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- Original (As adopted by EU)
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This is the original version (as it was originally adopted).
The method determines the ash (including P2O5) content of:
acid caseins
The ash (including P2O5) content: the content of ash as determined by the method specified.
A portion of the sample is incinerated at 825 o C ± 25 o C in the presence of magnesium acetate to bind all phosphorus of organic origin. The final ash is calculated after the weighing of the residue and subtraction of the mass of ash originating from the magnesium acetate.
As described in Section 1.2 of the General Provisions.
Heat two dishes (A,B) (5.3) in the electrical furnace (5.5), controlled at 825 o C ± 25 o C, for 30 minutes. Allow the dishes to cool somewhat and then place in the desiccator (5.7) to the temperature of the balance room and weigh to the nearest 0,1 mg.
Weigh, to the nearest 0,1 mg approximately 3 grams of the test sample (6.1), directly into one of the prepared dishes (A).
Using the pipette (5.2), add to the dish (A) exactly 5 ml of the magnesium acetate solution (4.1) so as to wet all of the test portion, and allow to stand for 20 minutes.
To the other prepared dish (B), add with the pipette (5.2) exactly 5 ml of the magnesium acetate solution (4.1).
Evaporate the contents of both dishes (A and B) to dryness on the boiling water bath (5.6).
Place both dishes in the oven (5.4), controlled at 102 oC ± 1 oC, for 30 minutes.
Heat dish A with its contents on a low flame, a hot plate or under an I/R lamp, until the test portion is completely charred, taking care that it does not burst into flame.
Transfer both dishes (A and B) to the electrical furnace (5.5), controlled at 825 oC ± 25 oC, and heat for at least one hour until all carbon has disappeared from dish A. Allow both dishes to cool somewhat and then place in the desiccator (5.7) to the temperature of the balance room and weigh to the nearest 0,1 mg.
Repeat the operations of heating for approximately 30 minutes, in the electrical furnace (5.5), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass.
The content of ash, including P2O5, in the sample, as a percentage by mass, is given by:
where:
is the mass, in grams, of the test portion;
is the mass, in grams, of dish A and residue;
is the mass, in grams, of the prepared dish A;
is the mass, in grams, of dish B and residue;
is the mass, in grams, of the prepared dish B.
Calculate the final result to the nearest 0,01 %.
The difference in results between the determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,1 grams per 100 grams of product.
The repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.
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