Professional Documents
Culture Documents
Objective This method determines the calcium content of flour and bread by a titrimetric procedure. Apparatus 1. Platinum, silica, or porcelain ashing dishes, about 60-mm diameter, 35-ml capacity. Porcelain evaporating dishes of about 25-ml capacity are satisfactory. Do not use flat-bottom dishes of greater diameter than 60 mm. 2. Muffle furnace capable of operating at 550. 3. Filter (choose one of the following): a. Quantitative filter paper, medium speed; Whatman No. 40 or equivalent. b. Fritted glass crucible, fine porosity. c. Microporous porcelain filter crucible, medium porosity. 4. Glassware as required. 5. Acid-washed ashless filter paper. Reagents 1. Ashing aid. a. Magnesium nitrate solution. Dissolve 50 g Mg(NO3)26H2O in water and dilute to 100 ml. Or: b. Redistilled HNO3. 2. Oxalic acid solution, 3%. 3. Potassium permanganate, 0.05N. Prepare and standardize as directed in Method 70-50A. 4. Bromcresol green indicator, 1%. 5. Sodium acetate solution, 20%. 6. Ammonium hydroxide (1 + 50). 7. Hydrochloric acid (HCl), concentrated, ACS grade. 8. Sulfuric acid (H2SO4), concentrated, ACS grade. Procedure 1. Weigh 10.0 g prepared sample (for bread, Method 62-05) into ashing dish that has been ignited, cooled in desiccator, and weighed soon after attaining room temperature. Begin preparation of reagent blank at this point. 2. Incinerate in furnace at about 550 (dull red) until light-gray ash results, or to constant weight. See Note. 3. Cool in desiccator and weigh soon after room temperature is attained, if percent ash is desired. 4. Add 5 ml HCl, allowing acid to rinse upper portion of dish; evaporate to dryness on steam bath.
Inorganic Constituents