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1、BRITISH STANDARD BS EN ISO 6869:2001 BS 5766-25: 2001 Animal feeding stuffs Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc Method using atomic absorption spectrometry The European Standard EN ISO 6869:2000 has the status of a British Standard
2、. ICS 65.120 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 6869:2001 This British Standard, having been prepared under the direction of the Consumer Products
3、and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 March 2001 BSI 03-2001 ISBN 0 580 36933 1 National foreword This British Standard is the official English language version of EN ISO 6869:2000. It is identical with ISO 6869:2000.
4、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. Cross-references Attention is drawn to the fact that CEN and
5、CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section
6、entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Com
7、pliance with a British Standard 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 the UK interests informed; monitor relat
8、ed international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 15, the annex ZA page, an inside back cover and a b
9、ack cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROP
10、ENNE EUROPISCHE NORM EN ISO 6869 December 2000 ICS 06.012 English version Animal feeding stuffs - Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc - Method using atomic absorption spectrometry (ISO 6869:2000) Aliments des animaux - Dtermination
11、 des teneurs en calcium, cuivre, fer, magnsium, manganse, potassium, sodium et zinc - Mthode par spectromtrie dabsorption atomique (ISO 6869:2000) Futtermittel - Bestimmung der Gehalte an Calcium, Kupfer, Eisen, Magnesium, Mangan, Kalium, Natrium und Zink - Atomabsorptionsspektrometrisches Verfahren
12、 (ISO 6869:2000) This European Standard was approved by CEN on 1 December 2000. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bi
13、bliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility o
14、f a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Nor
15、way, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2000 CENAll rights of exploitation in any form and by any means reserved worldwide
16、 for CEN national Members. Ref. No. EN ISO 6869:2000 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Foreword The text of the International Standard ISO 6869:2000 has been prepared by Technical Committee ISO/TC 34 “Agricultural food produc
17、ts“ in collaboration with Technical Committee CEN/TC 327 “Animal feeding stuffs - Methods of sampling and analysis“, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the
18、latest by June 2001, and conflicting national standards shall be withdrawn at the latest by June 2001. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, D
19、enmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 6869:2000 was approved by CEN as a European Standard without any modification
20、. NOTE: Normative references to International Standards are listed in annex ZA (normative). EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 6869:2000(E) INTERNATIONAL STANDARD ISO 6869 First edition 2000
21、-12-01 Animal feeding stuffs Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc Method using atomic absorption spectrometry Aliments des animaux Dtermination des teneurs en calcium, cuivre, fer, magnsium, manganse, potassium, sodium et zinc Mthod
22、e par spectromtrie dabsorption atomique EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 9686:
23、(0002)E iii Contents Foreword.iv 1Scope 1 2Normative references1 3Principle1 4Reagents and materials 1 5Apparatus.3 6Sampling.4 7Preparation of test sample4 8Procedure.4 8.1Detection of presence of organic matter.4 8.2Test portion4 8.3Dry ashing 4 8.4Decomposition.4 8.5Blank solution5 8.6Determinati
24、on of copper, iron, manganese and zinc.5 8.7Determination of calcium, magnesium, potassium and sodium6 9Expression of results 6 10Precision.7 10.1Interlaboratory tests7 10.2Repeatability.7 10.3Reproducibility.8 11Test report8 Annex A (informative) Results of interlaboratory tests.9 Bibliography15 EN
25、 ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 9686:(0002)E iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of prep
26、aring 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 organizations, governmental and non-governmental, in
27、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 ISO/IEC Directives, Part 3. Draft Internat
28、ional 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 the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International S
29、tandard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 6869 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 10, Animal feeding stuffs. Annex A of this International Standar
30、d is for information only. EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADRISO 9686:(0002)E 1 Animal feeding stuffs Determination of the contents of calcium, copper, iron, magnesium, manganese, potassiu
31、m, sodium and zinc Method using atomic absorption spectrometry 1Scope This International Standard specifies an atomic absorption spectrometric method for the determination of the contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn
