1、 Reference number ISO 5984:2002(E) ISO 2002INTERNATIONAL STANDARD ISO 5984 Second edition 2002-11-15 Animal feeding stuffs Determination of crude ash Aliments des animaux Dtermination des cendres brutes ISO 5984:2002(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with
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6、l. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2002 All rights reservedISO 5984:2002(E) ISO 2002 All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bo
7、dies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizatio
8、ns, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the
9、ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of th
10、e member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identiying any or all such patent rights. ISO 5984 was prepared by Technical Committee ISO/TC 34,
11、Food products, Subcommittee SC 10, Animal feeding stuffs. This second edition cancels and replaces the first edition (ISO 5984:1978), of which it constitutes a minor revision. Annex A of this International Standard is for information only. INTERNATIONAL STANDARD ISO 5984:2002(E) ISO 2002 All rights
12、reserved 1Animal feeding stuffs Determination of crude ash 1 Scope This International Standard specifies a method for the determination of crude ash of animal feeding stuffs. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute
13、provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of
14、 the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 6498, Animal feeding stuffs Preparation of test samples 3 Term and definition F
15、or the purposes of this International Standard, the following term and definition applies. 3.1 crude ash residue obtained after incineration at 550 C under the conditions specified in this International Standard NOTE It is expressed as a mass fraction of the sample in percent. 4 Principle The organi
16、c matter in a test portion is decomposed by incineration, then the ash obtained is weighed. 5 Apparatus Usual laboratory apparatus and, in particular, the following. 5.1 Analytical balance, capable of weighing to the nearest 0,001 g. 5.2 Muffle furnace, electrically heated, thermostatically controll
17、ed, and provided with a pyrometer. The furnace, when set at 550 C, shall be capable of being controlled in such a way that the temperature in the places where the incineration dishes will be placed will not differ by more than 20 C from this set temperature. 5.3 Drying oven, capable of being control
18、led at (103 2) C. 5.4 Hot-plate or gas burner ISO 5984:2002(E) 2 ISO 2002 All rights reserved5.5 Incineration dish, of platinum or platinum-gold alloy (e.g. 10 % Pt, 90 % Au) or of other material unaffected by the conditions of the test, preferably rectangular with a surface area of about 20 cm 2and
19、 a height of about 2,5 cm. For samples that are inclined to swell on carbonization, use dishes with a surface area of about 30 cm 2and a height of about 3 cm. 5.6 Desiccator, provided with an effective desiccant. 6 Sampling It is important that the laboratory receive a sample which is truly represen
20、tative and has not been damaged or changed during transport or storage. Store the sample in such a way that deterioration and change in composition are prevented. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 6497. 7 Proced
21、ure 7.1 Preparation of test sample Prepare the test sample in acordance with ISO 6498. 7.2 Test portion Weigh, to the nearest 0,001 g, about 5 g of the test sample (7.1) into the incineration dish (5.5), previously heated for at least 30 min in the muffle furnace (5.2) set at 550 C, cooled in the de
22、siccator (5.6) and weighed to the nearest 0,001 g. 7.3 Determination Place the incineration dish containing the test portion (7.2) on a hot plate or over a gas burner (5.4) and heat progressively until the test portion has carbonized. Transfer the dish to the muffle furnace (5.2), previously heated
23、to 550 C, and leave it for 3 h. Inspect visually whether the ash is free from carbonaceous particles. If it is not, replace the dish in the furnace and heat for another 1 h. If carbonaceous particles are still visible, or if there is doubt as to whether they are present, allow the ash to cool, moist
