Appendices towards the Operation Manual of Ultrasonic milk analyzer Lactoscan
APPENDIX 4 SAMPLING AND PREPARATION OF SAMPLES
FOR VERIFICATION THE ACCURACY OF THE MILK
ANALYSER, MAKING CORRECTIONS AND RECALIBRATION.
1. Necessary consumables and devices
• Distilled water;
• Minimum 3 milk samples with known content of fat, SNF, protein,
density, lactose, solids;
• Heating water bath;
• Cooling water bath or chamber;
2. General
Milk sampling and storage of samples of raw, thermally treated milk and its
derivatives (cream, whey, butter-milk etc.) aiming verification the accuracy of
the analyser, making corrections and recalibration is accomplished following
the recommendations below:
• Sample to be taken from homogeneous batches, observing all the
requirement;
• The sample’s volume to be enough for making minimum 5
measurements for each sample or not less than 0.5 l;
• The samples to correspond to the standard physic-chemical and
microbiological requirements, to be pure, without admixtures, without
added cleaning or other unusual substances and without falsifications;
• Do not use samples with total acidity of milk more than 17oT;
• Vessels, where the samples will be handled have to be clean, dry,
glass, metal or other suitable material, to be tightly closed with rubber
or other stopples. The stopples not to absorb water and fat and not to
influence the analyzed sample content;
• Till the start of the analyses the samples are stored in conditions,
assuring preservation of their content and quantities (advisable low
temperature – 1-3 oС).
For longer storage of the samples a preservative is added as was already
described in p.9.1.1, and then the sample has to be well stirred.
3. Representative Samples
The samples have to be representative for the corresponding milk type.
Changes in the analyzed parameters in the samples have, if possible, to
cover the whole measuring range – i.e. used samples to be with low, middle
and high content of the analyzed components.
Exemplary recommended values:
Cow milk
Parameter Low value High value
% fat content 2,00 6,00
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% Solids-Non-Fat content 8,00 9,00
The Lactose percentage content (4,0-5,5; average-4, 7), Protein (2,00-4,00;
average-3, 3), salts (0,7-0,8) is proportional to the SNF content. When
preparing samples these values vary within limited bounds.
Sheep milk
Parameter Low value High value
% fat content 5,50 10,00
% Solids-Non-Fat content 9,00 11,50
The Lactose percentage content (average - 4,6), Protein (average - 5,8), salts
(average - 1,0) is proportional to the SNF content. When preparing samples
these values vary within limited bounds.
Buffalo milk
Parameter Low value High value
% fat content 5,50 10,50
% Solids-Non-Fat content 9,00 11,00
The Lactose percentage content (average - 4,7), Protein (average - 4,3), salts
(average - 0,8) is proportional to the SNF content. When preparing samples
these values vary within limited bounds.
Goat milk
Parameter Low value High value
% fat content 2,00 6,00
% Solids-Non-Fat content 8,00 9,00
The Lactose percentage content (average - 4,6), Protein (average - 3,7), salts
(average - 0,8) is proportional to the SNF content. When preparing samples
these values vary within limited bounds.
Cream
Parameter Low value High value
% fat content 8,00 20,00
% Solids-Non-Fat content 2,50 5,00
The cream samples are diluted with distilled water. Degree of dilution is 2-3
times, in dependence of the initial fat content in the cream.
Whey
Parameter Low value High value
% fat content 0,20 0,80
% Solids-Non-Fat content 5,00 7,50
The content of fat and SNF in the whey depends on the kind of the dairy
product as a result of which the whey is received.
4. Samples preparation
Milk – raw or thermally treated
For raw milk sample with average content of the analyzed components is
advisable to be used milk, collected from at least 10 animals from the most
commonly met breed in the region where the analyser will be functioning.
Low fat and high fat samples are prepared on the following way:
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Available fresh or thermally treated milk is poured in a separating funnel,
which is place in a refrigerator for at least 12 hours at temperature 4 - 6 °С in
order to stratify. For a bigger stratification a longer time is required.
The layer at the bottom is poured in a vessel. It is well mixed by pouring it
from vessel to vessel and is warmed up to 40 °С in a water bath.
The upper layer is poured in another vessel.
Using the certified methods the density and the concentration of the analyzed
components - fat, protein, SNF, lactose, salts are determined.
The analyser’s accuracy depends only on the correctness of the chemical
analyses of the components in the samples and the normal acidity during
calibration!
It is recommended the first cow milk sample with low fat content to be with
the following parameters:
1.8-2% FAT; 8.7-9% SNF; 3,3-3,5 % Protein; 4,8-4,9% Lactose; 0,75 Salts;
1030-1033 kg/m3 Density.
The second cow milk sample with high fat content to be with the following
parameters:
5-5,5% FAT; 8.4-8,79% SNF; 3,1-3,2% Protein; 4,6-4,7% Lactose; 0,7 Salts;
1028-1029 kg/m3 Density.
Samples with medial values of the separate parameters are received by
mixing the two boundary values in a definite proportion.
Preserve the samples, using above described method for their longer
storage.
When using samples, stored shortly, preliminary pour the sample from one
vessel to another in order to distribute the milk components evenly paying
attention not to form foam in the sample.
When the samples are stored for a longer period it is recommended to warm
it up to 35-45 °С, and the vessel to be shaken carefully. In case that there is a
cream stuck on the vessel’s surfaces – remove it. The sample is poured from
vessel to vessel several times and is cooled down (advisable to 20 °С /.
