324.28 AOAC Official Method 945.37 Starch in Flour Polarization Method First Action 1945, A Reagents Calcium chloride solution—Dissolve 2 parts CaCl;61,0 ith | part H,0 and adjustto density of 1.30 a120°C (solution containsca, 33% CaCl,). Make faintly pink to phthin by adding 0.1 N NaOH. (Anhydrous CaCl, may be used, but itis usualy alkaline and requires adition of acid to bring ito correct pH.) B. Determination Grind sample finely (100-mesh if possible) and weigh 2.0-2.5 g into 50 ml. round-bottom centrifuge tube with lip, Wash with ether to remove fit, then with 10 mL ea 65% by weight aleohol (day ~ 0.88), and stir thoroughly with glass rod. Centrifuge (If no ‘centrifuge is available, wash samples on filter paper, using Pt cone and slight suction) and pour off solution. Repest washing until ‘60 mL wash liquid has been used, siring each time with same rd. Stir residue with 10mL HO and pour into 200-250 mL Erlenmeyer. Complete transfer by washing with total of 60 mL. CaCl; solution containing 2 mL 0.8% HOAc. Transfer rod to flask and bring mixture to bp quickly over wire gauze, siring frequently Boil briskly 15-17 min, taking precautions to prevent buming and foaming. Rub down particles on sides of flask with rod from time to time, Cool solution quickly in running water and pour into 100 mL Volumetric flask, rinsing thoroughly with CaCl, solution from wash bottle wth medium jet. In diluting to volume, add I drop alcohol, if necessary to destroy froth. ‘After thoroughly mixing sample, pour ea 10 mL solution onto ‘luted filter (Whatman Nos 42 or 44), wetting paper completely. Let filter run dry snd diseard filtrate, Resume filtration, using dry receiver, and collect 40-50 mL. As filtering aids, use Celite with Pyrex glass filters and asbestos with Hirsch-type funnel and suction, Polarize liquid in 10 em tube, taking 2 sets of 10 readings each, (Average of 2 sets should agree within 0,006°,) Starch, % = 100 » R x 100/1 « 203 9 RAP where R is observed angular rotation and Wis weight of sample; 203, is arbitrarily taken as specific rotation for all starches, 1f200 mm tube and saccharimeter are used, 2g sample weighed, and mixture diluted to 100 mL; °S « 4.2586 = % starch, References: Z. Untersuch. Lebensm, 4, 1(1920) Can. J. Res. 11, 751(1934) JAOAC 24, 113(1941}; 27, 87(1944). {© 2007 AAG INTERNATIONAL