melted. Add one drop of methyl red indicator and if a reddish color remains, titrate to
a yellow endpoint with 0.01N sodium hydroxide solution. The ppm acid halides, as HBr, shall be
calculated as follows:
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