AOAC Orson: Meters oF ANBLYSIS (1990) For ferlizer Is ane moist Fertilizer mints grin! xo pass sieve orth Tam cucular openings, or No. 20 sieves for dry sists chat tend w segregate, grind ta pass No. 40 sieve. Grind 8 rapidly a8 posstble 10 avai ass or gain ol moisture dt ‘operation. Mix thoroly andl store sa tightly steppoted hotles. Refs: SADAC 12, 98(1929); 28, 25311941), 917.034 Bone, Tankage, and Basie Slag Fertilizers Mechanical Analysis. Soe 2.008, 11tb ed. 957.01 Phosphate Rock Fertilizers Mechanical Analysis, Final Aetion A. Apparatus (a) Water pressure coasrol —See Tig, 987.01, Connect valve. A, sd pressare gsge, Mf, and aerator, C, with 5" diam, pie. Gb) Sieves.—Nos. 100 and 200, bronze ov stainless steel cloth, cheoked against ceniied sieves, Sieves §° dian. and 2” In depth to sicve eloth ure recommended for both wet and dry but other sizes may be used if dow 9 be sutale un ec conditions of method. (Other sieves i U.S. series ray he ‘used, wit precaution tm ansse complete sepa ef sample into ddssiod Fractions.) () Sieve sHaker —Ro-Vap (C-E Tyler. tae, 3200 Besse- uncr City Ru, Hisy 274, PO Lox 8900, Gastonia, NC-28053) Syoicon (FMC Corp., Material Handling Bquipment Div. Ho. mer City. PA (5748), or ether suitable machine 8. Reagent Dixpersing agent.— Dissolve 36 g Na hexamecsphosphate and 8 g Na,CO, In HO and dil. 40 1 L, “ \ geome FIG. 957.01—Apparatus for control of weter pressure Yooen it 6. Determination {a Ground phosphate rock, Place 100 ¢ snug oa No. 200 sews and sth with radu steam ef tp IFO at man ome resie 10.28 ks em Ut ys) unl #0 passing ee fs lear. th cate to vk ls ot sirple by speching {py materia emnsining on sive at 105" and te fo No 108 stewe i sce with Ne 200 sive ef vam dam, at Sept Shake ® min nraesh. shaker. Dat. sanmle passing No. 100 siowo ty subtracting wt of mari retained on that sive from ADO. Der, sul passing No, 200 sieve by sotrctng stn of ws of material retained on tht steve and on Nos 10 ove from 1 “hy Soft phowhate with cota cay. —Add 100 g sarmpe to apily tire soln of 90 ta, dispersing wet an 50m {up LO. wih care to avoid conta of unseted materia Shut of ser and’ aide of beaker Sir 3 er ac Sarnpe is completed, Tronser sary to No, 200 sive and po ceed asin (0) Ref JAOAC 40, 71 1957), 955.03 Ash (Acic-Insoluble) of Fertilizers: Final Action Surplus 1370 See 2.018, LLth ed, WATER 950.01 ‘Water (Total) in Fertilizers, Final Action (Not applicable to samples that yield vile substances otner ‘thas HO at dying emp.) Hear 2 2 sample, 929.02, 5 hr in oven at 100 1° In ease fof NaNO, ENH)SO,, ant K alls. heat to eonst set at 13021 Report 3 assim wi a6 HO at temp. used. Ret IAQAC 33, 2601950), 965.08 Water (Freo) in Fertilizers ‘Vacuum-Desiecation Methods First Action 1965, Final Aetion 1974 (Caution: See salety ote on magnesium perchlorate.) A. Mothod ! Place 2 g propd sample, 929.02, in tared weighing dish OWeigh extremely hyxeoseopic oe damp materials by uiffer= ence in covered dishes.) Dry sample al 25~30F (preciso results lepemd on ns cms temp, as possible} in wae, esieestoF Over hyd. MgICI0,}s,PyOs, oF Ba, under 250 em 120") or 55 fem (22") vac. (20-25 Cin (@-1G") absolute pressure) 16-18 br, Reweigh, ind report % loss in sits free H B. Method it {Net applicable to samples which yield volute substances ether tan HO) Weigh 2 ¢ prep sample, 929,02, into trad glass weighing sli, Dry saniple 2 Iu 10 min as SD= 15" in even ueuer va fof 48-53 cm 19-21") 23-28 om (9-17) absolute pressure) (Temp. contr within specified Iimite teu! even chamber12 Fesmuzens 4s essential.) Maintain vac. by passing desiccated sir thea ‘chamher. Coo| dried sample m desiceaior and reweigh. Report "lass in C8 foo HO. Refs: JAQAC 46, 382(196%), 47, 32, 1O40(L961}; 48, 98 4965), 972.01 Water (Free) in Fertilizers “Altemative Extraction Method Firet Ation 1972 Final Aetion 1974 A. Bcincip Five H.O fy cxtd with dioyane]and detd by titen wth Karl 1B. Reagents (Keep exposure of org. reagents 10 air at min.) (8) Kart Fischer reagent Stabilized single soln (Fisher Scignaiic Co., So-K-3, er equiv.) ld ea 1+ 1 with stabie Tizod diluent (Fisher, So-K-5, of equiv.y, or soln equty. 