6. AOACSPIFANMethods-2018Awards

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Jaudzems: J ournal of AOAC I nternational V ol. 98, N o. 5, 2015  1393

Figure 2015.08. Typical titration curve obtained from an automatic titrator.

(a)  Check and maintenance of the combined silver electrode .—Rinse electrode with deionized water and wipe before use. Renew the electrolyte periodically permanufacturer’s recommendations. If fat sticks to the electrodes during a series of analyses, then eliminate it by briefly immersing the electrode in acetone. Follow manufacturer’s recommendations for the storage of electrodes when not in use. ( Note : In place of the combined silver electrode, separate silver and reference electrodes may also be used.) (b)  Automated titration .—Prior to first use, check the system linearity by use of a range of required volumes (e.g., 0.1–15 mL) of 0.1 M NaCl solution. Additionally, prior to each use check the system suitability by preparing three calibration check samples using 5.0 mL 0.1 M NaCl solution. H. Extraction and Analysis (a)  Weigh an appropriate aliquot RTF or reconstituted powder (e.g., 25 g) into a suitable beaker (e.g., 150 mL, manual or semiautomatic procedure) or the autosampler titrator cups (automatic titration). For adult nutritionals with a high chloride content, weigh a smaller test portion, e.g., 5 g reconstituted or RTF product. (b)  Add 50 mL 2% (v/v) nitric acid solution as well as a magnetic stirring rod. Place the autosampler cup on a magnetic stirrer and stir until mixed or finely suspended. (c)  The pH of the test solution should be below 1.5. In case of doubt, check by means of a pH meter and, if necessary, add more 2% (v/v) nitric acid solution. (d)  Under continuous stirring, titrate the sample solution automatically with 0.1 M AgNO 3 solution up to the end

potential. Record the volume of 0.1 M AgNO 3 solution consumed. If performing manual titrations, plot a graph of the variation of potential difference as a function of the quantity of the titrant added, continuing the addition of the titrant beyond the presumed equivalence point. The end point of the titration corresponds to the point at which the potential changes most rapidly ( see Figure 2015.08 ). (e)  Special case: determination of very low amounts of chloride .—When determining chloride amounts below 20 mg/100 g, for greater accuracy and precision it is preferable to use a 0.01 MAgNO 3 solution for the titration. Determine the titer of this solution by means of a 0.01 M NaCl solution. I. Calculations Calculate chloride content (w) in mg/100 g RTF or reconstituted sample using the equation: w = A × Mw × Cm x F × 100 m where A = volume (mL) of 0.1 M or 0.01 M AgNO 3 solution used for titration; Mw = atomic weight of chloride (= 35.45 g/mol); Cm = exact molar concentration of the AgNO 3 solution (0.1000 or 0.0100); m = mass of the test portion, in g; and F = dilution factor for preparation of reconstituted powder or concentrate.

Results

The validation study was conducted in accordance with the SPIFAN SLV guidelines (3).