FED-STD-791D
Heptylic
7
6.21
10
Caprylic
8
10.82
15
Pelargonic
9
11.87
15
Capric
17.23
20
10
For convenience , these acids hereafter in this method will be referred to by the number
of their carbon atoms; e.g., butyric as C4 , isovaleric as is - C5.
These weights , or some multiole of them are recommended as giving a satisfactory
chromatogram of the acids relative to peak heights.
6. PROCEDURE
6.1 Preparation of apparatus
6.2 Column preparation.
6.3 Packing for chromatographic column prepared as follows
6.4 Dissolve 6.0 g of doethylene glycol adipate polyester in 150 mL of
chloroform with rapid stirring.
6.5 Add 1.06 g of phosphoric acid to the mix and continue stirring until the acid
is completely dispersed.
6.6 Add 23.1 g of Gas Chrom P to the mix and continue stirring for 10 min.
6.7 Remove bulk of chloroform from mix by flash evaporator or on steam bath.
6.8 Remove remaining chloroform by heating in a vacuum oven for 2 h at 200C
and 0.1 cm pressure
6.9 Cool and load into chromatographic column using vibrator on column to
insure uniform and complete packing.
6.10 Chromatograph- Mount the column in the chromatograph and use the
programmed temperature operation. For this operation, set the controls of the
chromatograph for an initial column temperature of140C (284 F), a final column
temperature of 210C (410 F), a temperature rate of 8C (46 F)/min., a hold time of 20
min at the final temperature, an injection port temperature of 220C (428F),a detector
temperature of 220C(428F), abridge current of 150mA, and the helium flow at 30.5
mL/min. The temperature programming must start immediately after injection.
6.11 Test procedure.
6.12 Hydrolysis of lubricant to be analyzed-Weigh 10 g of the lubricant into a
250 mL wide-mouth Erlenmeyer flask, add a solution consisting of 8g of potassium
hydroxide and 15 mL water, followed by 60mL ethyl alcohol. Swirl to mix contents.
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