MIL-DTL-14067C
f. With the syringe valve open and needle inserted through the septum, slowly pump the
plunger 5 - 10 times to fill and empty the syringe.
g. Fill the syringe with 100 microliters of gas from the flask, close the syringe valve and
remove the needle from the septum.
h. When ready to make injection into GC, depress the plunger of the syringe to 80
microliters and open the syringe valve.
i. Depress the plunger further to 50 microliter and quickly inject the syringe contents onto
the GC and run the sample.
j. Once GC run is complete, take a second sample from the flask and inject the same way
(4.5.4.1.6 e. through i.).
k. Identify and integrate the acetylene peak in each chromatogram. Under the recommended
conditions, C1-C2 peaks should elute between 3 and 4 minutes in order of increasing
molecular weight, however the blank may not show any signal above noise. Acetylene is
the second fastest-eluting peak. Average the acetylene peak areas and label this value
"A". Keep the sulfuric acid in the flask for preparation of calibration standard.
4.5.4.1.7 Calibration standard.
a. Attach regulator to reference gas cylinder. Check for leaks and proper operation.
b. Open main cylinder valve. Lower the outlet pressure by turning the regulator knob
completely counter-clockwise. The gauge of a single stage regulator displays the gas
pressure inside the cylinder, not the outlet pressure.
c. Attach needle to 25 milliliter syringe, open syringe valve and insert needle through
regulator s syringe adapter.
d. Slowly turn the regulator knob clockwise until the plunger begins to move and syringe
begins to fill. Fill and empty the syringe 5 times, then fill with 25 milliliters of reference
gas, close syringe valve and withdraw the needle.
e. Evacuate flask headspace using the vacuum pump and turn 3-way valve to exclusively
connect flask and manometer.
f. Record the atmospheric pressure and label it "B".
g. Depress 25 milliliter syringe plunger to 20 milliliters and open the valve, depress plunger
further to a volume between 10 and 12 milliliters, note the exact volume "C" to nearest
0.2 milliliter, and insert needle through reaction flask septum and inject syringe contents.
Then, withdraw the needle from the reaction flask septum.
h. Open addition funnel stopcock to let flask fill with air.
i. Close stopcock, allow 10 minutes for flask to warm to room temperature, then open and
close the valve to equilibrate pressure.
j. Withdraw a 100 microliter sample from the flask and inject 50 microliters of it onto the
GC in the same manner as the blank (4.5.4.1.6 e. through i.). Repeat twice more.
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