If there is separated liquefied fat or white particles with irregular form on the
vessel’s walls this sample could not be used.
Whey and buttermilk
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The samples are poured several times from vessel to vessel and if needed
gradual heating with stirring with cooling down is done.
Cream
The sample is slowly warmed up to 35 – 40 °С in water bath. The fat is
dispersed wholly by carefully shaking and if necessary, by stirring and
pouring it from vessel to vessel till its full homogenization.
From homogenized cream is prepared sample for analyses by diluting it with
distilled water in degree, sufficient for the components of the diluted cream to
be reached in the measuring range of the analyser.
5. Advisable scheme for independently determination the content of
different parameters in milk and its derivatives
When is not possible to use the help of authorized laboratories and above
mentioned milk analysers we recommend you to follow the scheme:
5.1. For cow milk (whole milk, low fat, skimmed milk) and UHT milk
Determination of fat content – Gerber’s method, described in Appendix
Methods.
Density determination – using aerometer, described in Appendix Methods.
SNF determination – by formula – p. [Link].B
Determination of Lactose content – by formula – p.[Link].А
Determination of salts content – by formula – p. [Link].А
Total protein content determination – by formula – p. [Link].А
Example: Determination of the quality parameters for two samples cow milk
(low fat and high fat), obtained and prepared according p. 2.3.1 and 2.4.1.
First – determine the fat content in the samples, using the Gerber’s method
(p.3.2.)
Suppose that for the first sample the result is 2,0 %F, for the second – 5,9
%F.
Second – determine the milk density, using aerometer (p.3.1.)
Suppose that the results are 1,0316 for the first sample and 1,0274
for the second
Third – Calculate the SNF content using the formula (p.[Link].B)
0,075 ∗ 2,0 + 100 − 100 / 1,0316
SNF = = 8,50%
0,378
0,075 ∗ 5,9 + 100 − 100 / 1,0274
SNF = = 8,23%
0,378
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Fourth – determine the lactose content by the formula (p.[Link].А)
Lact. = SNF * 0,55 = 8.50 * 0.55 = 4.67 %
Lact. = SNF * 0,55 = 8.23 * 0.55 = 4.53 %
Fifth – determine the salts content by formula (p.[Link].А /
Salts = SNF * 0,083 = 8.50 * 0.083 = 0.71 %
Salts = SNF * 0,083 = 8.23 * 0.083 = 0.68 %
Sixth – determine the total protein content by formula (p.[Link].А)
Proteins = SNF * 0,367 = 8.50 * 0.367 = 3.12 %
Proteins = SNF * 0,367 = 8.23 * 0.367 = 3.02 %
So, when calibrating the milk analyser we’ll use samples with the following
parameters:
I Ist sample II nd sample
(low fat) (high fat)
milk fat 2,00 5,90
SNF 8,50 8,23
density 1,0316 1,0274
lactose 4,67 4,53
salts 0,71 0,68
proteins 3,12 3,02
5.2. For sheep milk
Determination of fat content – Gerber’s method, described in Methods p. 3.4.
Density determination – using aerometer, described in Methods p. 3.3.
SNF determination – by formula – p. [Link].B
Determination of Lactose content – by formula – p. [Link].А
Determination of solids/salts content – by formula – p. [Link].А
Total protein content determination – by formula – p. [Link].А
Example: Determination of the quality parameters for two samples sheep
milk (low fat and high fat), obtained and prepared according p. 2.3.1 and
2.4.1.
First – determine the fat content in the samples, using the Gerber’s method
(p.3.2.)
Suppose that for the first sample the result is 5,6 %М, for the second – 9,8
%М.
Second – determine the milk density, using aerometer (p.3.1.)
Suppose that the results are 1,0352 for the first sample and 1,0300
for the second
Third – Calculate the SNF content using the formula (p.[Link].B)
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0,075 ∗ 5,6 + 100 − 100 / 1,0352
SNF = = 10,11%
0,378
0,075 ∗ 9,8 + 100 − 100 / 1,0300
SNF = = 9,65%
0,378
Fourth – determine the lactose content by the formula (p.[Link].А)
Lact. = SNF * 0,45 = 10.11 * 0.45 = 4.55 %
Lact. = SNF * 0,45 = 9.65 * 0.45 = 4.34 %
Fifth – determine the salts content by formula (p.[Link].А /
Salts = SNF * 0,075 = 10.11 * 0.075 = 0.76 %
Salts. = SNF * 0,075 = 9.65 * 0.075 = 0.72 %
Sixth – determine the total protein content by formula (p.[Link].А)
Proteins = SNF * 0,475 = 10.11 * 0.475 = 4.80 %
Proteins = SNF * 0,475 = 9.65 * 0,475 = 4.58 %
So, when calibrating the milk analyser we’ll use samples with the following
parameters:
I Ist sample II nd sample
(low fat) (high fat)
milk fat 5,60 9,80
SNF 10,11 9,65
density 1,0352 1,0300
lactose 4,55 4, 34
salts 0,76 0,72
proteins 4,80 4,58
5.3. For wheat, buttermilk and cream
Determination of fat content – Gerber’s method, described in Methods p. 3.4.
Density determination – using aerometer, described in Methods p. 3.3.
SNF determination – using drying - p. 3.3. and formula – p. [Link].А
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