44.5.
14
AOAC Official Method 964.21
Formaldehyde in Maple Syrup
Spectrophotometric Method
First Action 1964
Final Action 1965
(Not suitable for beet or cane sugars.)
A. Apparatus
(a) Distillation apparatus.—30 mL micro Kjeldahl flask, with
standard taper 19/38 joint and 10 cm H2O-cooled West condenser
with standard taper 19/38 inner joint bent at 90° angle. Insulate
condenser from standard taper joint to condenser H2O jacket. In-
stall adjustable flask heater equipped with conical porcelain coil el-
ement and hand-controllable rheostat placed on underside (Cenco,
Inc., 2600 Kostner Ave, Chicago, IL 60623, USA, No. 16530-1, or
equivalent).
(b) Spectrophotometer.—Suitable for measuring A at 415 nm;
with matched 1 cm cells or matched test tubes. Figure 964.21—Distillation apparatus for determining
B. Reagents formaldehyde in maple syrup.
(a) Nash’s Reagent “B”.—Dissolve 150 g NH4CH3COO, 3 mL
CH3COOH, and 2 mL acetylacetone in 200–300 mL H2O in 1 L flask
and dilute to volume. ure 964.21. Heat flask with heater, previously adjusted with control
(b) Formaldehyde.—Approximately 37% by weight. Assay by knob in such position that exactly 3 mL H2O is distilled from syrup
898.01B (see 7.8.04). in 12–14 min. Collect 3 mL distillate in 5 mL graduate with funnel
top. Using transfer pipets, place 1 mL distillate in 13 mm id test tube,
C. Preparation of Standard Solutions and add 1 mL H2O and 2 mL Nash’s reagent. Heat 30 min in H2O
(a) Stock solution.—1000 µg/g. Weigh 5.35 g 37.4% CH2O solu- bath at 37 ± 1°C to develop color. Transfer colored solution to 1 cm
tion (for other concentrates, g CH2O solution required = 200/% cell and measure A at 415 nm against H2O.
CH2O) into 2 L volumetric flask containing H2O and dilute to vol-
E. Blanks
ume with H2O.
To determine A due to reagents, substitute 1 mL H2O (from same
(b) Solution B.—50 µg/g . Pipet 10 mL stock solution into
source as used in determination) for 1 mL test distillate. Subtract A
200 mL volumetric flask and dilute to volume with H2O.
of blank from that for sample to obtain A due to CH2O. Or, as simpler
(c) Solution C.—100 µg/g. Pipet 10 mL stock solution into
operation, measure A of distillate with instrument adjusted to 0 A for
100 mL volumetric flask and dilute to volume with H2O.
blank.
(d) Solution D.—200 µg/g. Pipet 10 mL stock solution into Obtain concentration of CH2O in syrup from A, using standard
50 mL volumetric flask and dilute to volume with H2O. curve.
(e) Formaldehyde standard solutions.—Prepare 1, 2, and 4 µg/g
standard solutions by pipetting 10 mL Solutions B, C, and D, respec- F. Preparation of Standard Curve
tively, into 500 g syrup and stirring mechanically 15 min. Construct standard curve by plotting A obtained for syrups con-
taining 1, 2, and 4 ppm CH2O against concentration of added CH2O
D. Determination
in ppm.
Weigh 20 ± 0.20 g syrup into tared 30 mL micro Kjeldahl flask Straight line relationship is obtained for standard curve. Project
and insulate flask neck with asbestos cord as in A(a) from base of this line to Y axis (A); Y intercept indicates blank for syrup. Since
standard taper joint down to body of flask. (This insulation is tempo- syrup used to construct curve from A values may be atypical, draw
rary; repeat after each washing and weighing.) Add 2 drops antifoam and use parallel curve with 0 intercept. Correct ppm values obtained
agent, and connect West condenser. Mount apparatus, adjusting from this curve for average syrup blank (ca 0.9 ppm).
slope of condenser at 45° angle, with flask bottom centered in coni-
References: JAOAC 47, 548(1964); 56, 132(1973).
cal cavity and at such height that syrup level in flask is even with top
plate of heater, without touching hot element at any point; see Fig- CAS-50-00-0 (formaldehyde)
© 2000 AOAC INTERNATIONAL
