MIL-DTL-14067C
should be less than 10 kiloPascal and should not increase faster than 2 kPa/min. Check
connections and eliminate leaks.
Addition funnel with stopcock, >50 mL, 24/40 ground glass joint,
1.
Round-bottom-3-neck flask, 500 mL, 24/40 ground-glass ports,
2.
24/40 ground-glass barbed adapter,
3.
24/40 ground-glass barbed adapter,
4.
Rubber stopper/septum,
5.
Tubing, thick-wall rubber, 1/4 inch ID,
6.
Valve, 3-way, glass stopcock,
7.
Tubing, thick-wall rubber, 1/4 inch ID,
8.
Union, barbed, reducing 1/4 in to 1/8 inch,
9.
Tubing, thick-wall rubber, 1/8 inch ID,
10.
Manometer, digital, 0 to ≥ 30 psi.
11.
FIGURE 1. Reaction apparatus set-up & connections.
4.5.4.1.6 Blank.
a. Add 50.0 milliliters of 5 % wt sulfuric acid reagent to the addition funnel.
b. Evacuate reaction vessel, then turn 3-way valve to exclusively connect the flask and
manometer.
c. Open addition funnel to allow acid to dispense; keep stopcock open long enough for air
to enter flask and internal pressure to reach atmospheric.
d. Wait 5 minutes for the flask to warm to room temperature and open and close the
stopcock to equilibrate pressure.
e. Puncture the rubber septum with the 0.1 milliliter syringe.
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