1 AS 2300.4.

4 —1994

Australian Standard
Methods of chemical and physical testing for
the dairying industry

Method 4.4: Dried milk and dried milk

products— Determination of insolubility index

PREFACE
This Standard was prepared by the Standards Australia Committee on Chemical Analysis
This is a free 2 page sample. Access the full version at http://infostore.saiglobal.com.

of Dairy Products to supersede a method for determination of solubility index given in

AS 1629—1974, Methods for the analysis of dried milk and whey. This method is based
on ISO 8156, Dried milk and dried milk products—Determination of insolubility index.

FOREWORD
For routine purposes, including grading, the most widely used procedure for determining
the solubility of dried milk has been the solubility index method of the American Dry
Milk Institute (ADMI), in which a test portion is mixed with water and the reconstituted
product is centrifuged. The volume, in millilitres, of the sediment obtained, i.e. the
insoluble residue, is the solubility index. The superseded method in AS 1629 is based on
the ADMI method.
Although the ADMI solubility index has been widely used for a considerable period it has
become evident that its precision (repeatability and reproducibility) is unsatisfactory with
some types of roller-dried milk and milk products. A joint group of experts from the
International Dairy Federation (IDF), the International Organization for Standardization
(ISO) and the Association of Official Analytical Chemists (AOAC) investigated
alternative methods and also ways to improve the precision of the ADMI method. In order
to keep most of the existing ADMI solubility index specifications for grading, the
IDF/ISO/AOAC Group of Experts (Group E2—Physical properties of dried milk products)
directed its effort to improving the precision of the ADMI method. However, since the
method provides a measure of the insoluble residue it seemed more rational to adopt the
term ‘insolubility index’ to designate what is determined by the modified
sediment-volume method.
In sediment-volume solubility tests on dried milks or dried milk products, the temperature
at which the test portion is reconstituted is the main factor influencing the result. In the
ADMI method a reconstituting temperature of 24°C (75°F) is specified. In modifying the
method, the IDF/ISO/AOAC Group of Experts decided that the product should be
reconstituted in either ‘cold’ water or ‘warm’ water according to normal practice or to the
product’s quality specification. The reconstituting temperatures chosen are, in general,
24°C for spray-dried products and 50°C for roller-dried products. Exceptions to this
general rule may be spray-dried milk-based baby food, and perhaps in some instances
spray-dried whole milk or partly skimmed milk, intended to be reconstituted in warm
water. However, it is important to note that if the insolubility index of spray-dried
fat-containing milks is determined at 50°C, all values obtained will tend to be very small
because the method will no longer detect products which have been subjected to excessive
dry heat through faulty manufacture or storage.
 AS 2300.4.4— 1994 2

This is because milk protein denatured by dry heat is insoluble at 24°C and, along with
entrapped or combined fat, is centrifuged down in the method; at 50°C, the dry-heat-
denatured protein is soluble and this, with the release of the associated fat, can cause a
marked reduction in the volume of sediment.
The introduction of alternative reconstituting temperatures means that the temperature
used needs to be stated when reporting the insolubility index value obtained, e.g. 0.25 mL
(24°C), or 0.10 mL (50°C).
The modified method published as IDF Standard 129 and as ISO 8156 also takes account
of improved models of mixer, and all apparatus and experimental conditions are as closely
defined as practicable. The precision of the method has been determined in an inter-
laboratory collaborative study and is considered to be satisfactory.

METHOD
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1 SCOPE This Standard sets out a method for determining the insolubility index, as a
means of assessing the solubility of instant or non-instant dried milks, dried buttermilk,
dried whey, and dried milk-based infant food. The method is also applicable to these
products where the milk fat has been replaced by another fat.

2 REFERENCED DOCUMENTS The following documents are referred to in this

Standard:
AS
2300 Methods of chemical and physical testing for the dairying industry
2300.4.1 Method 4.1: Dried milk and dried milk products—General information and
preparation of samples
ISO
5725 Precision of test methods—Determination of repeatability and reproducibility
for a standard test method by inter-laboratory tests

3 DEFINITION For the purpose of this Standard, the definition below applies.
3.1 Insolubility index—the volume, in millilitres, of sediment (insoluble residue)
obtained when a dried milk or dried milk product is reconstituted and centrifuged in
accordance with this Standard.

4 PRINCIPLE A test portion of the dried product is reconstituted at a specified

temperature under specified conditions. After a specified period the reconstituted product
is centrifuged and the supernatant liquid removed. The insoluble residue is redispersed in
water and centrifuged and the volume of sediment is measured.

5 REAGENTS
5.1 Water Distilled water or water of equivalent purity.
5.2 Silicone antifoaming agent (e.g. an aqueous emulsion containing 30% m/m of
silicone). The suitability of the silicone antifoaming agent shall be tested by carrying out
the procedure described in Clause 8, without a test portion. Not more than a trace of
silicone fluid (less than 0.01 mL) should be visible at the bottom of the tube.

6 APPARATUS
6.1 Thermometers—capable of measuring temperatures of 24°C and 50°C to an
accuracy of ±0.2°C.

COPYRIGHT
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AS 2300.4.4-1994, Methods of chemical and

physical testing for the dairying industry Dried
milk and dried milk products - Determination of
This is a free 2 page sample. Access the full version at http://infostore.saiglobal.com.

insolubility index

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