10 2.5 yim. Sulze daily with on D.2 g Na tartrate 24,0, 1 fa tare, 2,0 = 0.1566 mg HO. “yy Methanol —Low in HO. . Determination Accurately weigh 2.5 g prepd sample, 929.02, into 125 mb. cerfonmeyer, add 50.0 mb tedlovaue, sapper. wis bs swirk ing, and tos sand 15 min. Mix thoroly by swirling, and cent. in closed mabe. (Caution: See safery note on centalsges.) Transfer 10 mL aliquot to ttm vessel eemtepretited MeOH, and Ur, with Karl Fischer reagent, (Discard contents of citen vessel after 3 ums, replace with enough MeOH to cover elec trades, and pret. belore proceeding with rext sample.) Det bank on 10-mL dioxane sx above aad subtruct from sample ems, Cale. and report as free HO. Refs.: JADAC 52, 112711969), 58, 699(1972). PHOSPHORUS 957.02 Phosphorus (Total) in Fertilizers Preparation of Sample Solution Final Action A. Reagent Magnesium nitrate soln, Dissolve 950 g P-Iree Mg(NO).6HL,0 is 10 and il. 0.1L, .B. Preparation of Solution «Cation: See safety notes. on wet oxidation, sitic acid, poe chloric acid, suturic seid, and oxidizsrs.» Treat 1 g sample by (a), (bp, (6), (@}, oF (e)- as indicated (Cool soln, taster to 200 or 250 mb. vel, Rask, lil Ho vo snke, and filter dhru dey fer. (an) Materials containing smell quantities of organic mat fer =—Dissoive it 30 tal HNO} 28) 3-5 mL ACI, and boil cuntl org. matter is destroyed (0 min for ligs and suspen sions) 4D} Fenilizers comaining mach Fe or Al phosphate. and basic slag +See 2.017, 100 cc. (6) Organic material like cononseed meal alone or in mir- res. —Lvap, with $ mil. Mg(NO,jp sola, 987.024, ignite, and dissolve in HCI AOAG OrFicia, METHODS OF ANAL YSS (1990) (9) Materials or mistnres contcining large smouuus of or anus mattere See 2.0078), 1th ee (e) AM fernizers.— Boil gently 30-48 ain with 20-30 mit HINO, in suitable Mask (greferubly Kjell for saerples conta large arts of ore. matter! to oxidize all easily oxidizable mat ter, Cool. Aud 10-20 ml. 70-724 HCIO,, Bes] very gently Until soln is colorless oF ucatly so and dense white fumes ap ‘pear in ask. Do got boil ty dryness al any time (Danger!). (OWidh samples comp fargs ames of ors. matter, rave ep. 10 fuming point, 62 170", over period of 21 br.) Cool slighty. ‘6d 50 mL. FEO, amd boil fee min Ref.. JAGAC 40, 691957). CAS-7723-14.0 (phasphonss) 958.0 Phosphorus (Total) in Fertilizers Spectrophotometric Molybdovanadophosphate Method Final Action (Not applicable to materials yielding colored solns or soins {ent ions other than orthophosphate which form colored cor plexes with molydovanauste. Not recommended for basic shag.) A. Apparatus Photaneter.»-Spoctrophte with stray hight filter and matched | em cells. Amalyst must det, suitability for usc and conditions for satisfactory performace, Means Tor dispelling heat foun Tighe source is desicable 8. Reagents (a) Molyodovenadate reagent. Dissolve 40) y NH, molyb- dare. H,0 in 400 mL hot HO and cool. Dissoive 2 g NI, ‘metavanadete io 250 mL hot HO, cool, and adé 450 mL 70% HCIO,, (Canion: See safety notes en perchloric acid.) Grad- ily aid molybdate soln to vanadate Solu wath shining, and dil. to 2L. (b) Phosphate std solv. —Dry pure KH,PO, (52.15% P,0,) 2 ar at 108°, Prep. solns erty 0.4—1.0 mg POs frm in 0.1 ime increments bY weighing 0.0767. (0.0959, 0.1151, 0.1342, 0.1534, 0.1726, and 0.1918 g KH.PO, and dily each € 100 ink. With HO. Prep. fresh soins comtg 0.4 and 0.7 sug P.O4/ sm weekly, . Preparation of Standard Curve Pipct § ml. aliquots of 7 std phosphate solns (2S mg P20; / aliquot) into 100 mab vol, Hlasks and add 45 mu, HO, Then, within 5 min for entice series, add 20) mL molybdowanaate reagem by huret or pipet, dil. to vol. end mix. Let stand 10 cet 2 absomption eels (st6 and sample cells) and fill ort ‘vit 2 mg sid, Set speetrophtr to 400 my anchacjust to 2670 A with sil cell. Saenphe cell must check zet0 4 within 0.001 lunt: eshesvise read 4 Tor sample cell and correct subsequent readings, (Chose cell showing pos. A against other as sample ell so that this pos. A is always subrrscted) Using sanple cell, det A of other ss with imstrement adjsted 40 2620 A foo 2 mg std. After each dein empiy and refill cell comy 2 mg Sd, and reads! Zero to avoid errr that night vise Som ten, changes. Plot A against conen in my P.O; fra sid soln D. Preparation ot Solution Treat 1 g sample asin 987,028, preferably (e), when these scidy are suitabic sole. (Soln should be tree of N oxides and Nocti (a) Por P.O, content 5%, dil, co 250 roL.