FERTILIZERS ‘AOAC OFFICIAL METHODS OF ANALYSIS (2012) Chapter 2, p. 10 2.3.40 . Determination (Final Action 1974) AOAC Official Method 963.03 (8) Gravimetric quinolinium molybdophosphate method —Treat Phosphorus (Citrate-Insoluble) 1 g test portion asin B(a) or (b). Transfer aliquot of citate-insoluble in Fertilizers 0, containing <25 mgP,O, and proceedasin 962,02C (see 23.03). First Action 1963 (b) Spectrophotometric molybdovanadophosphate Final Action 1964 ‘method.—Treat 1 g test portion as in B(a) or (b). Adjust concentration of citrate-insoluble PO, solution as in 958,01D(a) or A. Reagents (2) Ammonium citrate solution.—Should have specific gravity of 1.09 at 20°C and pH of 7.0 as determined potentiometrcaly. Dissolve 370 g crystalline citric acid in 1.5 L H,O and neatly neutralize by adding 345 mL NH,OH (28-29% NH;). If concentration of NH, is <28%, add correspondingly larger volume and dissolve citric acid in correspondingly smaller volume H,0. Cool, and check pH. Adjust with NH,OH (1 + 7) or citric acid solution to pH 7. Dilute solution, if necessary, to specific gravity of| 1.09 at 20°C. (Volume will be ea 2 L.) Keepin tightly stoppered bottles and check pH from time to time. I pH has changed from 7.0, readjust (b) Other reagents and solutions. —See 957.024 (see 23.01), 958.018 (see 23.02), oF 962.02A (see 2.3.03) 2. Preparation of Test Solution (a) Acidulated materials, mixed fertilizers, and materials containing water-soluble compounds,—After removing 1,0-soluble P,0,, 97.01 (see 2.3.06), transfer filter and residue, Within 1h, to 200 or 250 mL flask containing 100 mL. ammonium citrate solution previously heated to 65°C, Close flask tightly with smooth rubber stopper, shake vigorously until paper is reduced to Pulp, and relieve pressure by removing stopper momentarily. Continuously agitate stoppered flask in constant temperature Spparatus at exactly 65°C. (Action of apparatus should be such that. lispersion of test sample in citrate solution is continually ‘maintained and entire inner surface of flask and stopper is ‘continually bathed with solution.) Exactly 1 h after adding fiter and residue, remove flask from apparatus and immediately filter by suction as rapidly as possible tough Whatman No. 5 paper, or equivalent, using Bichner or ‘ordinary funnel with PL or other cone. Wash with H,O at 65°C until volume filtrate is ca 350 mL, allowing time for thorough draining before adding more HO. If matetal yields cloudy filtrate, wash with 5% NH\NO, solution (w/s). Prepare citrate-insoluble residue for analysis by one of following methods: (J) Dry paper and contents, transfer to crucible, ignite until all organic matter is estroyed, and digest with 10-15 ml. HCI until all phosphate dissolves; or (2) treat wet filter and contents as in 957.02B(a), (©), (@), oF (€) (see 2.3.01), Dilute solution to 250 mL, of other suitable volume, mix well, and filter through dry paper. [Note: For ammoniated fertilizers, treat wet filter and contents as in 957.02B(a), (d), or (e) (see 2.3.01). Dilute solution to 250 mL, or ‘other suitable volume, mix wel, and filter through dry paper.] (b) Nonacidulated materials.—Place |g test portion (ground to pass No. 40 sieve in case of calcium metaphosphate) on dry 9 em paper, Without previous washing with H,O, proceed as in (a). If Product contains much organic matter (bone, fish, etc), dissolve Fesidu insoluble in ammonium citrate as in 957.02B(), (€), or (€) (s0e 23.01). "AOAC INTERNATIONAL (W) (ee 2.3.02) and proceed as in 958.01E (see 2.3.02) q (€) Alkalimetric quinolinium molybdophosphate ‘method—Treat | g test portion by (a) or (b). Transfer aliquot of ue citrate-insoluble P;0, containing <5 mL concentrated acid to fe ‘500 mL Erlenmeyer. Add 20 mi 10% citi acid solution (wiv) and dilute t 100 mL with H,O. Continue asin 969.02C(a) (see 2.3.04), beginning “Add 60 mL quimociac reagent, References: JAOAC 5, 443, 460(1922y; 6, 384(1923); 14, 182(1931); 19, 269(1936); 22, 254(1939), 42, 503, $12(1959); 48, 40, 201, 999(1962);, 46, 579(1963); 47, 420(1964); 82, $87(1969). Z Anal. Chem. 189, 243(1962) CAS-1314-56-3 (phosphorus pentoxide) 23.11 (Note: This method will give recovery of phosphite source ‘materials as available phosphorus, even though the Association of American Plant Food Control Officials does not recognize phosphite asa source of available phosphorus.) Subtract sum of H,0-soluble and citrate-insoluble P,O, ftom total P,0, to obtain citrate-soluble P,O Revised: March 2002 ; 23.42 AOAC Official Method 960.02 Phosphorus (Available) in Fertilizers Indirect Method First Action 1960 i Final Action 1960 Subtract citrate-insoluble P,O, from total P,O, to obtain available P05 2.3.13 AOAC Official Method 960.03 Phosphorus (Available) in Fertilizers First Action 1960 Final Action 1964 A. Reagents Caution: See Appendix B, safety notes on perchloric acid (8) Nitric-perchloric acid mixture —Add300 mL 70% HCIO,t0 700 mL. HNO, (b) Ternary acid mixture. Add 20 mL-H,80, 0 100 mL HNOs, ‘mix, and add 40 mL. 70% HCI0,