SAMPLING A N D ANALYSIS OF COMMERCIAL FATS A N D OILS

AOCS Official Method Ca 5a-40

Reapproved 1997
CP

Free Fatty Acids'

DEFINITION
This method determines the free fatty acids existing in the sample.
SCOPE
Applicable to all crude and refined vegetable oils, marine oils and animal fats.

APPARATUS (a) Free fatty acids as oleic, % =

I . Oil sample bottles-I15 or 230 mL (4 or 8 oz), or 250-
mL Erlenmeyer flasks.
REAGENTS
1. Ethyl alcohol, 95%-USSD formulas 30 and 3A are
permitted (see Notes, 1). The alcohol must give a defi-
nite, distinct and sharp end point with phenolphthalein
and must be neutralized with alkali to a faint, but
permanent pink color just before using.
2. Phenolphthalein indicator solution-1 % in 95% alcohol.
3. Sodium hydroxide solution-accurately standardized.
See AOCS Specification H 12-52. See Table I for the
appropriate normality of the sodium hydroxide solu-
tion, depending on the expected free fatty acid concen-
tration range in the sample.
Table 1
Free fatty acid range, alcohol volume and strength of alkalia
FFA range (%) Sample (g) Alcohol (mL) Strength of alkali
mL of alkali x N x 28.2
mass, g of sample
(b) Free fatty acids as lauric,% =
mL of alkali x N x 20.0
mass, g of sample
(c) Free fatty acids as palmitic, % =
mL of alkali x N x 25.6
mass, g of sample
2. The free fatty acids are frequently expressed in terms
of acid value instead of percentage free fatty acids. The
acid value is defined as the number of milligrams of
KOH necessary to neutralize 1 g of sample. To convert
percentage free fatty acids (as oleic) to acid value,
multiply the percentage free fatty acids by 1.99.
PRECISION
Precision data for refined, bleached and deodorized oils are
shown in Table 2. Precision data for crude oils are shown in
Table 3.

Table 2
The average, expected between-laboratory variation (stan-
dard deviation of reproducibility, SR) for the determination
"FFA, free fatty acid; N, normality. of free fatty acids in refined, bleached and deodorized oilsa
-- - - - -

Approximate
PROCEDURE ,

FFA value (%) 0-0.05 0.05-0.1 0.1- 1.0 1.0-2.0

I . samples must be well mixed and entirely liquid before
weighing; however, do not heat the sample more than R , 0.007 0.0 10 0.046 0.073
10°C over the melting point. RSD (CV, %) 33.93 12.73 9.90 4.75
2. Use Table I to determine the sample weight for various R (95%)= 2.8 x SR 0.02 0.03 0.13 ., 0.20
ranges of fatty acids. Weigh the designated sample size "Values obtained from the AOCS Smalley Laboratory Proficiency
into an oil sample bottle or Erlenmeyer flask (see
Program.
Notes, 2).
3. Add the specified amount of hot neutralized alcohol
and 2 mL of indicator. Table 3
4. Titrate with standard sodium hydroxide, shaking vigor- The average, expected between-laboratory variation (stan-
ously until the appearance of the first permanent pink dard deviation of reproducibility, SR) for the determination
color of the same intensity as that of the neutralized of free fatty acids in crude oilsa
alcohol before the addition of the sample. The color Approximate
must persist for 30 seconds. FFA value (%) 0.1-1 .O 1 .O-2.0
0.077 0.156
CALCULATIONS R
1. The percentage of free fatty acids in,most types of fats RSD (CV, 9%) 14.57 9.84 .
and oils is calculated as oleic acid, although in coconut R (95%)= 2.8 x S , 0.22 0.44
and palm kernel oils it is frequently exp6sed as lauric "Values obtained from the AOCS Smalley Laboratory Proficiency
acid and in palm oil in terms of palmitic acid. Program.

Page 1 of 2
 SAMPLING A N D ANALYSIS O F COMMERCIAL FATS A N D OILS ',

AOCS Official Method Ca 3a-46

Replacing Ca 3-25 and Ca 3-46 Reapproved 1997
h

Insoluble impurities"
DEFINITION
This method determines dirt, meal and other foreign substances insoluble in kerosene and petroleum
ether.
SCOPE
Applicable to all normal fats and oils.

APPARATUS
1. Gooch crucible--prepared with a glass-fiber filter with-
out organic filler (Reeve Angel 934 AH or WhatmanJ
GF/C). Wash the filter with y , ~ x , all;l2b& and e h s
Dry to constant weight at I0 I k 1"C Cool in a desicca-
tor to room temperature and weigh. J
2. Filter flask of convenient size ahd Gooch crucible
v in a desiccator and weigh.
(
adapter.
F
3. Filter through the prepared Gooch crucible with the aid
of a vacuum. Wash with five 10-mL portions of hot
kerosene, allowing each portion to drain before adding
the next.
4. Wash thoroughly with petroleum ether to remove all of
the kerosene. Dry the crucible and contents to a
constant weight at 101 k 1°C. cool to room temperature

REAGENTS (see Notes, Caution) CALCULATIONS

1. Petroleum ether-AOCS Specification H 2-41.
2. Kerosene-refined petroleum distillate with a flash
point not below 23°C (75°F). as determined by the
American Society for Testing and Materials Standard
Method D56, using the tag closed tester. The kerosene
should be filtered through a Gooch crucible, prepared
as in Apparatus, I, before using.
PREPARATION O F SAMPLE
1. Samples must be mixed thoroughly. If necessary, soften
with gentle heat (do not melt) and mix thoroughly with
an efficient mixer.
PROCEDURE
1. Use the residue from the moisture and volatile matter
determination (AOCS Official Methods Ca 2b-38 or Ca
2d-25), or a sample prepared in the same manner (see
Notes, I).
2. Add 50 mL of kerosene to the residue.and heat in a
,,,-
\
.- water bath to dissolve the fat.
1. Insoluble impurities, % =
gain in mass.of crucible
x loo
mass of sample taken for moistvre
NOTES
Caution
Petroleum ether and kerosene are flammable solvents. A
fume hood should be used at all times when working with
these solvents.
NUMBERED NOTES
. I . Samples (e.g., certain feed stocks) with a higher than
usual percentage of insoluble impurities may be diffi-
cult, if not impossible, to filter. A study among five
laboratories indicated that, for such samples, a 2-g
subsample (rather than a 5-g subsample as specified in
AOCS Ofticial Methods Ca 2b-38 and c a 2d-25) can be
used without greatly affecting the precision of the
method.

Page 1 of 1