ISO 663:2017 download free.Animal and vegetable fats and oils-Determination of insoluble impurities content.
1 Scope
ISO 663 specifies a method for the determination of the insoluble impurities content of animal and vegetable fats and oils.
If it is not desired to include soaps (particularly calcium soaps) or oxidized fatty acids in the insoluble impurities content, it is necessary to use a different solvent and procedure. In this case, an agreement is to be reached between the parties concerned.
Milk and milk products (or fat coming from milk and milk products) are excluded from the scope of ISO 663.
2 Normative reference
The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of ISO 663. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 661. Animal and vegetable fats and oils — Preparation of test sample
3 Terms and definitions
For the purposes of ISO 663, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
Use only reagents of recognized analytical grade.
5.1 n-Hexane, or in the absence of this, light petroleum, having a distillation range between 30 C nd 60 C and having a bromine value of less than 1.
For either solvent, the residue on complete evaporation shall not exceed 0,002 g per 100 ml.
5.2 Kieselgur, purified, calcinated, with loss in mass at 900 C (red heat) of less than 0,2 % by mass.
6 Apparatus
Usual laboratory apparatus and, in particular, the foilowing.
6.1 Analytical balance, with an accuracy of ±0.001 g.
6.2 ElectrIc drying oven, capable of operating at 103 C ±2°C.
6.3 Conical flask. o1250 ml capacity, with ground Iass stopper.
6.4 DesIccator, containing an efficient desiccant.
6.5 Ashless filter paper (maxinwm ash content 0,0) %, by mass), retention value of 98%, by mass, for particles olsize greater than 2,5 pmt). or an equivalent glass-fibre filter, of diameter 120 mm, together with a metal (preferably aluminium) or glass vessel with a well.titting lid.
These are alternatives to the filter (6.6) for all products except acid oils.
6.6 FIlter crucible, glass, of grade P16 (pore sIze 10 pm to 16 pm). diameter 40 mm, of capacIty 50 ml, together with a suction bottle,
This is an alternative to 6.5 for all products including acid oils.
7 Sampling
representative sample should have been sent to the laboratory. It should not have been damaged or :hanged during transport or storage.
Sampling Is not part 01 the method specified in ISO 663. A recommended sampling method is tlven In ISO 5555.
8 Preparation of test sample
Prepare the test sample in accordance with ISO 661.
9 Procedure
9.1 Test portion
Weigh, to the nearest 0,01 g. approxImately 20 g of the test sample (Clause 8) Into a conical flask (3).
9.2 Determination
9.2.1 Dry the filter paper and the vessel (6.5) with Its lid, or the filter crucible (6.6). In the oven (6.2) set at 103 °C. Allow to cool in the desiccator (6.4) then weigh to the nearest 0.001 g. For acid oils, prepare the crucible as described in 9.21 and continue as in 92.2.
9.2.2 Add 200 ml of ,,-hexane or light petroleum (5.1) to the flask containing the test portion (9.1). Stopper tiw flask and shake.
For castor oil, the quantity of solvent may be increased to facilitate the operation and this may necessitate the use of a larger flask.
Leave to stand at about 20°C for about 30 mm.
9.2.3 Filter through the filter paper in a suitable funnel or through the filter crucible, using suction if necessary. Rinse the flask to ensure that all Impurities arc washed Into the filter/crucible.
Wash the filter paper or filter crucible by pouting through it small amounts of the same solvent as used in 9.22. but no more than is necessary for the final filtrate to be free from fat or oil. Warm the solvent. if necessary, to a maximum temperature of 60 °C In order to dissolve any solidified fats retained on the filter
9.2.4 If a filter paper is used, remove it from the funnel and place it in the vessel. Allow most of the solvent remaining in the filter paper to evaporate in air and complete the evaporation in the oven set at 103 C. Then remove from the oven, close the vessel with Its lid, allow to cool In the desiccator (6.4) and weigh to the nearest 0,001 g.
9.2.5 If a filter crucible is used, allow most of the solvent remaining in it to evaporate in air under a fume hood and complete the evaporation in the oven set at 103 °C. Then remove from the oven, allow to cool In the desiccator (6.4) and weigh to the nearest 0001 g.
9.2.6 If It Is desired to determine the content of organic Impurities, the use of a previously dried and weighed, ashless filter paper is necessary. In this case, the filter paper containing the insoluble impurities shall be ignited and the mass of ash obtained subtracted from the mass of insoluble impurities.
The organic Impurities content, expressed as a percentage by mass, Is then calculated by multiplying this difference in mass by 100/mo, where m is the mass, in grams, of the test portion.
9.2.7 If analysing acid oils, coat the glass filter crucible with kieselgur (5.2) as follows. In a 100 ml glass beaker, prepare a slurry consisting of 2 g of kieselgur and approxImately 30 ml of light petroleum (5.1). Pour the mixture into the filter crucible under reduced pressure in order to obtain a layer of kieselgur on the glass filter.
Dry the prepared glass filter crucible for I h In the oven (62) set at 103 °C. Allow to cool In the desiccator (6.4) and weigh to the nearest 0,001 g.
Carry out two determinations on test portions taken from the same test sample (Clause 8).
mc is the mass of the test portion (9Jj. in grams;
mi Is the mass of the vessel with its lid and lilter paper, or of the filter crucible (see 9.2.1). in grams;
mz is the mass o(the vessel with its lid and filter paper contaIning the dry residue (see 92.4). or of the filter crucible and dry residue (see 92.5). in grams.
Report the result to the second decimal place.
11 Precision
11.1 Interlaboratory tests
Details of interlaboratory tests on the precision of the method are summarized in AnnexA The values derived from these interiaboratory tests may not be applicable to concentration ranges and matrices other than those given.
11.2 Repeatability
The absolute difference between two independent single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not more than S % of the cases exceed the value of the repeatability limit, r, given in Thhlei1.
11.3 Reproducibility
The absolute difference between two single test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment, will in not more than 5 % olcases exceed the value olthe reproducibility limit, R, given in Table A.1.
12 Test report
The test report shall specify the following:
a) all information necessary for the complete Ide.nlfication of the sample;
b) the sampling method used, if known;
c) the test method used, with reference to this document, i.e. ISO 663;
d) the solvent used;
e) any operating details not specified in this document, or regarded as optional, together with details of any incidents which may have influenced the test results;
f) the test result obtained or. it the repeatability has been checked, the final result obtained.