FERTILIZERS Chapter 2, p.6 ‘AOAC OFFICIAL METHODS OF ANALYSIS (2012) (©) Allfertlizers-—Boil getly 30-45 min with 20-30 mL HNO, in suitable flask (preferably Kjeldahl test for products containing large amounts of organic matter) to oxidize all easily oxidizable ‘matter, Cool. Add 10-20 mL 70-72% HCIO,. Boil very gently until solution is colorless or nearly so and dense white fumes appear in Mask. Do nor boil 1 dryness at any time. (With produets containing large amounts of organic matte, raise temperature to fuming point, 4 170°C, over period of 21 h.) Cool slightly, add 50 mL H,0, and boil few minutes, Reference: AOAC 40, 691957), (CAS-7723-14-0 (phosphorus) 2.3.02 Notapplicable to materials yielding colored solutions or solutions ‘containing ions other than orthophosphate which form colored complexes with molybdovanadate. Notrecommended for basic slag) A. Apparatus Photometer—Spectvophotometer with 1 cm cells, Analyst must detemine suitability for use and conditions for satis ictory perfomance, 8B. Reagents (a) Molybdovanadare reagent.—Dissolve 40 g ammonium molybdate-4H1,0 in 400 mL. hot water and cool. Dissolve 2 g ammonium metavanadate in 250 mL hot water, cool, and add 450 mL 70% HCI0,. (Caution: See Appendix B, safety notes on perchloric acid.) Gradually add molybdate solution to vanadate ‘olution with siting, and dilute to 2 L. (b) Phosphate standard solution.—Dry pure KH,PO, (52.15% P.O.) 2 hat 105°C. Prepare solutions containing 0.4-.0 mg P,OymL in 0.1 mg increments by weighing 0.0767, 0.0959, 0.1151, 0.1342, 0.1534, 0.1726, and 0.1918 g KH,PO, and diluting each to 100 mL. with H,0. Prepare fresh solutions containing 0.4 and 0.7 mg, P,O/mL weekly . Preparation of Standard Curve Pipet Sm. aliquots of the 7 standard phosphate solutions (2-5 mg P,O,aliquot) into 100 mL. volumetic flasks and add 45 mL. H,O. ‘hea, within 5 min for entite series, add 20 ml. molybdovanadate reagent by buretor pipet, ilut(o volume and mix. Letstand 10 min Select2 absorption cells (standard and test solution cells) and fill both with 2 mg standard, Set spectrophotometer to 400 nm and ‘adjust to zero 4 with standard cell. Test solution cell must check zero 4 within 0.001 unit; otherwise read 4 for test solution cell and comet subsequent readings. (Choose cell showing positive ‘against other as test solution cell so that this positive 4 is always subiracted.) Using test solution cell, determine 4 of other standards With instrument adjusted to zero 4 for 2 mg standard. After each etcrmination empty and refill cell containing 2 mg standard, and ‘eadjyst zero to avoid error that might arise from temperature ‘changes. Plot A against concentration in mg P,OJmL. standard solution. G52 AOAC INTERNATIONAL . Proparation of Test Solution ‘Treat Ig test sample as in E, preferably (b), when these acids are suitable solvents. (Solution should be free of nitrogen oxides and Nocl) (a) For P,0, content <5%, dilute to 250 mL. (b) For P;0, content >5% dilute to such volume that Sor 10 aL. aliquot contains 2-5 mg P,0,, . Dotormination Pipet, into 100 mL volumetric flasks, $ mL aliquots of standard Phosphate solutions containing 2 and 3.5 mg P,O,/aliquot, respectively and develop color as in C. Adjust instrument to zero A for 2 mg standard, and determine A of 3.5 mg standard, (It is ‘essential that 4 of latter standard be practically identical with corresponding value on standard curve.) (a) Materials containing up to 5% P50,.—Pipet, into 100 mL. volumetric flask, 5 mL test solution, D(a), and 5 mL standard phosphate solution containing 2 mg P,O,. Develop color and determine A concurrently with and in same manner as for standard phosphate solutions in preceding paragraph, with instrument adjusted to zero 4 for 2 mg standard, Read P,O, ‘concentration from standard curve. With series of test solutions, empty and refill cell containing 2 mg standard after each determination Percent POs in test sample = 100 x {(mg P.O, from standard curve ~ 2920] (b) Materials containing more than 5% P;0,—Pipet Sor 10 mL {est solution, D(b), into 100 ml. volumetric flask. Without adding standard phosphate solution, proceed asin (a). Percent PO, in test sample = 100 x (mg PO, ftom standard curvelmg test portion in aliquot) References: JAOAC 41, 517(1958); 42, 03(1959); 44, 133(1961),. CAS-1314-56-3 (phosphorus pentoxide) 2.3.03 AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinotinium Molybdophosphate Method First Action 1962 Final Action 1965 A. Reagents (Store solutions in polyethylene bottles.) (a) (Citric-molybdic acid reagent.—Dissolve 54 g 100% ‘molybaic anhydride (MoO,) and 12 g NaOH with stirring in 400 mL hhot water, and cool. Dissolve 60 g citric acid in mixture of 140 mL. HCl.and 200 mL H,0, 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) Tfnecessary, add 0.5% KBrO, solution dropwise until green color pales. Store in dark (b) Quinoline solution.—Dissolve $0 ml. synthetic quinoline, ‘with stirring, in mixture of 60 mL HC1 and 300 mLH,0. Cool, dilute to L, and filter,