33.2.27A AOAC of Fi Cial Method 2000.18 Fat Con Tent of Raw and Pas Teur Ized Whole Milk

33.2.27A $3.0 mm; external width, $10.0 mm.
Graduated with permanent,

AOAC Official Method 2000.18 clean lines of 0.10–0.20 mm width and permanently fused color
Fat Content contrasting sharply with color of milk fat, perpendicular to flat tube
of Raw and Pasteurized Whole Milk axis. Graduated volume in flat tube at 20°C is 1.000 mL (13.546 g
Gerber Method by Weight Hg), divided into 80 equal parts, each equivalent in volume to
First Action 2000 0.0125 mL. Error of total calibrated length is not to exceed ±½ of
Final Action 2004 smallest graduation. Graduation lines are uniformly centered on flat
(Applicable to whole milk that is raw, batch pasteurized or high tube face, with 0.1% lines not less than 3 mm long, the 0.5% lines
temperature short time [HTST] pasteurized, and/or homogenized.) extending 1 mm on each side beyond the 0.1% lines, and the 1.0%
lines extending not less than 1 mm on each side beyond the 0.5%
Caution: See Appendix B, safety notes on centrifuges, sulfuric lines or extending across the entire flat face. Each whole percent
acid, mercury, and organic solvents. Dispose of waste graduation is identified by pigmented numbers running serially
solvents according to applicable environmental rules from 0 to 8, at the right and just above the whole-percent lines, with
and regulations. the zero measurement nearest the large bulb. Bottles are identified
“Milk,” with the name or symbol of the manufacturer or distributor
See Table 2000.18A for the results of the interlaboratory study permanently inscribed on the body and a symbol applied after
supporting acceptance of the method. recalibration where required to attest conformance with regulatory
A. Principle specifications.
Milk is weighed into Gerber butyrometer containing H2SO4. (5) Testing.—Accuracy of each bottle should be determined
Isoamyl alcohol is added and butyrometer contents are vigorously before use (usually by manufacturer or calibration laboratory).
mixed to dis solve curd and re lease fat. Fat is iso lated by Mercury is added to the butyrometer by means of a special
centrifugation and quantified in the graduated portion of the Gerber volumetric apparatus. Testing is conducted at ambient temperature
butyrometer. at 20° ± 2°C. The small bulb is opened to prevent trapped air
B. Reagents bubbles. The apparatus has 2 volumetric settings. The first setting
delivers a variable volume that permits filling mercury into the
(a) Sulfuric acid.—Specific gravity 1.820–1.825 at 15.5°C.
butyrometer until the meniscus reaches the 0 graduation line. The
Technical grade.
second setting dispenses 1.000 mL mercury, corresponding to 8% on
(b) Isoamyl alcohol.—Specific gravity 0.814–0.816 at 15.5°C,
the graduated scale. The difference between the expected and
bp 128° to 133°C, free of water, acid, fat, and furfural. (Caution: observed scale readings must not exceed ±½ division of a graduation
Vapors are poisonous.) line (±0.05% fat). The accuracy of the testing apparatus is regularly
C. Apparatus verified with officially calibrated glassware.
(a) Standard Gerber milk-test butyrometer (graduated 0–8%) (6) Lock stopper and key.—Lock stopper is of reagent-resisting
with lock stop per and key.—(See Fig ure 2000.18.) Clear rubber, of standardized dimensions to fit in neck of butyrometer,
transparent, colorless, resistant borosilicate glass, annealed and free molded to provide a seat for the ball or plug, and with a channel for
from defects; neck, large bulb, flat tube, and small bulb on a straight the key. Rim and channel are reinforced by metal, plastic, or other
median axis, joined smoothly to permit free flow of liquid; wall firm binding insert. Key is of noncorrodible material suitable for
thickness adequate to provide sufficient strength but not less than inserting into the stopper.
0.9 mm at any point. Total length 190 ± 2.5 mm.
(b) Butyrometer support rack.—To hold butyrometers in a
(1) Small bulb.—Tapered, with matte surface on side above
secure, vertical position.
graduations for sample identification; #15.0 mm od; capacity,
measured between top graduation line and internal end of bulb (c) Dispensers.—To deliver 10 mL H2SO4 and 1 mL isoamyl
$1.5 mL. alcohol.
(2) Large bulb.—#25.0 mm od; capacity, 21.5 ± 0.4 mL. (d) Centrifuge.—For butyrometers, preferably provided with a
(3) Neck.—Cylindrical and plain; length, 15 ± 1.0 mm; 11.5 ± speed indicator to assess 1150 ± 70 rpm. If not equipped with speed
0.5 mm id; rim, optionally reinforced; total thickness of external indicator, check operation speed of Gerber centrifuges under full
rim, #2.5 mm diameter. load regularly with a tachometer. Design of the centrifuge shall
(4) Flat tube.—Uniform in cross-section graduated length, ensure that temperature of butyrometer contents after centrifuging is
$70 mm; uniform cross-section beyond each terminal graduation, between 30° and 50°C.
a
Table 2000.18A. Interlaboratory study results for percent fat in milk (g/100 g) determined by Gerber by weight method
Sample ID Mean No. of labs sr sR RSDr, % RSDR, % r R HorRat
