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The mass of the sample presented to the laboratory for analysis shall be at least 200 grams.
The sample shall always be kept in an air-tight and moisture-tight container.
All chemicals used shall be of recognized analytical reagent quality except where otherwise specified.
The lists of equipment contain only those items with a specialized use and items to a particular specification.
Analytical balance means a balance capable of weighing to at least 0,1 mg.
The test ieves to be used are to be fitted with a lid, to be of diameter 200 mm, to be constructed of wire cloth with a nominal aperture size of 500 urn. The aperture tolerances and wire diameters to be permitted are as given in ISO 3310/1. (Test sieves — Technical requirements and testing — Part 1: Metal wire cloth. ISO 3310/1 — 1975).
The sieves are to be fitted with a receiver.
For grinding the laboratory sample if necessary (see 1.2.4), without development of undue heat and without loss or absorption of moisture, a hammer mill shall not be used.
The result stated in the analytical report is to be the mean value obtained from two determinations which satisfy the repeatability criterion for that method.
Except where otherwise specified, the result shall be calculated as a percentage by mass of the sample.
The test report shall identify the method of analysis used as well as the results obtained. In addition, it shall mention all details of procedure not specified in the method of analysis or which are optional, as well as any circumstances that may have influenced the results obtained. The test report shall give all the information necessary for the complete identification of the sample.
This method determines the moisture content in:
acid caseins
rennet caseins
caseinates
The moisture content of caseins and caseinates: the loss of mass as determined by the method specified.
The residual mass of a test portion is determined after drying at atmospheric pressure in an oven at 102 oC ± 1 oC to constant mass. The loss of mass is calculated as a percentage by mass of the sample.
As described in Section 1.2 of the General Provisions.
Place 3 to 5 grams of the test sample (5.1) into the dish, cover with the lid and weigh to the nearest 0,1 mg (m1).
If an increase in mass occurs, use the lowest recorded mass in the calculation (6.1).
Let the final weight recorded be m2g. The total drying time should not normally exceed six hours.
The loss of mass on drying of the sample, expressed as a percentage by mass, is given by:
×
=
mass, in g of the dish and its lid after process 5.2;
=
mass, in g of the dish, its lid and the test portion before drying (process 5.3);
=
mass, in g of the dish, its lid and the test portion after drying (process 5.4.3 or 5.4.4).
Calculate the loss on drying to the nearest 0,01 %.
The difference in results between two 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 g of moisture per 100 grams of product.
This repeatability interval should be achieved in 95 % of the times that the method is carried out.
This method determines the protein content of:
acid caseins,
rennet caseins,
caseinates,
except those containing ammonium caseinate or other ammonium or nitrogenous non-protein compounds.
The protein content: the nitrogen content as determined by the method specified and then multiplied by 6,38 and expressed as a percentage by mass.
A test portion is digested with a mixture of potassium sulphate and sulphuric acid, in the presence of copper (II) sulphate as catalyst, to convert organic nitrogen to ammoniacal nitrogen. The ammonia is distilled and absorbed into boric acid solution and then titrated with standard hydrochloric acid solution. The nitrogen content is converted to protein content by multiplying by 6,38.
As described in Section 1.2 of the General Provisions.
If the presence of ammonium caseinate or other ammonium compounds is suspected, carry out the following test. Add to 1 gram of sample in a small conical flask 10 ml of water and 100 mg of magnesium oxide. Rinse down any magnesium oxide adhering to the walls and close the flask with a cork stopper, inserting a piece of moistened red litmus paper between the stopper and the neck of the flask. Mix the contents of the flask carefully and heat the flask in a water bath at 60 to 65 o C. If the litmus paper colours blue within 15 minutes ammonia is present, and the method is not applicable (see Section 1).
At the same time as the determination of the nitrogen content of the sample perform a blank determination using 0,5 grams of the sucrose (4.4) instead of the test portion, using the same apparatus, the same quantities of all reagents and the same procedure as described in 6.5. If the titration in the blank determination exceeds 0,5 ml of 0,1 mol/1 acid, the reagents shall be checked and the impure reagent or reagents purified or replaced.
Transfer to the Kjeldahl flask (5.2) 0,3 to 0,4 grams of the test sample (6.1), weighed to the nearest 0,1 mg.
Add 0,2 g of the copper (II) sulphate (4.3) and wash down the neck of the flask with a little water. Add 20 ml of the concentrated sulphuric acid (4.1). Mix the contents of the flask.
Heat gently on the digestion apparatus (5.3) until any frothing has ceased, boil gently until the solution is clear and a pale green-blue colour persists. During heating, swirl the flask occasionally.
Continue the boiling, regulating the heating so as to condense the vapours in the middle of the flask neck. Continue the heating for 90 minutes avoiding local overheating.
Allow to cool to room temperature. Carefully add about 200 ml of water and a few pieces of pumice (5.10.2). Mix and cool again.
Immediately connect the Kjeldahl flask to the condenser by means of the splash-head (5.6).