24、en with distilled water, evaporate carefully to dryness in the oven (5.3), set at 103 C. Then replace the dish in the furnace and heat for another 1 h. Allow the dish to cool in the desiccator to room temperature then weigh rapidly to the nearest 0,001 g. NOTE The crude ash obtained by the above pro
25、cedure may be used subsequently for the determination of ash insoluble in hydrochloric acid (see ISO 5985). Carry out two determinations on test portions from the same test sample. 8 Expression of results The crude ash, w, expressed as a mass fraction in percent of the test sample, is equal to: 20 1
26、0 100 % mm w mm = ISO 5984:2002(E) ISO 2002 All rights reserved 3where m 0is the mass, in grams, of the empty dish; m 1is the mass, in grams, of the dish containing the test portion; m 2is the mass, in grams, of the dish and the crude ash. Take as the result the arithmetic mean of the two determinat
27、ions, provided that the requirement for repeatability (see 9.2) is satisfied. Report the result to the nearest 0,1 % (mass fraction). 9 Precision 9.1 Interlaboratory tests Details of interlaboratory tests on the precision of the method are given in annex A. The values derived from these tests may no
28、t be applicable to concentration ranges and matrices other than those given. 9.2 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, will in
29、not more than 5 % of cases exceed the repeatability limit (r) given in Table 1. Table 1 Repeatability limit (r) and reproducibility limit (R) Values in grams per kilogram Sample Crude ash r R Fishmeal 179,8 2,7 4,4 Tapioca 59,1 2,4 3,6 Meat meal 175,6 2,4 5,6 Piglet feed 50,2 2,1 3,3 Broiler feed 42
30、,7 0,9 2,2 Barley 20,0 1,0 1,9 Molasses 119,9 3,6 9,1 Palm kernel expellers 35,8 0,7 1,6 9.3 Reproducibility The absolute difference between two single test results, obtained using the same method on identical test material in different laboratories by different operators using different equipment,
31、will in not more than 5 % of cases exceed the reproducibility limit (R) give in Table 1. ISO 5984:2002(E) 4 ISO 2002 All rights reserved10 Test report The test report shall specify: a) all information required for the complete identification of the sample; b) the sampling method used, if known; c) t
32、he test method used, with reference to this International Standard; d) all operating details not specified in this International Standard, or regarded as optional, together with details of any incident which may have influenced the result(s); e) the test result(s) obtained; f) if the repeatability h
33、as been checked, the final quoted results obtained. ISO 5984:2002(E) ISO 2002 All rights reserved 5Annex A (informative) Results of interlaboratory tests The precision of the method was established by interlaboratory tests carried out in accordance with ISO 5725-1 and ISO 5725-2, in which the Dixon
34、test is replaced by the Grubbs test in the case of outliers. In the tests, 40 to 52 laboratories participated and samples were investigated of fishmeal, tapioca, meat meal, piglet feed, broiler feed, barley, molasses, palm kernel expellers. The results of the interlaboratory tests are given in Table
35、 A.1. Table A.1 Statistical results of interlaboratory tests Sample aParameter 1 2 3 4 5 6 7 8 Number of laboratories 52 48 47 50 48 48 40 49 Number of accepted results 50 47 43 49 44 45 39 46 Mean crude ash, g/kg 179,8 59,1 175,6 50,2 42,7 20,0 119,9 35,8 Repeatability standard deviation (s r ), g/
36、kg 1,0 0,9 0,9 0,8 0,3 0,4 1,3 0,2 Repeatability coefficient of variation, % 1,5 4,1 1,4 4,2 2,1 5,0 3,0 2,0 Repeatability limit (r), g/kg 2,7 2,4 2,4 2,1 0,9 1,0 3,6 0,7 Reproducibility standard deviation (s R ), g/kg 1,4 1,1 1,9 1,1 0,7 0,6 3,1 0,5 Reproducibility coefficient of variation, % 2,5 6
37、,0 3,2 6,6 5,1 9,6 7,6 4,4 Reproducibility limit (R), g/kg 4,4 3,6 5,6 3,3 2,2 1,9 9,1 1,6 a1: fishmeal; 2: tapioca; 3: meat meal; 4: piglet feed; 5: broiler feed; 6: barley; 7: molasses; 8: palm kernel expellers. ISO 5984:2002(E) 6 ISO 2002 All rights reservedBibliography 1 ISO 5725-1, Accuracy (tr
38、ueness and precision) of measurement methods and results Part 1: General principles and definitions 2 ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 3 ISO 5985, Animal feeding stuffs Determination of ash insoluble in hydrochloric acid 4 ISO 6497, Animal feeding stuffs Sampling ISO 5984:2002(E) ICS 65.120 Price based on 6 pages ISO 2002 All rights reserved
