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 LAWBS EN ISO 6869:2001 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into e
3、ffect 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. The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs, w
4、hich 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 CENELEC Standards normally include an annex which lists normative references to international publications w
5、ith 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 entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standard
6、s 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. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to
7、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 related international and European developments and promulgate them in the UK. Summary of pages This document com
8、prises 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 back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Am
9、endments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO6869 December2000 ICS06.012 Englishversion AnimalfeedingstuffsDeterminationofthecontentsofcalcium, copper,iron,magnesium,manganese,potassium,sodiumand zincMethodusingatomicabsorptionspectromet
10、ry(ISO 6869:2000) AlimentsdesanimauxDterminationdesteneursen calcium,cuivre,fer,magnsium,manganse,potassium, sodiumetzincMthodeparspectromtriedabsorption atomique(ISO6869:2000) FuttermittelBestimmungderGehalteanCalcium,Kupfer, Eisen,Magnesium,Mangan,Kalium,NatriumundZink Atomabsorptionsspektrometris
11、chesVerfahren(ISO 6869:2000) ThisEuropeanStandardwasapprovedbyCENon1December2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcern
12、ings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthes
13、amestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENOR
14、MALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO6869:2000EForeword ThetextoftheInternationalStandardISO6869:2000hasbeenpreparedbyTechnicalCommittee ISO/TC34
15、“Agriculturalfoodproducts“incollaborationwithTechnicalCommitteeCEN/TC327 “AnimalfeedingstuffsMethodsofsamplingandanalysis“,thesecretariatofwhichisheldbyNEN . ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyJune2001,andcon
16、flictingnationalstandardsshallbe withdrawnatthelatestbyJune2001 . AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,L
17、uxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO6869:2000wasapprovedbyCENasaEuropeanStandard withoutanymodification. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO6869:2000
18、 Reference number ISO 6869:2000(E) INTERNATIONAL STANDARD ISO 6869 First edition 2000-12-01 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
19、 teneurs en calcium, cuivre, fer, magnsium, manganse, potassium, sodium et zinc Mthode par spectromtrie dabsorption atomique ENISO6869:2000 ii ENISO6869:2000 ISO 9686:(0002)Eiii Contents Foreword.iv 1 Scope 1 2 Normative references 1 3 Principle1 4 Reagents and materials 1 5 Apparatus .3 6 Sampling.
20、4 7 Preparation of test sample4 8 Procedure .4 8.1 Detection of presence of organic matter.4 8.2 Test portion 4 8.3 Dry ashing 4 8.4 Decomposition.4 8.5 Blank solution 5 8.6 Determination of copper, iron, manganese and zinc.5 8.7 Determination of calcium, magnesium, potassium and sodium 6 9 Expressi
21、on of results 6 10 Precision.7 10.1 Interlaboratory tests 7 10.2 Repeatability.7 10.3 Reproducibility.8 11 Test report 8 Annex A (informative) Results of interlaboratory tests.9 Bibliography15 ENISO6869:2000 ISO 9686:(0002)E iv Foreword ISO (the International Organization for Standardization) is a w
22、orldwide 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 represented
23、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 drafte
24、d in accordance with the rules given in the ISO/IEC Directives, Part 3. 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 the member bodies casting a vote. A
25、ttention 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 identifying any or all such patent rights. International Standard ISO 6869 was prepared by Technical Committee ISO/TC 34, Food prod
26、ucts, Subcommittee SC 10, Animal feeding stuffs. Annex A of this International Standard is for information only. ENISO6869:2000 INTENRATIONAL TSANDADR ISO 9686:(0002)E1 Animal feeding stuffs Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc Meth
27、od using atomic absorption spectrometry 1 Scope 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) in animal feeding st
28、uffs. The method is applicable to all animal feeding stuffs. The limit of determination for the elements concerned is as follows: K and Na 500 mg/kg; Caa ndMg 5 0mg /kg ; Cu, Fe, Mn and Zn 5 mg/kg. 2 Normative references The following normative documents contain provisions which, through reference i
