MIL-DTL-450D
4.4.19 Solvent analysis for Composition L coating compound.
4.4.19.1 Separation of volatile portion.
4.4.19.1.1 Equipment.
a. Large test tube (22 mm by 175 mm)
b. Antibumping stones or Berl saddles
c. 2-hole rubber stopper
d. Glass delivery tube (5-mm diameter) with stopcock
e. Test tube (20 mm by 150 mm) with sidearm
f. Dry ice-acetone bath
g. Silicone oil bath
h. Vacuum pump
4.4.19.1.2 Reagents.
a. Tricresyl phosphate
4.4.19.1.3 Method.
a. Pour approximately 15 g of coating material into a large test tube (22 mm by 175 mm).
b. Add 10 mL of tricresyl phosphate and several antibumping stones or Berl saddles.
c. Fit a 2-hole rubber stopper into the mouth of the test tube to accommodate a stopcock and
a glass delivery tube (5-mm diameter) which is attached to another test tube (20 mm by 150 mm)
to serve as receiver. The latter test tube should have a sidearm for attaching a vacuum pump.
The glass delivery tube should reach 1 inch from the bottom of the receiver tube.
d. Immerse the receiver in a dry ice-acetone bath.
e. Preheat a silicone oil bath to 160 ºC. Raise the oil bath until the oil reaches the sample
level.
f. Reduce the pressure slowly to 10 mm of mercury. After all the solvent has distilled,
carefully release the vacuum using the stopcock that is connected to the sample tube.
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