41.1.
49 H2O), break up by running off almost all H2O layer, adding little
AOAC Official Method 871.01
Oil (Peanut) in Oils and Fats
Modified Renard Test
First Action 1871
Final Action
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
containing boiling mixture of 100 mL H2O and 120 mL 20%
(CH3COO)2Pb 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 (CH3COO)2Pb solution,
and wash Pb soap with cold water and alcohol, 90% by volume. Add
200 mL ether, cork, and let stand until soap disintegrates; heat on water
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 undissolved. Cool ether solution of soap to 15°–17°C and let
stand until all insoluble soaps separate (ca 12 h).
Filter on Büchner 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 minutes 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. If few undecomposed lumps of Pb soap remain
(indicated by solid particles remaining after third washing with
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°C, shaking to aid crystallization. Let
stand 30 min at 15°C.
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 solu tions at defi nite
temperature in order to apply solubility corrections given below.
Dissolve arachidic acid on filter with boil ing absolute al cohol,
evaporate to dry ness in weighed dish, dry, and weigh. To this
weight add 0.0025 g/10 mL of 90% alcohol used in crystallization
and washing, if con ducted at 15°C; if conducted at 20°C, add
0.0045 g/10 mL.
Mp of arachidic acid thus obtained is 71°–72°C. Weight arachidic
acid ´ 20 = approximate weight peanut oil present. Arachidic acid
has char ac ter istic ap pear ance and may be iden ti fied un der
microscope. As little as 5–10% peanut oil can be detected by this
method.
References: Compt. rend. 73, 1330(1871).
Lewkowitsch (1922) Chemical Technology and
Analysis of Oils, Fats and Waxes, 6th Ed., Vol. 2, p.
316.
CAS-8002-03-7 (peanut oil)
ã 2005 AOAC INTERNATIONAL