1、BRITISH STANDARD BS ISO 5984:2002 Incorporating Corrigendum No. 1 Animal feeding stuffs Determination of crude ash ICS 65.120 BS ISO 5984:2002 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10 January 2003 BSI 15 March 2006 ISBN 0 580 41038
2、2 National foreword This British Standard reproduces verbatim ISO 5984:2002 and implements it as the UK national standard. It supersedes BS 5766-1:1979 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the respons
3、ibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International St
4、andards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Stand
5、ard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European de
6、velopments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 6, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the docum
7、ent was last issued. Amendments issued since publication Amd. No. Date Comments 15699 Corrigendum No. 1 March 2006 Table 1 and Table A.1 replacedReference number ISO 5984:2002(E) INTERNATIONAL STANDARD ISO 5984 Second edition 2002-11-15 Animal feeding stuffs Determination of crude ash Aliments des a
8、nimaux Dtermination des cendres brutes BS ISO 5984:2002iiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committee
9、s. 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 organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Inter
10、national Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International St
11、andards 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 the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard
12、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, Food products, Subcommittee SC 10, Animal feeding stuffs. This second edition cancels and replaces the first edition (ISO 5984:
13、1978), of which it constitutes a minor revision. Annex A of this International Standard is for information only. BS ISO 5984:2002 iiiblankAnimal feeding stuffs Determination of crude ash 1 Scope This International Standard specifies a method for the determination of crude ash of animal feeding stuff
14、s. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agre
15、ements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of 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
16、 of currently valid International Standards. ISO 6498, Animal feeding stuffs Preparation of test samples 3 Term and definition For 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 s
17、pecified in this International Standard NOTE It is expressed as a mass fraction of the sample in percent. 4 Principle The organic 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 An
18、alytical balance, capable of weighing to the nearest 0,001 g. 5.2 Mufflefurnace, electrically heated, thermostatically controlled, 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 incinerati
19、on dishes will be placed will not differ by more than 20 C from this set temperature. 5.3 Dryingoven, capable of being controlled at (103 2) C. 5.4 Hot-plate or gas burner BS ISO 5984:2002 15.5 Incineration dish, of platinum or platinum-gold alloy (e.g. 10 % Pt, 90 % Au) or of other material unaffec
20、ted by the conditions of the test, preferably rectangular with a surface area of about 20 cm 2and 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 d
21、esiccant. 6 Sampling It is important that the laboratory receive a sample which is truly representative 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 speci
22、fied in this International Standard. A recommended sampling method is given in ISO 6497. 7 Procedure 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),
23、 previously heated for at least 30 min in the muffle furnace (5.2) set at 550 C, cooled in the desiccator (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 t
24、he test portion has carbonized. Transfer the dish to the muffle furnace (5.2), previously heated 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
25、 still visible, or if there is doubt as to whether they are present, allow the ash to cool, moisten 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 te
26、mperature then weigh rapidly to the nearest 0,001 g. NOTE The crude ash obtained by the above procedure 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 result
27、s The crude ash, w, expressed as a mass fraction in percent of the test sample, is equal to: 20 10 100 % mm w mm BS ISO 5984:2002 2where 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
28、 ash. Take as the result the arithmetic mean of the two determinations, 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 metho
29、d are given in annex A. The values derived from these tests may not 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
30、laboratory by the same operator using the same equipment, will in 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 rR Fishmeal 179,8 2,7 4,1 Tapioca 59,1 2,4 3,1
31、 Meat meal 175,5 2,5 5,4 Piglet feed 50,2 2,1 3,0 Broiler feed 42,7 0,9 2,1 Barley 19,6 1,0 1,8 Molasses 119,9 3,6 8,8 Palm kernel expellers 35,8 0,7 1,5 9.3 Reproducibility The absolute difference between two single test results, obtained using the same method on identical test material in differen
32、t laboratories by different operators using different equipment, will in not more than 5 % of cases exceed the reproducibility limit (R) give in Table 1. BS ISO 5984:2002 310 Test report The test report shall specify: a) all information required for the complete identification of the sample; b) the
33、sampling method used, if known; c) the 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)
34、 obtained; f) if the repeatability has been checked, the final quoted results obtained. BS ISO 5984:2002 4 Annex 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 th
35、e Dixon 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
36、in Table A.1. BS ISO 5984:2002 Table A.1 Statistical results of interlaboratory tests Sample aParameter 1 2 3 4 5 6 7 8 Mean crude ash content, g/kg 179,8 59,1 175,5 50,2 42,7 19,6 119,9 35,8 Repeatability standard deviation (s r ), g/kg 1,0 0,9 0,9 0,8 0,3 0,4 1,3 0,2 Repeatability coefficient of v
37、ariation, % 0,5 1,5 0,5 1,5 0,8 1,8 1,1 0,7 Repeatability limit (r), g/kg 2,7 2,4 2,5 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, % 0,8 1,9 1,1 2,1 1,7 3,2 2,6 1,5 Reproducibility limit (R), g/kg 4,1 3,
38、1 5,4 3,0 2,1 1,8 8,8 1,5 a1: fishmeal 2: tapioca 3: meat meal 4: piglet feed 5: broiler feed 6: barley 7: molasses 8: palm kernel expellers NOTE ISO 5984:2002 contains incorrect figures due to miscalculations in the reproduction of the performance characteristics. The following Table A.1 contains t
39、he correct numbers. 5Bibliography 1 ISO 5725-1, Accuracy (trueness 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 repeatabili
40、ty 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 BS ISO 5984:2002 6blankBS ISO 5984:2002 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution
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