Gently rotate the Kjeldahl flask to mix its contents. Boil gently at first, avoiding any frothing. Continue the distillation so that 150 ml of distillate are collected in approximately 30 minutes. The distillate should have a temperature below 25 o C. About two minutes before the end of the distillation, lower the conical flask so that the tip of the outlet tube is no longer immersed in the acid solution, and rinse the tip with a little water. Stop heating, remove the outlet tube and rinse its outer and inner walls with a little water, collecting the washings in the conical flask.
The protein content of the sample, expressed as a percentage by mass, is given by:
where:
is the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4.7) used in the determination (6.5);
is the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4.7) used in the blank test (6.3);
is the strength of the standard volumetric hydrochloric acid solution (4.7) in mol/1;
is the mass, in grams, of the test portion.
Calculate the protein content to the nearest 0,1 %.
The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst under the same conditions shall not exceed 0,5 grams of protein per 100 grams of product.
This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.
The method determines the titratable acidity of:
acid caseins.
The titratable acidity of acid caseins: the volume in millilitres, of a 0,1 mol/1 standard sodium hydroxide solution required to neutralize an aqueous extract of 1 gram of the product.
An aqueous extract of the sample at 60 o C is obtained and filtered. The filtrate is titrated against standard sodium hydroxide using phenolphtalein indicator.
Any water used in the method procedure or in the preparation of reagents shall be freed from carbon dioxide by boiling for 10 minutes before use.
As described in Section 1.2 of the General Provisions.
Weigh about 10 grams of the test sample (6.1) to the nearest 10 mg and transfer it to the conical flask (5.2).
Using the 250 ml measuring cylinder (5.6), add 200 ml of freshly boiled and cooled water, previously heated to 60 o C. Stopper the flask, mix by swirling and place in the water bath at 60 o C (5.8) for 30 minutes. Shake the flask at intervals of about 10 minutes.
Filter, and cool the filtrate to about 20 oC. The filtrate must be clear.
Transfer 100 ml of the cooled filtrate into the conical flask (5.5), using the pipette (5.3). Add 0,5 ml of the phenolphtalein indicator solution (4.2), using the pipette (5.4). Titrate with the standard volumetric sodium hydroxide solution (4.1), until the appearance of a faint pink colour, persisting for at least 30 seconds. Determine and record the volume used to the nearest 0,01 ml.
The titratable acidity of the acid casein is given by:
where:
is the volume, in millilitres, of the standard volumetric sodium hydroxide solution (4.1) used;
is the strength of the standard volumetric sodium hydroxide solution (4.1) in mol/1;
is the mass, in grams, of the test portion.
Calculate the titratable acidity to two decimal places.
The difference in results between two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,02 ml of 0,1 mol/1 sodium hydroxide per 1 gram of product.
This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.
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.
This method determines the ash (including P2O 5) content of:
rennet casein
The ash (including P2O5) content: the content of ash as determined by the method specified.
A portion of the sample is incinerated at 825 oC ± 25 oC to constant mass. The residue is determined by weighing and calculated as a percentage by mass of the sample.
As described in Section 1.2 of the General Provisions.
Heat the dish (4.2) in the electrical furnace (4.3), controlled at 825 oC ± 25 oC, for 30 minutes. Allow the dish to cool somewhat and then place in the desiccator (4.4) 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 (5.1) directly into the prepared dish.
Heat the dish with its contents on a low flame, a hot plate or an I/R lamp until the test portion is completely charred, taking care that it does not burst into flame.
Transfer the dish to the electrical furnace (4.3), controlled at 825 oC ± 25 oC, and heat for at least one hour until all carbon has disappeared from the dish. Allow the dish to cool somewhat and then place in the desiccator (4.4) 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 (4.3), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass.
The ash content of the sample, including P2O5, as a percentage per mass, is given by:
where:
is the mass, in grams, of the test portion;
is the mass, in grams, of the dish and residue;
is the mass, in grams, of the prepared dish.
Calculate the final result to the nearest 0,01 %.
The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,15 grams of ash per 100 grams of product.
This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.
This method determines the pH of:
caseinates.
The pH of caseinates: the pH, at 20 oC, of an aqueous solution of caseinates, as determined by the method specified.
The electrometric determination of pH of an aqueous solution of caseinate, using a pH meter.
Any water used in the preparation of the reagents or in the Procedure (6) shall be recently distilled water that has been protected from carbon dioxide absorption.
Two standard buffer solutions with pH values at 20 oC which are known to the second decimal place and will bracket the pH value of the sample under test, for example phtalate buffer solution of pH approximately 4 and a borax buffer solution of pH approximately 9.
As described in Section 1.2 of the General Provisions.
Adjust the temperature of the buffer solutions (4.1) to 20 oC and calibrate the pH meter in accordance with the manufacturer's instructions.
Transfer to the beaker (5.7) 95 ml of water, add 5,0 grams of the test sample (6.1), and mix using the mixer (5.6) for 30 seconds.
Allow to stand for 20 minutes at about 20 oC, covered with a watch glass.
Record, as the pH of the aqueous solution of caseinate, the value read from the dial of the pH meter to at least two decimal places.
The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,05 pH unit.
This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.
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