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4.8.09 AOAC Official Method 975.08 Fluorine in Animal Feed: Distillation Method First Action 1975 Final Action 1976
4.8.09 AOAC Official Method 975.08 Fluorine in Animal Feed: Distillation Method First Action 1975 Final Action 1976
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AOAC Official Method 975.08 bottle. (2) Intermediate solution I.—100 µg/mL. Pipet 20 mL
Fluorine in Animal Feed stock solution into 100 mL volumetric flask, dilute to volume
Distillation Method with H2O, and mix. (3) Intermediate solution II.—10 µg/mL.
First Action 1975 Pipet 2 mL stock solution into 100 mL volumetric flask, dilute to
Final Action 1976 volume with H2O, and mix. (4) Working solutions.—Pipet 3, 5,
Determine as in 944.08, especially E (see 9.2.11). 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,
Ion Selective Electrode Method 1.0, 5.0, and 10 µg/mL F working solutions, respectively. To each
First Action add 10.0 mL 1N HCl, 25.0 mL NaCH3COO⋅3H2O solution, (a),
Final Action
and 25.0 mL sodium citrate solution, (b). Dilute to volume with
H2O and mix.
A. Apparatus
C. Preparation of Sample
(a) Electrodes.—Fluoride ion selective electrode
(Model 94-09 [replaced by 94-09-BN], Orion Research, Inc., or Accurately weigh well-mixed test portion containing ca 400 µg F
equivalent) and single junction calomel reference electrode, plas- into 200 mL volumetric flask. Pipet in 20 mL 1N HCl and stir 20 min
tic sleeve-type (Model 90-01 [replaced by 90-01-00], Orion Re- at high speed on magnetic stirrer. Add 50.0 mL NaCH3COO solu-
search, Inc., or equivalent). tion, C(a), and 50.0 mL sodium citrate solution, C(b), to test solu-
(b) Magnetic stirrer.—With 4 cm (1 12″) Teflon-coated stirring tion. Dilute to volume with H2O and mix.
bar. Use mat to insulate sample from motor heat. D. Determination
(c) pH meter.—Corning digital Model 112 (Corning Scientific Connect F and reference electrodes to pH meter, place electrodes
Instruments, 63 North St, Medfield, MA 02052, or equivalent). in low concentration F solution, and warm up pH meter. Pour
50–70 mL standard and corresponding test solutions into separate
B. Reagents
100 mL beakers. Place electrodes in each solution and while stirring
(Deionized H2O may be used.) with magnetic stirrer at constant rate, read mV of standard and un-
( a ) S o d i u m a c e t a t e s o l u t i o n. — 3 M . D i s s o l v e 4 0 8 g known solutions. Rinse and blot off electrodes and stirring bar be-
NaCH3COO⋅3H2O with H2O in 1 L volumetric flask. When solu- tween solutions. Construct standard curve on 3 cycle
tion warms to room temperature, dilute to volume with H2O. Ad- semilogarithmic paper. Read µg/mL F of sample solution from stan-
just to pH 7.0 with few drops CH3COOH. dard curve.
(b) Sodium citrate solution.—1.32M. Dissolve 222 g sodium
citrate⋅2H2O with ca 250 mL H2O in 1 L volumetric flask. Add F, % =
28 mL HClO4, dilute to volume, and mix. µg/mL F × test solution, mL × 10–6 × 100/test portion, g
( c ) F l u o r i d e s t a n d a r d s o l u t i o n s . — ( 1 ) S t o c k s o l u-
Reference: JAOAC 58, 477(1975).
tion.—500 µg/mL (mg/L). Accurately weigh 1.105 g NaF (re-
agent grade, dried 4 h at 100°C) into 1 L volumetric flask. Dis- CAS-7782-41-4 (fluorine)