43.1.14 Weigh test portion as specified in Table 962.17.

Quantitatively
AOAC Official Method 962.17 transfer test portion to 2 L Erlenmeyer flask. Add ca 1200 mL H2O or
Volatile Oil in Spices NaCl solution, C(b), (see Table 962.17 for distillation solvent) and
First Action 1962 add 2–3 drops of antifoam. Insert stirring bar.
Final Action 1965 Before placing volatile oil trap on flask, ensure that trap is clean.
Revised First Action 1996 Place trap on flask using small amount of non-volatile stopcock
A. Principle grease on ground joints. Fill collection arms with H2O or NaCl
solution as specified in Table 962.17. {Note: For allspice, anise, and
Test portion is boiled in H2O or NaCl solution. Released volatile
cloves add trap additive to graduated portion (see Table 962.17).
oil (vapor form) is condensed and collected in trap, and then
Add 2 mL xylene using 5 mL pipet and verify added volume using
measured through trap calibration.
volatile oil trap calibration [see B(a)]. Repeat analysis if part of
B. Apparatus xylene passes back into flask during distillation.}
(a) Volatile oil trap.—5 mL, without stopcock, or distilling Connect trap to condenser using small amount of nonvolatile
receivers crankcase oil, ASTM, 5.0 ´ 0.1 mL subdivisions (see stop cock grease and con nect con denser to re frig er ated
Figure 962.17). Available from Wilmad Labglass (Part No. LX circulating bath set at 20°C. Insulate neck of trap and flask with
4448-1002; 1002 Harding Hwy, Buena, NJ 08310-0688, USA). insulating tape.
Once a year calibrate trap for xylene retention by running 3 blanks. Heat flask on stirring hot plate with constant stirring. Adjust
Use average volume. trap and con denser so that drops flow down the wall of trap and do
(b) West condenser.—400 mm long with drip tip and standard not drop directly on surface of liquid. Gently swirl flask several
taper 24/40 ground joints. times during initial heating until test portion is at rolling boil to
(c) Centrifugal grinding mill.—Set with 0.75 mm mill screen. eliminate scorch ing of test portion on walls. Maintain reflux rate
Cold grinder can be used. (Note: To pre serve vol a tile oil of 5–15 drops/10 s. Distill 8 h or until 2 consecutive readings
constituents, it is critical that mill does not generate heat during taken at 1 h intervals show no change of oil vol ume in trap. If
grinding of test sample.) separation of oil is not sat isfactory, add 1–2 drops of dishwashing
(d) Erlenmeyer flask.—2 L; equipped with standard taper 24/40 liquid to trap through condenser or 2–3 mL saturated NaCl
ground joint. solution.
(e) Stirring hotplate.—Suitable for 2 L flask with variable Cool to 20°C either by allowing trap to stand at ambient
voltage transformer. temperature or by immersing in water bath. If trap is read at
(f) Stirring bars.—Teflon-coated, egg-shaped.
(g) Pipet filler.
(h) Cylinder.—2 L, graduated.
(i) Tubing.—Tygon tubing Norton, 79 mm id, or equivalent.
(j) Refrigerated circulating bath.—Maintaining 20°C.
(k) Insulating tape.
(l) Blender.
C. Reagents
(a) Xylene.—Reagent grade.
(b) Sodium chloride (NaCl) solution.—10% (w/v).
(c ) A n t i f o a m B . —Sil i cone emul sion con tain i ng 1%
hydrogenated tallow glycerides (Dow Corning or equivalent).
(d) Liq uid glassware cleaner.—Such as Fisherbrand
Versa-Clean Concentrate.
D. Determination
Weigh 200 g test portion. Crack ginger and turmeric before
grinding. Set grinder with 0.75 mm mill screen. More than 99% must
pass through 0.85 mm sieve during the first run. Regrind oversize
until test portion passes sieve.
Mix ground material thoroughly and store in re frigerator
(2°–6°C) in tightly sealed container until analysis.
Clean volatile oil trap by soaking overnight in liquid glassware
cleaner solution, C(d). Rinse with tap water. Check cleanliness of
trap by adding small volume of distilled water. Water should flow
down the wall of trap smoothly. Otherwise, repeat cleaning
procedure.
Before removing test portion for analysis, mix ground material in
container by rotating, to avoid stratification. Allow test sample to
equilibrate to ambient temperature. Figure 962.17. Apparatus for volatile oil in spices.
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Table 962.17. Weights, distillation solvents, and trap Volatile oil, % (v/w) = (Vo/Ws) × 100
additives for various spices

