Oxidizing, Bleaching, and Maturing Agents

AACC Method 48-42 Page 1 of 3

Quantitative Method for Bromates

Final approval April 13, 1961Reapproval November 3, 1999

Objective This method determines the amount of potassium bromate, a flour improver, in white and whole-wheat flour. Apparatus 1. Glass stirrer, motor-driven, variable-speed. 2. Beaker, 800-ml. 3. Erlenmeyer flask, 200-ml. 4. Filter paper, Whatman no. 12, 24-cm, fluted. 5. Buret, 10-ml, graduated in 0.05 ml. Reagents 1. Zinc sulfate solution. Dissolve 20 g ZnSO47H2O in water and dilute to 1 liter. 2. NaOH, 0.4N. Dissolve 17 g NaOH in water and dilute to 1 liter (Method 7070). Titrate against standard acid and adjust to 0.4 0.01N. 3. NaOH, 0.5N. Dissolve 21 g NaOH in water and dilute to 1 liter (Method 7070). Titrate against standard acid and adjust to 0.5 0.01N. 4. Dilute H2SO4. Add 112 ml concentrated H2SO4 to 800 ml water. Cool and dilute to 1 liter. 5. KI solution. Dissolve 25 g KI in 30 ml water; dilute to 50 ml. Store in amber bottle in cool place. Discard solution showing yellow tinge of free iodine. 6. Ammonium molybdate. Dissolve 3 g (NH4)6Mo7O244H2O in 80 ml water; dilute to 100 ml. 7. Potassium bromate stock, 5 mg/ml. Dissolve 5.000 g KBrO3, dried 1 hr at 110 in about 800 ml water. Dilute to 1 liter. 8. Potassium bromate standard, 0.25 mg/ml. Dilute 25 ml stock solution to 500 ml. 9. Potassium iodate stock, 0.0898N. Dissolve 3.204 g KIO3, dried 1 hr at 110 in about 800 ml water. Dilute to 1 liter. 10. Potassium iodate standard, 0.00359N. Dilute 10 ml stock solution to 250 ml. Prepare fresh daily. 11. Starch solution. Mix 1 g soluble starch with enough cold water to make a thin paste. Add 100 ml boiling water and boil 1 min. 12. Sodium thiosulfate stock. Dissolve 22.5 g Na2S2O35H2O and 0.06 g anhydrous Na2CO3 in 800 ml water. Dilute to 1 liter. Dilute 10 ml to 250 ml. Transfer 5 ml diluted solution to 200-ml Erlenmeyer flask. Add 100 ml water, 10 ml dilute H2SO4, and 1 ml KI solution. Add 5 ml freshly prepared starch solution (reagent11), and titrate with 0.00359N KIO3 from 10-ml buret graduated in 0.05ml increments. Adjust Na2S2O35H2O stock solution so that 10 ml diluted to 250 ml is 0.00359N. Store stock solution in amber bottle in cool place.

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AACC Method 48-42 Page 2 of 3

Quantitative Method for Bromates (continued)

13. Sodium thiosulfate standard, 0.00359N. Dilute 10 ml stock solution to 250 ml. Prepare fresh daily and check at least monthly. Procedure 1. Transfer quantitatively 200 ml ZnSO4 solution to 800-ml beaker and stir by means of variable-speed stirrer with glass agitator. (Sufficient agitation to disperse flour will be obtained with vortex about 1.5 in. deep that does not extend quite to bottom.) Transfer 50 0.1 g sample to stirred ZnSO4 solution in 2- to 5-g portions. Continue stirring 5 min or until all dry flour on surface is uniformly dispersed. With continued stirring, add 50 ml 0.4N NaOH. Decrease stirrer speed and stir for another 5 min. 2. Filter or centrifuge, clarifying supernatant by filtering through Whatman no. 12, if necessary. 3. Transfer 50 ml of this solution to 200-ml Erlenmeyer flask, or, if smaller aliquot is taken, dilute to about 50 ml with water. Add 10 ml 4N H2SO4, 1 ml KI, 1 drop ammonium molybdate solution, and 50 ml water. With continuous agitation, add excess of 0.00359N Na2S2O3 (510 ml). 4. Add 5 ml freshly prepared starch solution and titrate excess thiosulfate with 0.00359N KIO3 from 10-ml buret graduated in 0.05-ml increments. As end point approaches, add KIO3 slowly, 12 drops at a time, swirling and viewing flask on white surface after each addition. Take first reddish or purplish tinge as end point, read buret, and add 12 drops to confirm. 5. Add another 1 ml thiosulfate and again titrate to end point. Add two differences between amounts of thiosulfate and KIO3 used in titrations. KBrO3 (ppm) = 10 (ml 0.0359N Na2S2O3 ml 0.00359N KIO3). 6. Correct results by recovery factor determined as follows: Dilute known volume (X ml), > 3 ml but < 10 ml, of standard KBrO 3 to 250 ml. Using 50-ml aliquot, proceed as in paragraphs 3 and 4 above. Added bromate in ppm = 10 (ml 0.00359N Na2S2O3 ml 0.00359N KIO3). 7. Suspend 50-g portions of nonbromated flour in two separate 200-ml portions ZnSO4 solution by stirring as above. 8. To one (blank) suspension, add 10 ml water; to other (recovery) suspension add X ml standard KBrO3 and (10 X) ml water. Continue as above, except add 40 ml 0.5N NaOH with continuous stirring. Use 5 ml standard Na2S2O3 for blank and 10 ml for recovery suspension. Deduct blank value, if any, from value of KBrO3 found in recovery data and multiply result by 10 to obtain ppm recovered bromate. Calculation
Recovery factor = added bromate recovered bromate

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AACC Method 48-42 Page 3 of 3

Quantitative Method for Bromates (continued)

References
1. AOAC International. 1995. Official Methods of Analysis of AOAC International, 16th ed. Method 956.03. The Association, Arlington, VA. 2. Rainey, W. L. 1954. Report on potassium bromate in flour. J. Assoc. Off. Agric. Chem. 37:395.