33.2.43
Only touch
AOAC Official Method 990.19
Solids (Total) in Milk
By Forced Air Oven Drying
after Steam Table Predry
First Action 1990
Final Action 1993
IDF–ISO–AOAC Method
Results of the interlaboratory study supporting acceptance of the
method:
sr = 0.017; sR = 0.047; RSDr = 0.136%; RSDR = 0.370%
A. Principle
Total solids are determined by weighing milk, drying milk, and
weighing dried milk residue. Test portion is predried 25 min on
steam bath and then dried 3 h at 100° ± 1°C in forced air oven. Total
solids content of milk is weight of dried milk residue as % of original
milk weight.
B. Apparatus
(a) Weighing dishes.—Flat bottom, ³5 cm diameter, without
cover. If disposable aluminum dishes are used, they should be ones
manu fac tured by “oil-free” pro cess to al low more uni form
spreading of test portion in dish.
(b) Calibration weights.—Class S standard calibration weights
to verify balance accuracy within weight ranges for weighing empty
dish and dish plus test portion.
(c) Analytical balance.—Readability to near est 0.0001 g.
Accuracy on verification within 0.0002 g. Check periodically and
whenever balance is moved or cleaned. Keep record of balance
calibration checks. Digital electronic balance is recommended for
fast response time for weighing warm milk.
(d) Water bath.—For tempering milk test samples before
weighing. Test sample temperature should be 38° ± 1°C.
(e) Steam table.—With individual openings that expose full
bottom surface of each test portion dish to steam.
(f) Desiccator.—Room temperature. For cooling weighing dishes
after preliminary drying of empty dishes and after final drying of dish
plus residue. Use coarse desiccant (6–16 mesh) that contains
minimum of fine particles and that changes color when moisture is
absorbed. Desiccator should seal tightly and contain a thermometer.
(g) Tongs.
(h) Forced air oven.—Capable of rapid temperature recovery after
loading and of maintaining 100° ± 1°C. To evaluate temperature
recovery, heat empty oven to 100° ± 1°C and stabilize for 15 min.
Turn oven off and fully open door for 2 min. Close oven door, turn
oven back on, start timing, and record time for oven to reach 99°C.
Time should be £7 min.
C. Determination
(a) Weighing dish preparation.—Number clean weighing dishes
and dry ³2 h in 100° ± 1°C forced air oven. Store dishes in desiccator
until needed (must be used within 1 week or redried).
predried dishes with clean, dry tongs.
(b) Test portion preparation.—Temper milk to 38° ± 1°C and
mix until homogeneous as in 925.21 (see 33.2.02).
(c) Initial weighing.—(Note: Remove and weigh milk at 38° ±
1°C. Record all weights to 4 decimal places.) Remove metal shelf
from oven and place next to balance. Weigh predried weighing dish.
Pipet ca 3 g of 38° ± 1°C prepared milk test portion directly into
preweighed dish. Do not chase drift. Record test portion weight to
nearest 0.1 mg immediately after weight stabilizes and just before
start of steady drift to lower numbers. Remove dish from balance
and place on oven shelf for transport to steam bath. Check balance
zero between weighings.
(d) Blanks.—Weigh 2 empty, predried dishes.
(e) Predrying.—Place dishes on steam bath so that full surface of
dish bottom is exposed to steam. Be sure that all holes in steam bath
contain a dish or are covered during predry period. Expose blank
dishes to steam as for dishes containing test portions. Do not have
steam so high that dishes float or tip over. Predry milk until there is
little or no free liquid movement in dish (£25 min).
(f) Drying.—Preheat oven to 100° ± 1°C. After steam table
predry, place all dishes (including blanks) on oven shelf, turn oven
off, and place shelf plus all dishes into forced air oven. (Note: Do not
place dishes on solid trays; this does not allow heat to circulate
evenly around dishes. Do not place any thing else in oven.)
Immediately after loading all dishes in oven, close door and turn
oven on again, and dry 3 h at 100° ± 1°C. Do not open oven door until
3 h drying is completed.
(g) Cooling.—Remove dishes from oven and cool to room
temperature in desiccator (³30 min). Weigh dish plus dry milk on
same balance that was used for initial weighings.
D. Calculations
Always use blank values in calculation. If mean blank is negative,
be sure to add blank weight instead of subtracting it. Cause of
negative blank weight should be de termined and cor rected.
Negative blank weight is usually caused by pans not being
completely dry before use in analysis.
(W 2 - W ) - B
Total solids, % = ´ 100
W1 - W
where W weight of dish; W1 = weight of dish + milk test portion; W2
= weight of dish + dry milk; and B = mean blank weight.
Maximum recommended difference between duplicates = 0.05%
total solids.
E. Repeatability and Reproducibility
Repeatability (r) and reproducibility (R) values established in the
collaborative study were 0.049 and 0.133, respectively.
Reference: JAOAC 72, 712(1989).
2006 AOAC INTERNATIONAL
ã 2005 AOAC INTERNATIONAL