29、n 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 possibility of applying th
30、e 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 laboratory use Speci
31、fication and test methods. ISO 6498, Animal feeding stuffs Preparation of test samples. 3P r i n c i p l e 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 filtration. The prec
32、ipitate 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. 4 Reagents and m
33、aterials Use only reagents of recognized analytical grade. 4.1 Water, complying with at least grade 3 in accordance with ISO 3696. ENISO6869:2000 ISO 9686:(0002)E 2 4.2 Concentrated hydrochloric acid, c(HCl) = 12 mol/l ( =1,19g/ml ). 4.3 Hydrochloric acid, c(HCl) = 6 mol/l. 4.4 Dilute hydrochloric a
34、cid, c(HCl) = 0,6 mol/l. 4.5 Lanthanum nitrate solution. Dissolve 133 g of La(NO 3 ) 3 6H 2 Oi n1li t r eo fw a t e r( 4 .1 ) . Another lanthanum salt may be used if the lanthanum content of the prepared solution is the same. 4.6 Caesium chloride solution. Di sso lv e10 0go fCsCli n1l itreo fw a te
35、r(4 .1 ). Another caesium salt may be used if the caesium content of the obtained solution is the same. 4.7 Stock solution of Cu, Fe, Mn and Zn. Mix 100 ml of water (4.1) and 125 ml of concentrated hydrochloric acid (4.2) in a 1 litre volumetric flask. Weigh out the following: 392,9 mg of copper(II)
36、 sulfate pentahydrate (CuSO 4 5H 2 O); 702,2 mg of ammonium iron(II) sulfate hexahydrate (NH 4 ) 2 SO 4 . FeSO 4 6H 2 O; 307,7 mg of manganese sulfate monohydrate (MnSO 4 H 2 O); 439,8 mg of zinc sulfate heptahydrate (ZnSO 4 7H 2 O). Transfer the weighed salts to the volumetric flask and dissolve th
37、em 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. NOTE Ready-prepared commercially available solutions may be used. 4.8 Standard solution of Cu, Fe, Mn and Zn. Dilute 20,0 ml of the stock solution (4.7) with water (4.1) to 1
38、00 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. 4.9 Stock solution of Ca, K, Mg and Na. Weigh out the following: 1,907 g of potassium chloride (KCl); 2,028 g of magnesium sulfate heptahydrate (MgSO 4 7H 2
39、 O); 2,542 g of sodium chloride (NaCl). Transfer the weighed salts to a 1 litre volumetric flask. ENISO6869:2000 ISO 9686:(0002)E3 Add 50 ml of hydrochloric acid (4.3) to a beaker. Weigh into the beaker 2,497 g of calcium carbonate (CaCO 3 ). CAUTION: Beware of the development of carbon dioxide. Boi
40、l for 5 min on an electric hot plate (5.4). Cool and transfer the solution to the volumetric flask containing the weighed 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
41、of Mg of the solution is 200 g/ml. NOTE Ready-prepared commercially available solutions may be used. 4.10 Standard solution 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 a
42、re 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 store it in a polyethylene bottle. 4.11 Lanthanum/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 ac
43、id (4.3) to a 100 ml volumetric flask. Dilute to the mark with water (4.1). 5 Apparatus Rinse all volumetric ware, including 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 neces
44、sary to boil with hydrochloric acid each time before use. Usual laboratory apparatus and, in particular, the following. 5.1 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.2 Incineration dishes of platinum, quartz or porcelain, free from potassium and sodium, with a smooth unetched
45、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). 5.3 Glassware of hard borosilicate glass. Before use, boil with hydrochloric acid (4.3) and rinse with water. 5.4 Electric hot plate
46、 or gas burner. 5.5 Boiling water bath. 5.6 Electric muffle furnace, capable of being maintained at (550 15) C. 5.7 Atomic absorption spectrometer (see ISO 6956 6), suitable for measuring at the wavelengths specified in 8.6.1 and 8.7.1, provided with an air-acetylene flame and a facility for correct
47、ion for, or measurement of, background absorption. 5.8 Hollow cathode lamps or electrode-less discharge lamps, for the determination of Ca, Cu, Fe, K, Mg, Mn, Na or Zn. 5.9 Filter paper which does not release minerals. ENISO6869:2000 ISO 9686:(0002)E 4 6 Sampling Sampling is not part of the method s
48、pecified in this International Standard. A recommended sampling method is given in ISO 6497 5. 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 so that deterioration and other changes in composition are prevented. 7 Preparation of test sample Prepare the test sample in accordance with ISO 6