32、) in animal feeding stuffs. The method is applicable to all animal feeding stuffs. The limit of determination for the elements concerned is as follows: K and Na500 mg/kg; Ca and Mg50 mg/kg; Cu, Fe, Mn and Zn5 mg/kg. 2Normative references The following normative documents contain provisions which, th
33、rough 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 agreements based on this International Standard are encouraged to investigate the possibili
34、ty of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative documents referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical lab
35、oratory use Specification and test methods. ISO 6498, Animal feeding stuffs Preparation of test samples. 3Principle A test portion is dissolved in hydrochloric acid, if necessary after ashing in a muffle furnace at (550 ? 15) C. Any silica compounds present are removed by precipitation and filtratio
36、n. The precipitate is dissolved in hydrochloric acid and diluted to the desired volume, then aspirated into the air-acetylene flame of the atomic absorption spectrometer. The absorbance of each element is measured by comparison with the absorbance of calibration solutions for the same element. 4Reag
37、ents and materials Use only reagents of recognized analytical grade. 4.1Water, complying with at least grade 3 in accordance with ISO 3696. EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 9686:(0002)E 2 4.2Concentrated h
38、ydrochloric acid, c(HCl) = 12 mol/l (? = 1,19 g/ml). 4.3Hydrochloric acid, c(HCl) = 6 mol/l. 4.4Dilute hydrochloric acid, c(HCl) = 0,6 mol/l. 4.5Lanthanum nitrate solution. Dissolve 133 g of La(NO3)36H2O in 1 litre of water (4.1). Another lanthanum salt may be used if the lanthanum content of the pr
39、epared solution is the same. 4.6Caesium chloride solution. Dissolve 100 g of CsCl in 1 litre of water (4.1). Another caesium salt may be used if the caesium content of the obtained solution is the same. 4.7Stock solution of Cu, Fe, Mn and Zn. Mix 100 ml of water (4.1) and 125 ml of concentrated hydr
40、ochloric acid (4.2) in a 1 litre volumetric flask. Weigh out the following: ?392,9 mg of copper(II) sulfate pentahydrate (CuSO45H2O); ?702,2 mg of ammonium iron(II) sulfate hexahydrate (NH4)2SO4.FeSO46H2O; ?307,7 mg of manganese sulfate monohydrate (MnSO4H2O); ?439,8 mg of zinc sulfate heptahydrate
41、(ZnSO47H2O). Transfer the weighed salts to the volumetric flask and dissolve them in water (4.1). Dilute to the mark with water. The contents of Cu, Fe, Mn and Zn of this stock solution are each 100 ?g/ml. NOTEReady-prepared commercially available solutions may be used. 4.8Standard solution of Cu, F
42、e, Mn and Zn. Dilute 20,0 ml of the stock solution (4.7) with water (4.1) to 100 ml in a volumetric flask. The contents of Cu, Fe, Mn and Zn of this solution are each 20 ?g/ml. Prepare the solution fresh on the day of use. 4.9Stock solution of Ca, K, Mg and Na. Weigh out the following: ?1,907 g of p
43、otassium chloride (KCl); ?2,028 g of magnesium sulfate heptahydrate (MgSO47H2O); ?2,542 g of sodium chloride (NaCl). Transfer the weighed salts to a 1 litre volumetric flask. EN ISO 6869:2000 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 13:51:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I
44、SO 9686:(0002)E 3 Add 50 ml of hydrochloric acid (4.3) to a beaker. Weigh into the beaker 2,497 g of calcium carbonate (CaCO3). CAUTION:Beware of the development of carbon dioxide. Boil for 5 min on an electric hot plate (5.4). Cool and transfer the solution to the volumetric flask containing the we
45、ighed salts of K, Mg and Na. Dissolve the salts and dilute to the mark with dilute hydrochloric acid (4.4). The contents of Ca, K and Na of this solution are each 1 mg/ml; the content of Mg of the solution is 200 ?g/ml. NOTEReady-prepared commercially available solutions may be used. 4.10Standard so
46、lution of Ca, K, Mg and Na. Dilute 25,0 ml of stock solution (4.9) with dilute hydrochloric acid (4.4) to 250 ml in a volumetric flask. The contents of Ca, K and Na of this solution are each 100 ?g/ml; the content of Mg of the solution is 20 ?g/ml. Prepare the solution fresh in the week of use and s
47、tore it in a polyethylene bottle. 4.11Lanthanum/caesium blank solution Add 5 ml of lanthanum nitrate solution (4.5), 5 ml of caesium chloride solution (4.6) and 5 ml of hydrochloric acid (4.3) to a 100 ml volumetric flask. Dilute to the mark with water (4.1). 5Apparatus Rinse all volumetric ware, in
48、cluding the pipettes used for preparing calibration solutions, with dilute hydrochloric acid (4.4) before use. If dedicated incineration dishes and glassware are used, it is not necessary to boil with hydrochloric acid each time before use. Usual laboratory apparatus and, in particular, the followin
49、g. 5.1Analytical balance, capable of weighing to the nearest 0,1 mg. 5.2Incineration dishes of platinum, quartz or porcelain, free from potassium and sodium, with a smooth unetched inner surface, upper internal diameter 4 cm to 6 cm, lower internal diameter 2 cm to 2,5 cm, and a height of about 5 cm. Before use, boil with hydrochloric acid (4.3). 5.3Glassware of hard borosilicate glass. Before use, boil with hydrochloric acid (4.3) and rinse with water. 5.4Electric hot plate or gas burner. 5.5Boiling water bath. 5.6Electric muffle furnace,