AOAC OFF|ctAL METHODS oF ANALySts (2005) FERTILIZERS

Chapter 2, p. 5

Reduce gross )aboratory sample to amount sufficient for analysis References: JA OA C 12, 9 8(\929); 24, 253 (19 4 l) ;
or grind >225 g (0 5 lb) of reduced laboratory sample without 52, t 121 (r 9 69); 5s, 699 (197 2).
previous sieving. For fertilizer materials and moist fertilizer
mixtures, grind to pass sieve with I mm circular openings, or No. 20
sieve: for dry mixtures that tend to segregate, grind to pass No. 40
sieve Grind as rapidly as possible to avoid loss or gain of moisture Subchapter 3

during operation Mix thoroughly and store in tightly stoppered PHOSPHORUS

bottl es
\r,'eigh 2 g test portion into tared glass weighing dish. Dry 2 h + 2.3.01
I0 rnin at 50" + I .5'C in oven undervacuum of48-53 cm (19-21 in.) AOAC Official Method 957.02
(23-28 cm [9-11 in.] absolute presnre). (Temperature control Phosphorus (Total) in Fertilizers
within specified limits throughout oven chamber is essential.) Preparation of Test Solution
N{aintain vacuum by passing desic.cated air through chamber. Cool First Action 1957
dried test sample in desiccator and rew-eigh. Report percent loss in Final Action
u,eight as free HrO.
A. Reagent
Re ferenc es : JA O A C 12, 9 8(l 9 29): 24, 253 (1 9 4 t); Magnesium nitrate solution 950 g P-free
4 6. s 82 (r9 63) ; 47, 32, 1040(19 64) : 48, 9 8( 1 9 6s). Mg(NO3)2.6HrO in HrO and dilute to I L.
-Dissolve
B. Preparation of Solution
(Caution: See Appendix B, safety notes on perchloric acid.)
Treat 1 g testportion by (a), (b), (c), (d), or (e), as indicated. Cooi
2.2.03
AOAC Official Method 972.01 solution, transfer to 200 or 250 tortl- volumetric flask, dilute to
Water (Free) in Fertilizers volume, mix, and filter through dry filter.
(a) Materials containing small quantities of organic
Alternative Extraction Hethod
First Action 1972
matter-Dissolve in 30 mL HNO3 and 3-5 mL HCl, and boii until
Final Action 1974 organic matter is destroyed (30 min for liquids and suspensions).
(b) Fertilizers containing much Fe or Al phosphate, and basic
A. Principle slag.-See 2.017, loth Ed.
Free H.O is ext-acted u.ith dioxaae and detenrrined by titration (c) Organic material like cottonseed meal alone or in
qiti Karl FGcber reagent- mixtures.-Etaporate with 5 mL Mg$1O,)2 solution, A, ignite, and
dissolve in HCl.
8. Reagents
(d) Materials or nixture,s conlaining large amounts o_[ otganic
(Ke+ erposure of or$anic reas€nrs to air at minimurn.) matter-See 2.017(d), 11th Ed.
(e) Kari Fischer reagenr.-stzbillzed silgle solution (Fisher (e) A I Ifer ti I iz ers oil gently 3 0-45 min with 2 0-3 0 mL HNO,
Scienn-fic Co . SK--l. or equivalent) dilued ca 1 + i with stabilized -B
in suitable flask (preferably Kjeldahl test for products containing
diluent lFisher, SK5, or equiralent). orsolution equivalent to 2.5 mg large amounts of organic rnatter) to oxidize ali easily oxidizabie
H.O'mI . Standardrze daily *.itb ca 02 g 56dium tart-ate.2HrO. matter. Cool. Add70-20mL70-'12oAHCirO4. Boil very gently until
i mg sodium tartrate-2H,O :0.1566 mg HzO. solution is colorless or nearly so and dense white fumes appear in
(h) -l[e thanol.-Lon' i.o H,O. flask. Do not boil lo dryness at any time. (With products containing
large amounts of organic matter, raise temperature to fuming point,
C. Determination
ca 770"C, over period of >1 h.) Cool slightly, add 50 inl- HrO, anC
Reduce gross laborator;' sample to mount sufficient for analysis
boil few minutes.
or grind >J25 g (0.5 lb) of reduced laboratory sample u'ithout
prerious sieving. For fertilizer materials and moist fertilizer Reference: JAOAC 40, 690(1957).
mirtures. grind to pass sieve with I mm circular openings, orNo. 20 C AS -7 7 23 - | 4-0 (phosphorus)
siese: for dq'mixt',res that tend to segregate, grind to pass No. 40
sieve- Grild as rapidly as possible to avoid loss or gain of moisture
2.3.02
durl'rg operation- Mix thoroughly
-d store in tightly stoppered AOAC Official Method 958.01
bonles. Phosphorus (Total) in Fertilizers
Accnrately weigh 2.5 g test portion imo 125 mL Erlenm eyet, add Spectrophotometric Molybdovanadophosphate Method
50.0 mI 1,4{ioxane, stopper, mix by srirling, and let stand l5 min. First Action 1958
14ft ft6serrghly by swirling, and cenuifirge in closed tube. Final Action
Trar:sfer I 0 rnl- aliquot to tit-ation vessel pontaining pretitrated (Not applicabie to materials yielding colored solutions or solutions
methenol and titrate with Karl Fisher reagent. @iscard contents of containing ions other than orthophosphate which form colored
tiuation vessel after 3 tirations, replace with enough methanol to complexes with molybdovanadate. Not recommended for basic slag.)
cover electrodes, and pretit-ate before proceeding with next test.) A. Apparatus
Determine blank on l0 mL dioxane as above and subtract from test I
Photometer--Spectophotometer with crn cells. Analyst must
sample titrations. Calculate and report as free H2O. deterrnine suitability for use and conditions for satisfbctory perforrrance.

