2.3.02
Plot A against
AOAC Official Method 958.01
Phosphorus (Total) in Fertilizers
Spectrophotometric Molybdovanadophosphate Method
First Action 1958
Final Action
(Not applicable to materials yielding colored solutions or solutions
containing ions other than orthophosphate which form colored com-
plexes with molybdovanadate. Not recommended for basic slag.)
A. Apparatus
Photometer.— Spectrophotometer with 1 cm cells. Analyst must de-
termine suitability for use and conditions for satisfactory performance.
B. Reagents
(a) Molybdovanadate reagent.—Dissolve 40 g ammonium
molybdate⋅4H2O in 400 mL hot H2O and cool. Dissolve 2 g ammo-
nium metavanadate in 250 mL hot H2O, cool, and add 450 mL 70%
HClO4. (Caution: See Appendix B, safety notes on perchloric acid.)
Gradually add molybdate solution to vanadate solution with stirring,
and dilute to 2 L.
(b) Phosphate standard solution.—Dry pure KH2PO4 (52.15%
P2O5) 2 h at 105°C. Prepare solutions containing 0.4–1.0 mg
P2O5/mL in 0.1 mg increments by weighing 0.0767, 0.0959, 0.1151,
0.1342, 0.1534, 0.1726, and 0.1918 g KH2PO4 and diluting each to
100 mL with H2O. Prepare fresh solutions containing 0.4 and 0.7 mg
P2O5/mL weekly.
C. Preparation of Standard Curve
Pipet 5 mL aliquots of 7 standard phosphate solutions (2–5 mg
P2O5/aliquot) into 100 mL volumetric flasks and add 45 mL H2O.
Then, within 5 min for entire series, add 20 mL molybdovanadate re-
agent by buret or pipet, dilute to volume and mix. Let stand 10 min.
Select 2 absorption cells (standard and test solution cells) and fill
both with 2 mg standard. Set spectrophotometer to 400 nm and ad-
just to zero A with standard cell. Test solution cell must check zero A
within 0.001 unit; otherwise read A for test solution cell and correct
subsequent readings. (Choose cell showing positive A against other
as test solution cell so that this positive A is always subtracted.)
Using test solution cell, determine A of other standards with instru-
ment adjusted to zero A for 2 mg standard. After each determination
empty and refill cell containing 2 mg standard, and readjust zero to
avoid error that might arise from temperature changes.
concentration in mg P2O5/mL standard solution.
D. Preparation of Test Solution
Treat 1 g test sample as in E, preferably (b), when these acids are
suitable solvents. (Solution should be free of nitrogen oxides and
NOCl.)
(a) For P2O5 content ≤5%, dilute to 250 mL.
(b) For P2O5 content >5%, dilute to such volume that 5 or 10 mL
aliquot contains 2–5 mg P2O5.
E. Determination
Pipet, into 100 mL volumetric flasks, 5 mL aliquots of standard
phosphate solutions containing 2 and 3.5 mg P2O5/aliquot, respec-
tively, and develop color as in 958.01C. Adjust instrument to zero A
for 2 mg standard, and determine A of 3.5 mg standard. (It is essential
that A of latter standard be practically identical with corresponding
value on standard curve.)
(a) Test Samples containing up to 5% P2O5.—Pipet, into
100 mL volumetric flask, 5 mL test solution, 958.01D(a), and
5 mL standard phosphate solution containing 2 mg P 2O5. De-
velop color and determine A concurrently with and in same man-
ner as for standard phosphate solutions in preceding paragraph,
with instrument adjusted to zero A for 2 mg standard. Read P 2O5
concentration from standard curve. With series of test solutions,
empty and refill cell containing 2 mg standard after each
determination.
Percent P2O5 in test sample = 100
× [(mg P2O5 from standard curve – 2)/20]
(b) Test Samples containing more than 5% P2O5.—Pipet 5 or
10 mL test solution, 958.01D(b), into 100 mL volumetric flask.
Without adding standard phosphate solution, proceed as in (a).
Percent P2O5 in test sample = 100
× (mg P2O5 from standard curve/mg test sample in aliquot)
References: JAOAC 41, 517(1958); 42, 503(1959);
44, 133(1961).
CAS-1314-56-3 (phosphorus pentoxide)
© 2000 AOAC INTERNATIONAL