AOAC Official Method 2000.18 Fat Content of Raw and Pasteurized Whole Milk
Uploaded by
ScribdTranslationsAOAC Official Method 2000.18 Fat Content of Raw and Pasteurized Whole Milk
Uploaded by
ScribdTranslationsAOAC Official Method 2000.
18
Content of fat in raw and pasteurized whole milk
Gerber method by weight
Applicable to whole milk that is raw, pasteurized batch, or high-temperature pasteurized and
short time, and/or homogenized whole milk.
Caution: See Appendix B, safety notes on centrifuges, sulfuric acid, mercury and
organic solvents. Disposal of solvent waste in accordance with rules and regulations
applicable environmental
VerTabla2000.18A for interlaboratory study results supporting acceptance of the
method.
A. Principle
The milk is heavy in the Gerber butyrometer, containing H.2SO4Isoamyl alcohol is added and the
The contents of the butrometer are vigorously mixed to dissolve the curdled and released fat.
fat is isolated by centrifugation and quantified in the graduated portion of the Gerber butyrometer.
B. Reactvos
Sulfuric acid. - Specific gravity 1.820 - 1.825 at 15.5 °C. Technical grade.
Table 2000.18A. Interlaboratory study results for fat percentage in milk
(g/100g) determined by the Gerber method by weighta
Sample ID Media No. Sr SR RSDr’% RSDR’% r R HorRat
Laboratories
Raw 4.431 10-11 0.023 0.05 0.52 1.20 0.06 0.148 0.38
3 5
Pasteurized, homogenized 3.677 10-11 0.029 0.04 0.78 1.08 0.08 0.33
0 0
a
Average based on analysis of seven raw whole milks and four homogenized pasteurized whole milks, respectively. The
standard deviations (Sr, SR) and prediction values (r, R) are based on 8 raw milk samples (two in blind duplicates) and eight milks
Pasteurized homogenized (two in blind duplicates), for a total of 200 tests. Of the total 200 tests, the atypical values
States are identified for five raw milk tests and five pasteurized homogenized milk tests. The standard deviations
relatvas (RSDrRwere calculated as (Sr/media) x 100 y (SR(media) x 100, respectively.
Isoamyl alcohol - Specific gravity 0.814-0.816 at 15.5 °C, bp 128 to 133 °C, free.
of water, acid, fat, and furfural. (Caution: the vapors are poisonous.)
C. Devices
(a) Standard Gerber butyrometer milk testing (graduated 0-8%) with lock cap and
key. – (See figure 2000.18.) A colorless (clear, transparent) borosilicate glass,
resistant, annealed and defect-free; neck, long bulb, flat tube and small bulb,
they gently join on a medium and straight axis to allow for the free flow of liquid;
adjust the wall thickness to provide sufficient strength, but not less than 0.9 mm
at any point. Total length of 190 ± 2.5 mm.
(1) Small bulb. - marked, with matte tape on the side over the graduations for
identify the sample; ≤ 15.0 mm od; capacity measured between the line of
upper graduation and the inner tip of the bulb ≥ 1.5 mL.
Broad bulb. -≤ 25.0 mm od, capacity of 21.5 ± 0.4 mL.
(3) Neck.– Cylindrical and flat; length 15 ± 1.0 mm; 11.5 ± 0.5 mm id; edge,
optionally reinforced; total thickness of the outer edge, ≤ 2.5 mm in diameter.
Flat tube.– Uniform in length of graduated cross section, ≥ 70 mm;
uniform cross-section beyond each terminal graduation, ≥ 3.0 mm;
external width, ≥ 10.0 mm. Graduated with clean permanent lines of 0.10 -
0.20 mm wide and permanently fused color that contrasts clearly
with the color of the milk fat, perpendicular to the axis of the flat tube. The volume
The graduated flat tube at 25 °C is 1,000 mL (13.546 g Hg), divided into 80.
equal parts, each equivalent in volume to 0.0125 mL. The error of the
total calibrated longitudes should not exceed ± ½ of the smallest division.
The graduation lines are uniformly centered on the flat face of the tube.
with lines of 0.1%, no less than 3 mm long; the lines of 0.5% extend
1 mm on each side, beyond the 0.1% lines, and the 1.0% lines, is
extend no more than 1 mm on each side, beyond the lines of 0.5%, or it
extend across the entire flat face. Each whole percentage of graduation,
It is identified by pigmented numbers that run in a series from 0 to 8, to the
right and just over the whole percentage lines, with the measure of zero plus
close to the broad bulb. The bottles are identified as "Milk" with the name or
manufacturer or distributor symbol, permanently inscribed on the body and a
symbol applied after recalibration, where certification is required
compliance with regulatory specifications.
Tests.– The accuracy of each bottle must be determined before use.
