4.8.09
AOAC Official Method 975.08
Fluorine in Animal Feed
Distillation Method
First Action 1975
Final Action 1976
Determine as in 944.08, especially E (see 9.2.11).
Ion Selective Electrode Method
First Action
Final Action
A. Apparatus
( a ) E l e c t ro d e s . — F l u o r i d e i o n s e l e c t i v e e l e c t r o d e
(Model 94-09 [replaced by 94-09-BN], Orion Research, Inc., or
equivalent) and single junction calomel reference electrode,
plastic sleeve-type (Model 90-01 [replaced by 90-01-00], Orion
Research, Inc., or equivalent).
(b) Mag netic stir rer.—With 4 cm (1 12 in.) Tef lon-coated
stirring bar. Use mat to insulate sample from motor heat.
(c) pH meter.—Corning digital Model 112 (Corning Scientific
In stru ments, 63 North St, Medfield, MA 02052, USA, or
equivalent).
B. Reagents
(Deionized water may be used.)
(a) So dium ac e tate so lu tion.—3M. Dis solve 408 g
NaCH3COO×3H2O with H2O in 1 L volumetric flask. When
solution warms to room temperature, di lute to vol ume with H2O.
Adjust to pH 7.0 with few drops CH3COOH.
(b) Sodium citrate solution.—1.32M. Dissolve 222 g sodium
citrate×2H2O with ca 250 mL H2O in 1 L volumetric flask. Add
28 mL HClO4, dilute to vol ume, and mix.
( c ) Fluoride standard solutions. —(1) Stock
solution.—500 mg/mL (mg/L). Accurately weigh 1.105 g NaF
(reagent grade, dried 4 h at 100°C) into 1 L volumetric flask.
Dissolve and dilute to volume with H2O, and mix. Store in plastic
bottle. (2) Intermediate solution I.—100 mg/mL. Pipet 20 mL stock
solution into 100 mL volumetric flask, dilute to volume with H2O,
and mix. (3) Intermediate solution II.—10 mg/mL. Pipet 2 mL
stock solution into 100 mL volumetric flask, dilute to volume with
H2O, and mix. (4) Working solutions.—Pipet 3, 5, and 10 mL
intermediate solution II and 5 and 10 mL intermediate solution I
into five 100 mL volumetric flasks to prepare 0.3, 0.5, 1.0, 5.0, and
10 mg/mL F working solutions, respectively. To each add 10.0 mL
1N HCl, 25.0 mL NaCH3COO×3H2O solution, (a), and 25.0 mL
sodium citrate solution, (b). Dilute to volume with H2O and mix.
C. Prepa ration of Sample
Accurately weigh well-mixed test portion containing ca 400 mg F
into 200 mL volumetric flask. Pipet in 20 mL 1N HCl and stir 20 min
at high speed on magnetic stirrer. Add 50.0 mL NaCH3COO
solution, C(a), and 50.0 mL sodium citrate solution, C(b), to test
solution. Dilute to volume with H2O and mix.
D. Determination
Connect F and reference electrodes to pH meter, place electrodes in
low concentration F solution, and warm up pH meter. Pour 50–70 mL
standard and corresponding test solutions into separate 100 mL
beakers. Place electrodes in each solution and while stirring with
magnetic stirrer at constant rate, read mV of standard and unknown
solutions. Rinse and blot off electrodes and stirring bar between
solutions. Construct standard curve on 3 cycle semilogarithmic paper.
Read mg/mL F of test solution from standard curve.
F, % = mg/mL F ´ test solution, mL ´ 10–6 ´ 100/test portion, g
Reference: JAOAC 58, 477(1975).
CAS-7782-41-4 (fluorine)
ã 2005 AOAC INTERNATIONAL