MIL-DTL-14067C
k. Identify and integrate the acetylene peak in each chromatogram. Average the acetylene
peak areas and record this value as "D".
l. Disassemble reaction vessel and dispose of the sulfuric acid. Rinse the flask with distilled
water, then with acetone and air dry completely.
4.5.4.1.8 Sample analysis.
a. Insert the two 24/40 barbed adapters into the flask, but not the addition funnel.
b. Pre-weigh powder funnel and weighing paper.
c. Weigh (to the nearest 0.001 gram) a 0.500 ± 0.020 gram aliquot of sample magnesium.
d. Transfer sample into the flask using the powder funnel, making sure no powder gets on
the ground-glass joint.
e. Re-weigh the powder funnel and weighing paper to determine the weight "E" of sample
transferred to the flask.
f. Completely assemble the reaction apparatus, and transfer 50.0 milliliters of 5 % wt
sulfuric acid to the addition funnel.
g. Evacuate the flask using vacuum pump.
h. Turn 3-way valve to connect flask and manometer exclusively.
i. Open addition funnel stopcock to dispense acid into reaction flask; shut the stopcock
immediately after all the acid has dispensed. Wait 15 minutes after bubbling completely
stops in the reaction flask.
j. Record the flask internal pressure as "F", and the atmospheric pressure "G".
k. Withdraw two 100 microliter samples from the flask and inject 50 microliters of each
onto the GC using the same technique as the blank (4.5.4.1.6 e. through i.).
l. Average acetylene peak areas and record the value as "H".
m. Rinse the flask with distilled water, then with acetone and air dry completely.
n. Analyze a duplicate aliquot of magnesium the same way (4.5.4.1.8 a. through m.).
4.5.4.1.9 Sample calculation. Evaluate the expression below for each of the two aliquots
and average the results to calculate carbide content in terms of magnesium carbide (acetylide).
Report the average of the two aliquots.
Where:
A = Average acetylene peak areas. (see 4.5.4.1.6, k.).
B = Atmospheric pressure, (bar). (see 4.5.4.1.7, f.)
C = Exact volume, (mL). (see 4.5.4.1.7, g.)
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