MIL-DTL-23938B(AS)
b. Add approximately 5 gm of the undried sample to each. Stopper and weigh to the nearest
0.1 mg. Record weights as B.
c. Tilt stopper and place in oven at 220 °F for at least 3 hours.
d. Remove the bottles from the oven. Stopper and place in a CaCl2 desiccator for 30 ±5
minutes.
e. Weigh to the nearest 0.1 mg and record as C.
f. Calculate as follows:
B-C
Percent volatiles
=
x 100
B-A
Note: Use tongs or cotton gloves to handle glassware. Make all weighings rapidly.
4.5.3 Total acid insolubles determination. The total acid insolubles shall be determined as
follows:
a. Weigh a 5 gram sample to the nearest 0.1 mg in a 250 mL beaker.
b. Add about 50 mL of distilled water and 50 mL of concentrated hydrochloric acid.
c. Heat until the material is dissolved. Filter through a Munktell No. 00H filter paper or
equivalent, and wash 5 times with dilute HCl.
d. Transfer the filter paper to the original beaker and add 25 mL of water and 10 mL of HCl;
with the aid of a glass rod, tear the filter paper.
e. Heat to boiling and boil for 5 minutes. Again filter through a No. 00H filter paper or
equivalent and wash 5 times with dilute HCl.
f. Transfer the filter paper containing the insoluble residue into a pre-ignited and weighed
platinum crucible. Char the filter paper on a Meker burner and place the crucible in an electric
muffle furnace at 1450 ±50 °F. Heat for 30 minutes.
g. Cool in a desiccator and weigh.
h. Calculate as follows:
B-A
percent HCl insolubles
=
x 100
W
5
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