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2.3.03 AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers

This document outlines a gravimetric method for determining total phosphorus in fertilizers. It describes reagents, sample preparation, and determination steps involving precipitation, filtration, drying, and weighing of a quinolinium molybdophosphate complex to calculate the percentage of phosphorus pentoxide or phosphorus in the sample.

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1K views1 page

2.3.03 AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers

This document outlines a gravimetric method for determining total phosphorus in fertilizers. It describes reagents, sample preparation, and determination steps involving precipitation, filtration, drying, and weighing of a quinolinium molybdophosphate complex to calculate the percentage of phosphorus pentoxide or phosphorus in the sample.

Uploaded by

Jose Garcia
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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2.3.

03
AOAC Official Method 962.02
Phosphorus (Total) in Fertilizers
Gravimetric Quinolinium Molybdophosphate Method
First Action 1962
Final Action 1965

A. Reagents

(Store solutions in polyethylene bottles.)


(a) Citric-molybdic acid reagent.Dissolve 54 g 100%
molybdic anhydride (MoO3) and 12 g NaOH with stirring in 400 mL
hot H2O, and cool. Dissolve 60 g citric acid in mixture of 140 mL
HCl and 200 mL H2O, and cool. Gradually add molybdic solution
to citric acid solution with stirring. Cool, filter, and dilute to 1 L.
(Solution may be green or blue; color deepens on exposure to light.)
If necessary, add 0.5% KBrO3 solution dropwise until green color
pales. Store in dark.
(b) Quinoline solution.Dissolve 50 mL synthetic quinoline,
with stirring, in mixture of 60 mL HCl and 300 mL H2O. Cool, dilute
to 1 L, and filter.
(c) Quimociac reagent.Dissolve 70 g sodium molybdate
2H2O in 150 mL H2O. Dissolve 60 g citric acid in mixture of 85 mL
HNO3 and 150 mL H2O, and cool. Gradually add molybdate solution
to citric acid-HNO3 mixture with stirring. Dissolve 5 mL synthetic
quinoline in mixture of 35 mL HNO3 and 100 mL H2O. Gradually
add this solution to molybdate-citric acid-HNO3 solution, mix, and
let stand 24 h. Filter, add 280 mL acetone, dilute to 1 L with H2O,
and mix.
B. Preparation of Solution

Treat 1 g sample as in 957.02B (see 2.3.01), diluting to 200 mL.


C. Determination

Pipet, into 500 mL Erlenmeyer, aliquot containing 25 mg P2O5


and dilute to ca 100 mL with H2O. Continue by one of the following
methods:
(a) Add 30 mL citric-molybdic acid reagent and boil gently 3
min. (Solution must be precipitate-free at this time.) Remove from
heat and swirl carefully. Immediately add 10 mL quinoline solution
from buret with continuous swirling. (Add first 34 mL dropwise
and remainder in steady stream.) Or:
(b) Add 50 mL quimociac reagent, cover with watch glass, place
on hot plate in well-ventilated hood, and boil 1 min.
After treatment by (a) or (b), cool to room temperature, swirl
carefully 34 times during cooling, filter into Gooch with glass fiber
filter paper previously dried at 250 and weighed, and wash with
five 25 mL portions of H2O. Dry crucible and contents 30 min at
250, cool in desiccator to room temperature, and weigh as
(C9H7N)3H3[PO4 12MoO3]. Subtract weight reagent blank. Multiply by 0.03207 to obtain weight P2O5 (or by 0.01400 for P). Report
as % P2O5 (or % P).
References: Z. Anal. Chem. 189, 243(1962). JAOAC 45, 40,
999(1962); 46, 579(1963); 47, 420(1964).
CAS-7723-14-0 (phosphorus)
CAS-1314-56-3 (phosphorus pentoxide)

Copyright 1998 AOAC INTERNATIONAL

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