Test portion Distillation Trap where Vo = volume of oil collected in trap, mL; and Ws = weight of
Spice weight, g solvent additive test portion, g.
10% NaCl Xylene, When using 2 mL xylene (Vx) as trap additive, calculate
Allspice 40 solution 2.0 mL concentration of volatile oil, % (v/w), in test sample as follows:
10% NaCl Xylene,
Anise 50 solution 2.0 mL Volatile oil, % (v/w) = [(Vo – Vx)/Ws] × 100
Basil 50 H2O —
Bay leaves 60 H2O — where Vx = volume of residual xylene, mL.
Caraway 50 H2O — References: JAOAC 17, 70, 371(1934); 18, 611(1935);
Cardamon 50 H2O — 21, 435(1938); 22, 598(1939); 25, 700(1942);
Celery seed 50 H2O —
33, 575(1950); 36, 752(1953); 37, 390(1954);
38, 548(1955); 42, 312(1959); 45, 212(1962).
10% NaCl Xylene,
Cloves 10 solution 2.0 mL F. Specific Gravity of Volatile Oil
Coriander 70 H2O — Determine specific gravity at 25/25°C as in 948.22 (see 40.1.05)
Cumin 50 H2O — and 950.48 (see 40.1.06), using 1 mL Sprengel tube.
Dill seed 50 H2O — G. Refractive Index of Volatile Oil
Fennel 50 H2O — See 950.50 (see 40.1.09) and 950.51 (see 40.1.10).
Fenugreek 50 H2O —
H. Eugenol in Volatile Oil (Final Action 1965)
10% NaCl
Ginger 50 solution — Measure 2 mL volatile oil (transfer pipet) into Babcock milk
Marjoram 40 H2O — bottle, 989.04C(a) (see 33.2.27). Add 20 mL 3% KOH solution
(w/v), shake mixture 5 min, heat 10 min in boiling water bath,
Nutmeg 30 H2O —
remove, and cool to room temperature. When liquids separate
Mace 20 H2O — completely, add enough KOH solution to bring residual oil within
Oregano 40 H2O — graduated portion of neck and note volume. Calculate % by volume
Black pepper 50 H2O — from difference between volume of test portion used and residual
White pepper 40 H2O — oil.
Rosemary 50 H2O —
CAS-97-53-0 (eugenol)
Sage 50 H2O —
I. Volatile Oil and Resin in Ginger (Final Action 1965)
Savory 40 H2O —
Tarragon 40 H2O —
Place 50 g ground ginger in Soxhlet extractor and extract
completely with ether (ca 4 h). Transfer extract to 300 mL flask and
Thyme 50 H2O —
evaporate ether on steam bath until solvent is no longer detected. Add
Turmeric 50 H2O — 50 mL H2O to residue and determine yield of volatile oil (using trap
for oils lighter than H2O), specific gravity, and refractive index, as in
D–G.
temperature other than 20°C, include it in report. Read volume of oil Transfer residue in flask to separator and extract resin with ether.
collected to the nearest 0.01 mL. Transfer to tared beaker, evaporate ether on steam bath, and dry to
constant weight in vacuum desiccator.
E. Calculations
Calculate concentration of volatile oil, % (v/w), in test portion as Reference: JAOAC 19, 98, 411(1936).
follows: Revised: March 1998

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