CEREAL FOODS: Chapter 32, p.20 CAS-94-36-0 (benzoyl peroxide) 32.4.32 AOAC Official Method 956,03 _ Bromates aid lodates in White and Whole Wheat Flour First Action 1958 Final Action | ‘A. Qualitative Test for Bromates and lodates Cover bottom of white pan (a 150s, in} with reagent prepared by mixing equal volames HCI (1 +7) and 1% KI solution (wi). Distibute ca 4g flour evenly over ligudby siting through No. 60 sieve. Altematively, sift flour over surface of dry pan and spray nixed reagent onto flour ftom glass atomizer until all particles are wetted. Black specks or purple spois not observed before the reagent was add indicate presence of bromate or ods. 8. Qualitative Test foriodates () Applicable to 10 g/g or more.—Distibute ca 1 g flour evenly over bottom of Petri dish and completely cover with freshly prepared mixture of 1 volume 1% (wiv) KSCN to four volumes HCI (1 + 32), Break up any lumps with stirring rod and observe with dish on white surfzce. Interpret results as in A. + (0) Applicable to I yg/g or more.—Proceed as in A but use acid- KSCN reagent, (9). Quantitative Method for Bromates (Applicable in absence of iodates,) ©, Reagents (8) Zine sulfate solution —Dissolve 20 g ZnS0,7H,O in $00 mL. HO and dilute to 1 L. (8) Sodium Iyroxie standard solution—04 M. Dissolve 17 g NaOH in 1 LH,O. Titrete against standard acid and adjust to 0.4 001M. (©) Sodium hydroxide standard solution—0.5 M, Dissolve 21 g [NaOH in 1 1H, Tirate against standard acid and adjust to 0.5 01M, (@ Dilute sulfuric acid Approximately 2M. Add 112 mL 1,80, to 800 mL H,0. Cool, and (©) Potassium iodide soltion.—Dissolve 25 g KI in 30 mL H,0 ‘and dilute to 50 mL. Store in amber bottle in cool place. Discard solution showing yellow (Ere (Ammonium molybdate solution-—Dissolve 3g (NH).Mo,0,,-4H,0 in 80 mL 11,0 and dilue to 100 mL. (6) Potassium bromate standard solutions—{1) “Stock solution —$ mg/mL. Dissolve 5.000 g KBrO, (dried 1h at 110°C) in ex 800 mL HO and dilute to 1 'L. (2) Working solution. —0.25 mg/mL. Dilute 25 ml. stock solution to 500 mL. (1) . Potassium iodate standard solutiont—(1) Stock solution-—0.015 M. Dissolve 3.204 g KIO, (died 1h at 110°C) in 2 800 mLH,0 and dilute to 1 L. (2) Working slution.—0,0006 M, Dilute 10 mL stock solution to 250 mL, Prepare fresh daily (9 Sodium thiosulfate standard solutions —(0) Stock solution — Dissolve 22.5 Na,S,0,°5H,O and 0.06 g anhydrous Na,CO, in 800 mL. H,O, and difute to 1 L, Dilute 10 mL to 250 mL. Transfer 5 ml diluted solution to 200 mL Erlenmeyer. Add 100 mL H,0, 10 mL dilute H,SO,, and 1 mL KI solution. Add 5 ml freshly {5 2016 AOAC INTERNATIONAL ‘AOAC OFFICIAL METHODS OF ANALY prepared starch solution (mix 1 g soluble tach wi Water to make this pat, add 100 mi boiling wate 1 min), nd tate With 0.0006 M KIO, fromm 10a tg in 5 mL. adjust tock Nag 0, sluionso at 19 12000259, Sr tokction in amber ote inc Soatun suite working sluion 000359 4. Digg stock slutiono 250 mL. Prepare fesh daly and ches 8 monthly. 1 mL= 0.1 mg KBrO,, tka D. Determination uaatvly tense 200 2280, oon 60 oa beaker and str with speed contolled, motor-driven glee ot (Enough agitation o cise ori provided by Ver deep which doesnot etend to boom of beak) Tata et 0.1 g test portion to sired solution in 2-5 portions sting cx 5 mi, oc ut all dy fou on sure ipa in tigi. While sining, il 50 mL 04 Men from pipet. Dsteate spend of eran tea Sin Ft scatifge, clarifying supemate by Alsuion, i neces “Whatman No. 12 folded pape, or equivalent, is sat Transfer 50 mL of thie te portion slation to 3 ap Eenmeyer. smaller alqut i ken, dite toca SO nt oy HO. Add 10mL2MH,S0, 1 ml KI sition, 1 dp anearg molybdate solution, and SO ml H.O. While sting ald Su ra 0.00359 M NasS,0, (an exces). Add 5 mL freshly pepe starch sohtion and tte excess NBO, with 00006 W ho, (Gee 10m bret gradanedin 0.05 mfr sandard seas Point is best observed straight down.) As end point epproaiy, 81 KIO, solution slowly, one or two cops at ne, seen Viewing fas afi placing ton white surface afer cach afte Take fst edith or purple ge a endpoint then ad seed smote drops to confi. Ad addtional I mL NaS,0, sau ‘gain trate to addtional end pont. Averge the tro diferane Besween amounis of NaS,0, soliton added aad KIO, abt Sirations; ga KBrO, = 10 » (aL 0.00359 M NaS, ab 0.0006 M KIO,). Corect results by recovery factor dteint asbelow E Recovery Factor : Dilute known volume (xm, 3 but <10 ma, of standard KBO, solution to 250 mL. Using 50 mL aliquot, proceed as in sem! paragraph of Determination. th egy “Added bromate” in ygfmL = 10 x (mL 0.00359 MINA,S,0, ~ mi 0.0006 MKIQ) Suspend 50 g portions nonbromated flour in two spas 208 portions ZnSO, solution by sting as above. To eae CH) suspeasin, add 10 mL 1,0; to other (ecovery) suspension 2a standard KB(O, soltion and (10 ~z) m0. Cattio# ators exept ad O05 NaOH fm pie wik xte stirring, Use 5 ml. standard Na,S,0, for “blank” and 10 ml “recovery.” Deduct blank val, if any frm value of KB in “recovery” determination and multiply result by 10 #9 g/ml. recovered bromote” added bromate Recovery factor= © ‘recovered bromate Reference: JAOAC 39, 664(1956)