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2.3.02 AOAC of Fi Cial Method 958.01 Phos Pho Rus (To Tal) in Fer Til Izers

This document describes a spectrophotometric method for determining total phosphorus in fertilizers. It involves: 1) Preparing standard solutions of potassium dihydrogen phosphate at concentrations of 0.4-1.0 mg P2O5/mL. 2) Developing a standard curve by mixing aliquots of the standards with molybdovanadate reagent and measuring absorbance. 3) Treating fertilizer samples to prepare test solutions, then measuring their absorbance against the standard curve to determine phosphorus content. The content is calculated based on the sample amount used.

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330 views1 page

2.3.02 AOAC of Fi Cial Method 958.01 Phos Pho Rus (To Tal) in Fer Til Izers

This document describes a spectrophotometric method for determining total phosphorus in fertilizers. It involves: 1) Preparing standard solutions of potassium dihydrogen phosphate at concentrations of 0.4-1.0 mg P2O5/mL. 2) Developing a standard curve by mixing aliquots of the standards with molybdovanadate reagent and measuring absorbance. 3) Treating fertilizer samples to prepare test solutions, then measuring their absorbance against the standard curve to determine phosphorus content. The content is calculated based on the sample amount used.

Uploaded by

estefania
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© © All Rights Reserved
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2.3.02 changes.

Plot A against concentration in mg P2O5/mL standard


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

 2005 AOAC INTERNATIONAL

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