O 2OO5 AOAC INTERNATIONAL

 FERTILIZERS
Chapter 2, p. 6
B. Reagents
(a) Molybdovanadate reagent.-Dissolve 40 g ammonium
molybdate.4H2O in 400 mL hot water and cool. Dissolve 2 g
ammonium metavanadate in 250 mL hot water, cool, and add
450 mL 70o/o HC!O4. (Caution: See Appendix,R, 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 KHTPO, (52.15%
P,O) 2 h at 105"C. Prepare solutions containing 0.4-1.0 mg
P,Or/mL in 0. I mg increments by wei ghin g 0.07 67, 0.0959, 0. I I 5 1,
0.1342,0.1534, 0.1726, and 0. l9l8 g KHTPO. and diluting each to
100 mI rvith H,O. Prepare fiesh solutions containing 0.4 and 0.7 mg
PrOriml rveekly.
C. Preparation of Standard Cunre
Pipet 5 mL aliquots of the 7 standardphosphate solutions (2-5 mg
P,Oy'aliquot) into 100 mL volumetric flasks and add 45 mT H,O.
Then, within 5 min for entir'e series, add 20 nI- molybdovanadate
reagent by buret orpipet, dilute to volume andmix. Letstand l0 min.
Seiect 2 absorption cells (standard and test solution cells) and hll
both .uith 2 mg standard. Set spechophotometer to 400 nm and
adjust to zero ;{ with standard cell. Test solution cell must check zero
,{ within 0001 rrnit; othenvise read A for test solution cell and
correct subsequent readings. (Choose cell showing positive I
against other as test solution cell so that this positive I is always
subtracted.) Using test solution cell, determine,1 of other standards
rvrth inslrument adjusted to zero A for 2 mg standard. After each
Cetermination empty and retill cell containing 2 mg standard, and
readjust zero to avojd error that might arise fiom temperahlre
changes. PIot z1 against concenration in mg PrOr/mL standard
solution.
D. Preparation of Test Solution
Treat I g test sample :s in E, preferably (b), when these acids are
suitable solvenls. (Solution should be free of nitrogen oxides and
NOCI.)
(a) For P,O, content <-5%, dilute to 250 mL.
(b) For PrO, conteni >5%, dilute to such volume that 5 or l0 mL
aliquot contains 2-5 mg P,O,5
E. Determinatian
Pipet, into 100 mL volumetric flasks, 5 mL aliquots of standard
phosphale solutions containing 2 and 3.5 mg PrOr/aliquot,
respectively, and develop color as in C. Adjust instrument to zerol
for 2 mg standard, and detennine A of 3 5 mg standard. (It is
essential that ,4 of latter standard be practically identical with
corresponding value on standard curve )
(a) ilIaterials containing up to 59'o PrOr.-Pipe| into 100 mL
volumetric tlask, j mL test solution, D(a), and 5 mL standard
phosphate solution containing 2 mg PrOr. Develop coior and
determine z1 conc:rrrentiy with and in same manner as for
standarul phosphat: solntions in preceding paragraph, with
instLumenr adjusteri t,i zero A "'or 2 mg standard. Read PrO,
concentration liom starrCard curve . With series of test solutions,
