MIL-DTL-44411D
6.4.4 Conditions.
a.
Flow (He): 30 mL/min.
b.
Flow (H2): 30 mL/min.
c.
Flow (Air): 400 mL/min.
d.
Initial temperature: 230 °C.
e.
Initial time: 0.0 min.
f.
Temperature program rate: 10 degrees/min.
g.
Final temperature: 245 °C.
h.
Final time: 7.0 min.
i.
Run time: 8.5 min.
j.
Injector temperature: 250 °C.
k.
Detector temperature: 275 °C.
l.
Injection volume: 2 µ l.
6.4.5 External integrator settings.
a.
Attenuation: 7.
b.
Threshold: 5.
c.
Peak width: 0.04.
d.
Chart speed: 0.50 cm/min.
6.4.6 Standard preparation. In a 50-mL volumetric flask, weigh 50 mg of AgrEvo
Environmental Health, Permanone® 40 Manufacturing Concentrate to the nearest 0.001 gram
and dilute to volume with acetone. Transfer a small portion to a sample vial and label with
contents and date. Place the stopper back on the volumetric flask and label it accordingly.
6.4.7 Sample preparation. In a 50-mL volumetric flask, weigh 125 mg of insect repellent
sample to the nearest 0.001 gram and dilute to volume with acetone. Transfer a small portion to
a sample vial and label with contents and date. Place the stopper back on the volumetric flask
and label it accordingly.
6.4.8 Procedure. After the chromatograph is stable, make three or more injections of the
standard and average the area counts. The injections should be repeatable to within 1 percent.
Do the same for the sample. Calculate the percent purity by using the following formula:
Percent purity = average sample area X weight of standard X 100
average standard area X weight of sample
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