Raw 4.431 10–11 0.023 0.053 0.52 1.20 0.065 0.148 0.38
Pasteurized, homogenized 3.677 10–11 0.029 0.040 0.78 1.08 0.080 0.111 0.33
a
Mean based on analysis of 7 raw whole milk and 4 pasteurized homogenized whole milk, respectively. Standard deviations (sr, sR) and prediction values (r, R)
based on analyses of 8 raw milks (2 in blind duplicates) and 8 pasteurized homogenized milks (2 in blind duplicates), for a total of 200 tests. Of the total of 200
tests, statistical outliers were identified for 5 raw milk tests and 5 pasteurized homogenized milk tests. Relative standard deviations (RSDr, RSDR) were
calculated as (sr/mean) ´ 100 and (sR/mean) ´ 100, respectively.
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Figure 2000.18. 8% Gerber milk-test butyrometer.
When loaded, the centrifuge must produce, within 2 min, a butyrometer, adding milk slowly at first to prevent charring and
relative centrifugal acceleration of 350 ± 50 ´ g at the outer end of violent reaction with acid. Add 1 ± 0.05 mL isoamyl alcohol to
the butyrometer stop per. This ac cel er a tion is pro duced by butyrometer containing test portion. Insert lock stopper securely
centrifuges with the following effective radius (horizontal distance using hand-held key. Wearing insulated gloves, grasp butyrometer
between the center of the centrifuge spindle and the outer end of the at graduated neck with stoppered end up. Without allowing small
buty rometer stop per) op er ated at the speed in di cated bulb to empty, shake until all traces of curd disappear. Holding
(Table 2000.18B). butyrometer by both stoppered end and graduated neck, invert at
(e) Water bath for test butyrometers.—With thermometer, device least 4 times to mix acid remaining in the small bulb and graduated
to maintain temperature of fat column at 60°–63°C, and providing neck with the contents of larger bulb.
intermittent or constant agitation. Depth of water bath must permit
vertical immersion of butyrometer to terminal (small) bulb. Place butyrometers in centrifuge, small bulb pointing up, and
(f) Wa ter bath for tem per ing milk test samples prior to counterbalance. Centrifuge 4 min after proper speed is reached.
weighing.—With thermometer and device to maintain temperature Transfer butyrometers to water bath maintained at 60°–63°C and
of milk at 39° ± 1°C. immerse, leav ing only small bulb ex posed. Let fat col umn
(g) Analytical balance.—Weighing to nearest 0.01 g. Check equilibrate for ³5 min.
accuracy periodically and whenever balance is moved or cleaned.
Keep record of balance calibration checks. Remove one butyrometer from water bath and wipe dry. Apply
(h) Calibration weights.—Class S, standard calibration weights gentle pressure to lock stopper to bring bottom line of fat column
to verify balance accuracy within weight range to be used for upward to coincide with nearest whole percentage graduation mark.
weighing empty milk butyrometers and butyrometers containing Promptly read scale at bottom of upper meniscus to nearest 0.05%.
test portions.
(i) Reading light.—As background when measuring fat columns.
Light should be diffused (soft white) and provide illumination from E. Repeat Analysis
angles above and below level of fat column and at eye level.
Magnification device to aid reading is useful. Repeat analysis if fat column is turbid or dark in color, or if there is
white or black material at bottom of fat column. Acceptable fat
D. Determination
columns are pale to strong yellow and uniform throughout with no
(a) Preparation of milk test samples.—Place milk test sample in light or dark particles.
water bath maintained at 39° ± 1°C. Level of H2O should be at or
above milk level. Mix milk 10´ by inversion. If fat line remains on
F. Calculations
inside surface of container, run hot tap water (ca 50°–60°C) over
outside surface for 15–20 s. Mix thoroughly by inversion and weigh Calculate % (w/w) fat content in milk as follows:
test portion immediately. Do not allow milk to remain in water bath
more than 15 min after reaching 38°C.
(b) Testing.—Add 10.0 ± 0.2 mL of H2SO4 at 15°–21°C to Fat, % =
butyrometer. Tare butyrometer containing H2SO4 on analytical reading at upper meniscus – reading at lower meniscus
balance. Weigh 11.13 ± 0.03 g tempered milk test sample, D(a), into
Reference: J. AOAC Int. 84, 1499(2001).
Table 2000.18B. Centrifuge speed
Effective radius, mm Revolutions per min ±70 rpm

240 1140
250 1120
260 1100
270 1080
300 1020
2006 AOAC INTERNATIONAL
ã 2005 AOAC INTERNATIONAL

33.2.27A AOAC of Fi Cial Method 2000.18 Fat Con Tent of Raw and Pas Teur Ized Whole Milk

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33.2.27A AOAC of Fi Cial Method 2000.18 Fat Con Tent of Raw and Pas Teur Ized Whole Milk

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33.2.27A $3.0 mm; external width, $10.0 mm.

Graduated with permanent,

2006 AOAC INTERNATIONAL

ã 2005 AOAC INTERNATIONAL

Table 2000.18B. Centrifuge speed

Effective radius, mm Revolutions per min ±70 rpm

2006 AOAC INTERNATIONAL

ã 2005 AOAC INTERNATIONAL

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