empty and refill cell corrtaining 2 mg standard after each
de teruL ina lio n
Pcrcent P.(), in test sample - w ith five 25 mL portions of HrO. Dry crucible and contents 30 min
100 x [(mg PrO, fiom standard curve 2)lZ0)
ci )oos AoAc tNTERN;riol'rnr
AOAC OFF|C|AL METHODS OF ANALYS|S (2005)
(b) Materials containing morc than 5o4 p rOr.-pipet 5 or l0 mL
test solution, D(b), into 100 mL volumetic flask. Without adding
standard phosphate solution, proced as in (a).
Peicent P2O5 in test sample :
100 x (mg PrO, from standard curvdmg test portion in aliquot)
References: JAOAC 4f, 517(1958):,12, 503(1959);
44,133(1961).
CAS- l3 l4-55-3 (phosphorus pentoxide)
2.3.03
AOAC Officiat Method 962.02
Phosphorus (Total) in Fertilizers
Gravimetric Quinofi nium Molybdophosphate Method
First Action 1 962
Final Action i965
A. Reagents
(Store solutions in polyethylene botrles.)
(a) Citric-molybdic acid reagent.-Dissolve 54 g l0O%
molybdic anhydride (MoOr) and 12 g NaOH with stirring in .100 mL
hot water, and cool. Dissotve 60 g ciric acid in mixture of 140 mT
HCI and 200 mL HrO, and cool_ Gradually add molybdic solution to
citric acid solurion with stiring. Coof filter, and dilute to I L.
(Solution may be greeo orblue: color deepens on exposure to light.)
If necessary add0.5Yo KBrO, solution dropwise unril _oeen color
pales. Store in dark.
(b) Quinoline soluion--Dissolve 50 mL synthetic quinoline,
with stirring, in mixture of 60 mI HCI and 300 mI H,O. Cool, ditute
to 1 L, and filter.
(c) Quimociac reagent.-Dissolve 70 g sodium
molyMate-2HrO in 150 mT H2O. Dissolve 60 g citric acid in
mixture of 85 ml HNO, aad I 50 ml H2O, and cool. Gradually add
molybdate solution to citric acid-HNO, mixture with stirring.
Dissolve 5 mL synthetic quinoline in nixture of 35 rnl fl}{e, a1d
100 mL HrO. Gradually add this solution to molyMate__citric
acid-HNO, solution, mix. and let stand 24 h. Filter, add 290 mr
acetone, dilute to I L w:-th H.O, and mix.
B. Preparation of Test Solution
Treat I g test sample as in 957.028 (see 2.3.01), diluting to
200 mL.
C. Determination
Pipet, into 500 mL Erlenmeyer, aliquot containir g 9.5 mgprO5
and dilute to ca 100 ml with HrO. Contirue 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 l0 mI quinoline solution
from buret with continuous swirling. (Add flrrst 3-4 mL dropwise
and remainder in steady stream.) Or:
(b) Add 50 mL qtrimociac reagent, cover with watch glass, place
on hot plate in well ventilated hood, and boil I min.
After treatment by (a) or (b), cool to room temperature, swirl
carefully 3-4 times during cooling, filter into Gooch with glass fiber
filter paper previously dried at 250"C and w.eighed, and wash
at 250"C, cool in desiccator to room temperature, and weigh as
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