(usually by the manufacturer or the calibration laboratory). Mercury is added.
the butrometer through a special volumetric device. The test is
brought to room temperature at 20 ± 2 °C. The small bulb opens to
prevent trapped air bubbles. The device has 2 volumetric settings. The
The first adjustment releases a variable volume that allows the filling of mercury.
inside the butrometer, until the menisci reach the graduation line
zero. The second adjustment dispenses 1,000 mL of mercury, corresponding to 8% in
the graduated scale. The difference between what was expected and what was observed in the reading of
the scale should not exceed the division ± ½ of the graduation line (± 0.05 % of
fat). The accuracy of the testing device is regularly verified with a
officially calibrated glassware.
Lock and key cap. – The lock cap is made of durable rubber.
standardized dimensions to fit into the neck of the
button meter, shaped to provide a seat for the ball or the plug and with a
channel for the key. The edge and the channel are reinforced with metal, plastic, or another
insertion of firm union. The key is made of a non-corrosive material, suitable for
insert into the stopper.
Shelf support for the butrometer. - To hold the butrometers in a vertical position.
secure.
(c) Dispensers. - To release 10 mL HSO 2 4and 1 mL of isoamyl alcohol.
(d) Centrifuge. - For the butrometers, preferably provided with an indicator of
speed to evaluate 1150 ± 70 rpm. If it is not equipped with the speed indicator,
check the operating speed of the Gerber centrifuges, under a full load,
regularly with a tachometer. The design of the centrifuge must ensure that the
The temperature of the contents of the butrometer after centrifugation is between 30 and 50 °C.
When loaded, the centrifuge must produce an acceleration within 2 minutes.
relative centrifuge of 350 ± 50 xgen the outer end of the butyrometer stopper.
This acceleration is produced by centrifuges with the following effective radius (the
horizontal distance between the center of the axis of the centrifuge and the outer end of the
butrometer plug operated at the indicated speed. (Table 2000.18B).
(e) Water bath for the butrometer test. – With a thermometer, device for
maintain the temperature of the fat column at 60 - 63°C, and providing a
intermittent or constant agitation. The depth of the water bath should allow for a
vertical immersion of the buoy to the small terminal bulb.
Table 2000.18A. Centrifugal speed.
Effective radio, mm Revolutions per minute ± 70 rpm
240 1140
250 1120
260 1100
270 1080
300 1020
(f) Water bath to temper the milk test samples before weighing. – With a
thermometer and a device to maintain the temperature of the milk at 39 ± 1 °C.
(g) Analytical balance - Weighing to the nearest 0.01 g. Check the accuracy periodically.
and every time the balance is moved or deleted. Keep a record of the controls of
calibration of the balance.
(h) Calibration weights. – Classify S, standardize the calibration weights to verify the
precision of the balance within weight range to weigh the empty butrometers, and the
thermometers that contain test portions.
Reading light. – As a background when measuring fat columns. The light should be diffuse.
(smooth and white) and provide lighting from angles above and below the level of the
fat column and at eye level. It is a useful magnification device that helps to
the reading.
D. Determination
(a) Preparation of milk test samples. - Position the test sample of
milk in a water bath maintained at 39 ± 1 °C. The level of H2O must be at the level of the
milk or about it. Mix milk 10 times by inversion. If the fat line remains within
the surface of the container, let hot water from the tap run (50 – 60 °C
approximately) on the exterior of the surface for 15 - 20 s. Mix completely
for investment and despite the test portion immediately. Do not let the milk
stay in the water bathroom for more than 15 minutes before it reaches 38°C.
(b) Test. - Add 10.0 ± 2 mL of HSO 2 4at 15 - 20 °C in the butyrometer. Tare the butyrometer
containing H2SO4on an analytical balance. Weighed 11.13 ± 0.03 g tempering the sample of
milk test, D (a), inside the butyrometer, add milk slowly at the beginning, to
prevent violent reactions with the acid. Add 1 ± 0.005 mL of isoamyl alcohol to the
butrometer containing a portion of the sample. Insert the lock plug in the shape
safe, using the portable key. Using insulated gloves, hold the butrometer by the
graduated neck with the upper end covered. Without letting the small bulb empty,
beat until all traces of curd disappear. Holding the butrometer with
the two ends covered and the neck graduated, invert at least 4 times to mix
the remaining acid in the small bulb and the graduated neck, with the content of the bulb
longer.
Place the butrometers in the centrifuge, with the small bulb pointing upwards and
balancing. Centrifuge for 4 minutes after reaching the appropriate speed.
Transfer the butrometers to a water bath maintained at 60 – 63 °C and immerse, leaving
only the small bulb exposed. Allow the fat column to equalize for ≥
5 min.
Remove a water butt from the bathroom and let it dry. Apply pressure to the lock.
cap to carry the bottom line of the grease column upwards, to make it
match the nearest whole percentage grade mark. Read promptly
the scale of the upper meniscus bottom to the nearest 0.05%.
E. Repeat the analysis
Repeat the analysis if the fat column is cloudy or dark in color, or if there is white material or
black at the bottom of the fat column. Acceptable fat columns are yellow.
pale to strong and completely uniform, without light or dark particles.
F. Calculations
