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MM-P-50002i► <br /> Percent phosphate (PO4) - 5•02W <br /> 0.15 <br /> Where: W : veigttt of precipitate after drying <br /> 4.5.3 Man nese determination,(type M only). Pipette 10 al. of the dilute <br /> test solution see .5.1 into a 100 al. volumetric flask and fill to the <br /> mark with distilled water. Mix the solution thoroughly and pipette 10 al. of <br /> this solution into a 500 al. flask. Add 10 al. of nitric acid (sp. gr. 1.42) <br /> and 5 al. sulfuric acid (sp. gr. 1.84), and digest at a low heat to rises of <br /> sulfur trioxide. Remove from the heat and allow to cool. Repeat acid addi- <br /> tions and digestion until the hurling solution remains colorless or light <br /> amber in color. The solution should now be free of organic matter. Cool to <br /> room temperature and add 100 al. of distilled water slowly. Add 5 ml of <br /> approximately 0.1 N silver nitrate solution. Add 3 g. of amtsoni..m persul- <br /> fate. Seat to boiling and continue until all frothing has _eased. Cool to <br /> roes temperature and add 10 al. of approximately 0.13,9 ferrous ammonium sul- <br /> fate. Titrate with standard potassium pe:manjanate (about O.L`i)to a pink <br /> end point which persists for 20 seconds. Run a blank determination following <br /> the above procedure except that the addition of the sample shall be omitted. <br /> Calculate the percent manFpnese as follows: <br /> Percent manganese - (B-A)(a)(10.99) <br /> Where: B = al. of M304 for blank <br /> A = ml. of KKmO4 fcr sample <br /> B = normality of i44m0}6 solution <br /> 4.5.4 Mickel determination. The nickel content shall be determined using <br /> the following reagents and procedure. A blank determination s`al: also be <br /> rum. <br /> 4.5.4.1 Preparation of reagects. <br /> 4.5.4.1.1 A sodi:s nitrate solution shall be prepared 17 placing 24 g. of <br /> sodium nitrate in a one liter volumetric flask. Dilute to the mark vitt_ dis- <br /> tilled water and raiz well. <br /> 4.5.4.1.2 A chloride pyrophosphate mixture scall be prepared by dissolving <br /> 100 g. of tetrasodiun pyrophosphate, 500 g. of ammonium chloride, 2 g. of <br /> potassium iodide and 0.046 g. of nickel in one liter voltmetric flask. Dilute <br /> to the mark and mix well. <br /> 16.5.4.1.3 A sodium cyanide solution shall be prepared by dissolving 5 g. <br /> of sodium cyanide and 0.4 g. of silver nitrate in a one liter volumetric <br /> flask. Dilute to mark and mix well. The sodiuo cyanide solution should not <br /> be kept for more than tame months. <br /> T <br /> �.oh <br />