41.1.49
If few undecomposed lumps of Pb soap remain
AOAC Official Method 871.01
Oil (Peanut) in Oils
and Fats
Modified Renard Test
Final Action
Codex-Adopted—AOAC Method*
(Caution: See Appendix B, safety notes on distillation, flammable
solvents, and diethyl ether.)
Weigh 20 g oil into Erlenmeyer. Saponify with alcoholic KOH
solution, 920.160A (see 41.1.18); neutralize exactly with CH3COOH (1
+ 3), using phenolphthalein; and wash into 800–1000 mL flask contain-
ing boiling mixture of 100 mL H2O and 120 mL 20% Pb(CH3COO)2
solution. Boil 1 min and then cool precipitated soap by immersing flask
in H2O, swirling occasionally to cause soap to stick to sides. After
cooling, decant H2O and excess Pb(CH3COO)2 solution, and wash Pb
soap with cold H2O and alcohol, 90% by volume. Add 200 mL ether,
cork, and let stand until soap disintegrates; heat on H2O bath, using reflux
condenser, and boil ca 5 min. With oils, most of soap will be dissolved;
with lards, which contain much stearin, part of soap will be left undis-
solved. Cool ether solution of soap to 15–17° and let stand until all
insoluble soaps separate (ca 12 h).
Filter on Bchner and thoroughly wash insoluble Pb soaps with
ether. Wash ether-insoluble Pb soaps into separator with jet of ether,
alternating with HCl (1 + 3) at end of operation if little of soap sticks
to paper. Add enough HCl (1 + 3) so that total volume of acid is ca
200 mL and enough ether to make its total volume 150–200 mL, and
shake vigorously several min. Let layers separate, drain off acid
layer, and wash ether once with 100 mL HCl (1 + 3) and then with
several portions of H2O until H2O washings are no longer acid to
methyl orange.
(indicated by solid particles remaining after third washing with
H2O), break up by running off almost all H2O layer, adding little
HCl, and shaking; then continue washing with H2O as before.
Distil ether from solution of insoluble fatty acids and dry latter in
flask by adding little absolute alcohol and evaporating on steam bath.
Dissolve dry fatty acids by warming with 100 mL 90% alcohol by
volume. Cool slowly to 15°, shaking to aid crystallization. Let stand
30 min at 15°.
In presence of peanut oil, crystals of arachidic acid separate from
solution. Filter, wash precipitate twice with 10 mL alcohol, 90% by
volume, and then with alcohol, 70% by volume, taking care to keep
arachidic acid and wash solutions at definite temperature in order to
apply solubility corrections given below. Dissolve arachidic acid on
filter with boiling absolute alcohol, evaporate to dryness in weighed
dish, dry, and weigh. To this weight add 0.0025 g/10 mL of 90%
alcohol used in crystallization and washing, if conducted at 15°; if
conducted at 20°, add 0.0045 g/10 mL.
Mp of arachidic acid thus obtained is 71–72°. Weight arachidic
acid × 20 = approximate weight peanut oil present. Arachidic acid
has characteristic appearance and may be identified under micro-
scope. As little as 5–10% peanut oil can be detected by this method.
References: Compt. rend. 73, 1330(1871). Lewkowitsch, “Chemi-
cal Technology and Analysis of Oils, Fats and
Waxes,” 6th ed., 2, 316(1922).
CAS-8002-03-7 (peanut oil)
© AOAC INTERNATIONAL
*Adopted as a Codex Defining Method (Type I) for Renard test of
arachidic and higher fatty acid in edible arachis oil.