MIL-DTL-14067C
e. Valve, 3-way, glass stopcock, e.g. Kontes 843900-0002 or eq. Quantity: 1.
f. Rubber stopper/septum fitting barbed adapter, above, e.g. Fisher 20190 or eq. Quantity: 1
per sample run.
g. Gas regulator, single stage CGA-165 with syringe adapter, e.g. Sigma 501395 or eq.
Quantity:
h. Powder funnel, preferably metal, with 5 centimeter long stem fitting 24/40 port or eq.
made from aluminum foil. Quantity: 1.
i. Syringe, 0.1 milliliter, gas-tight with locking valve and 22 or 23 gauge, 2 inch needle, e.g.
SGE 100R-V-GT or eq. Quantity: 1, spares recommended.
j. Syringe, 25 milliliter, gas-tight with locking valve and Luer lock connection, e.g. SGE
25MR-VLLMA-GT or eq. Quantity : 1.
k. Needle, 22 or 23 gauge, 2 inch length, fitting Luer lock connection, e.g. SGE 039802 or
eq. Quantity: 1, spares recommended.
l. Silicone grease, high vacuum. Quantity: approximately 5 grams.
m. Support stand with clamp assortment. Quantity: 1, clamps as needed.
n. Tubing, thick-wall rubber, 1/4 inch ID. Quantity: approximately 1 foot.
o. Tubing, thick-wall rubber, 1/8 inch ID. Quantity: approximately 1 foot.
p. Union, barbed, reducing 1/4 in to 1/8 inch. Quantity: 1
q. Volumetric glassware, assorted. Quantity: as needed.
r. Gas chromatograph (GC) with flame ionization detector (FID) and computer/integrator.
Compressed air, hydrogen, and helium supply as recommended by GC manufacturer.
Quantity: 1
s. Vacuum pump or other vacuum source, 5 kiloPascal ultimate vacuum or better in less
than 5 minutes, e.g. Sartorius 16615 or eq. Quantity: 1
t. Laboratory balance, ≥ 200 gram capacity, 0.001 gram resolution or better. Quantity: 1
u. Manometer, digital, range: 0 to ≥200 kiloPascal, resolution: 0.2 kiloPascal or better, e.g.
Omega HHP4230 or eq. Quantity: 1
v. Room thermometer. Quantity: 1
w. Barometer, digital or analog, 0.2 kiloPascal resolution or better. Quantity: 1
4.5.4.1.5 Procedure. Set up the GC. Install and condition capillary column as required by
manufacturer. The following analysis conditions are recommended: oven maintained at 140oC
for a 5 minute analysis time, injector at 125oC flowing helium at 2 mL/min with a 20-fold split,
FID at 250oC and maximum sensitivity setting and burning a mixture of hydrogen and air, fed at
40mL/min 400 mL/min, respectively. Assemble reaction apparatus as illustrated in Figure 1.
Lubricate with silicone grease all moving parts and all joints and connections; remove excess
grease. Support assembly with clamps and stand. Test gas-tightness of the assembled glassware.
Evacuate the vessel and manometer connection using vacuum pump. Turn 3-way valve to
exclude the vacuum pump and connect manometer and vessel. Observed pressure reading
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