1、BRITISH STANDARDBS ISO 5984:2002IncorporatingCorrigendum No. 1Animal feeding stuffs Determination of crude ash ICS 65.120g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g4
2、4g42g43g55g3g47g36g58BS ISO 5984:2002This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10 January 2003 BSI 15 March 2006ISBN 0 580 41038 2National forewordThis British Standard reproduces verbatim ISO 5984:2002 and implements it as the UK natio
3、nal 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 It supersedes BS 5766-1:1979 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary.
4、Cross-referencesThe British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British S
5、tandards 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 Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to t
6、he responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front c
7、over, 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 document was last issued.Amendments issued since publicationAmd. No. Date Comments15699 Corrigendum No. 1March 2006 Table
8、 1 and Table A.1 replacedReference numberISO 5984:2002(E)INTERNATIONAL STANDARDISO5984Second edition2002-11-15Animal feeding stuffs Determination of crude ash Aliments des animaux Dtermination des cendres brutes BS ISO 5984:2002iiForeword ISO (the International Organization for Standardization) is a
9、 worldwide federation of national standards bodies (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 represente
10、d on that committee. International organizations, 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 draf
11、ted 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 Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Sta
12、ndard 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 may be the subject of patent rights. ISO shall not be held responsible for identiying any or all such patent rights. ISO 5984 w
13、as 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 5984:1978), of which it constitutes a minor revision. Annex A of this International Standard is for information only. BS ISO 5984:200
14、2iiiblankAnimal 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 p
15、rovisions 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
16、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 samples3 Term and definition For
17、 the purposes of this International Standard, the following term and definition applies. 3.1crude 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 organic m
18、atter 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 controlled,
19、 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 qC from this set temperature. 5.3 Drying oven, capable of being controlle
20、d at (103 r 2) C. 5.4 Hot-plate or gas burner BS ISO 5984:200215.5 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 cm2and a height of about 2,5 cm. For
21、samples that are inclined to swell on carbonization, use dishes with a surface area of about 30 cm2and 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 representative and has not been damaged
22、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 Procedure 7.1 Preparation of test samp
23、le 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 desiccator (5.6) and weighed to th
24、e 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 to 550 C, and leave it for 3 h.
25、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, moisten with distilled water, evapora
26、te carefully to dryness in the oven (5.3), set at 103 qC. 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 procedure may be used subsequently
27、 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: 2010100 %mmwmm uBS ISO 5984:20022wh
28、ere m0is the mass, in grams, of the empty dish; m1is the mass, in grams, of the dish containing the test portion; m2is the mass, in grams, of the dish and the crude ash. Take as the result the arithmetic mean of the two determinations, provided that the requirement for repeatability (see 9.2) is sat
29、isfied. 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 not be applicable to concentration ranges and matrices other than those
30、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 not more than 5 % of cases exceed the repeatability limit (r) given in
31、 Table 1. Table 1 Repeatability limit (r) and reproducibility limit (R)Values in grams per kilogram Sample Crude ash rRFishmeal 179,8 2,7 4,1Tapioca 59,1 2,4 3,1Meat meal 175,5 2,5 5,4Piglet feed 50,2 2,1 3,0Broiler feed 42,7 0,9 2,1Barley 19,6 1,0 1,8Molasses 119,9 3,6 8,8Palm kernel expellers 35,8
32、 0,7 1,59.3 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, will in not more than 5 % of cases exceed the reproducibility limit (R) give in T
33、able 1. BS ISO 5984:2002310 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) the test method used, with reference to this International Standard; d) all operating details not specified in t
34、his 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 has been checked, the final quoted results obtained. BS ISO 5984:20024Annex A (informative) Results of interlabo
35、ratory 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 test is replaced by the Grubbs test in the case of outliers. In the tests, 40 to 52 laboratories participated and samples were investigated o
36、f fishmeal, tapioca, meat meal, piglet feed, broiler feed, barley, molasses, palm kernel expellers. The results of the interlaboratory tests are given in Table A.1. BS ISO 5984:2002Table A.1 Statistical results of interlaboratory tests SampleaParameter 1 2 3 4 5 6 7 8 Mean crude ash content, g/kg 17
37、9,8 59,1 175,5 50,2 42,7 19,6 119,9 35,8 Repeatability standard deviation (sr), g/kg 1,0 0,9 0,9 0,8 0,3 0,4 1,3 0,2 Repeatability coefficient of variation, % 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 (sR), g/kg 1
38、,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 3,1 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:
39、2002 contains incorrect figures due to miscalculations in the reproduction of the performance characteristics.The following Table A.1 contains the correct numbers. 5Bibliography 1 ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definiti
40、ons2 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 method3 ISO 5985, Animal feeding stuffs Determination of ash insoluble in hydrochloric acid4 ISO 6497, Anima
41、l feeding stuffs SamplingBS ISO 5984:20026blankBS ISO 5984:2002BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is
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