1、STDmBSI BS EN IS0 bBb7-ENGL 2ORL B. 1b24bb9 0897010 707 I BRITISH STANDARD 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 IS0 6869:2000 has the statu
2、s of a British Standard. ICs 65.120 BS EN IS0 6869:2001 BS 5766-25: 2001 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW c STD=BSI BS EN IS0 bBbq-ENGL 2OOL W lb24bb9 0897OLL b43 M BS EN IS0 6869:ZOOl Amd. No. National foreword Date Comments This British Standard is the officia
3、l English language version of EN IS0 6869:2000. It is identical with IS0 6869:2000. The UK participation in its preparation was entrusted to Technical Committee AWI10, Animal feeding stuffs, which has the responsibility to: - - aid enquirers to understand the text; present to the responsible interna
4、tionallEuropean 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. - A list of organizations represented on this committee can be obtained on request to its
5、 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 with their corresponding European publications. The British Standards which implement these international or European pu
6、blications 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 Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. User
7、s of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0
8、title page, pages ii to iv, pages 1 to 15, the annex ZA page, an inside back cover and a back cover. This British Standard, having been prepared under the direction of the Consumer Products and Services Sector The BSI copyright date displayed in this document indicates when the was last Committee, w
9、as published under the authority of the Standards Committee and comes into effect on 15 March 2001 Amendments issued since publication 0 BSI 03-2001 STD-BSI BS EN IS0 b867-ENGL 2001 = 1624669 0897032 5BT E EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 6869 December 2000 ICs 06.012 English
10、 version Animal feeding stuffs - Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc - Method using atomic absorption spectrometry (IS0 6869:2000) Aliments des animaux - Dtermination des teneurs en calcium, cuivre, fer, magnsium, manganse, potassi
11、um, sodium et zinc - Mthode par spectromtrie dabsorption atomique (IS0 6869:2000) Futtermittel - Bestimmung der Gehalte an Calcium, Kupfer, Eisen, Magnesium, Mangan, Kalium, Natrium und Zink - Atomabsorptionsspektrometnsches Verfahren (IS0 6869:2000) This European Standard was approved by CEN on 1 D
12、ecember 2000. CEN members are bound to comply with the CEWCENELEC 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 bibliographical references concerning such national standards may be
13、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 of a CEN member into its own language and notified to the Management
14、 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, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROP
15、EAN COMMITEE FOR STANDARDIZATION COMITE EUROPBEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Sassar, 36 8-1050 Brussels Q 2000 CEN All rights of exploitation in any form and by any means resewed worldwide for CEN national Members. Ref. No. EN IS0 6869:2000 E STDeBSI BS
16、EN IS0 bBb9-ENGL 2003 M Lb24bb9 0897033 41b R EN IS0 6869:2000 Foreword The text of the International Standard IS0 6869:2000 has been prepared by Technical Committee ISO/TC 34 “Agricultural food products“ in collaboration with Technical Committee CEN/TC 327 “Animal feeding stuffs - Methods of sampli
17、ng 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 latest by June 2001, and conflicting national standards shall be withdrawn at the latest by June 20
18、01. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway,
19、Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 6869:2000 was approved by CEN as a European Standard without any modification. NOTE: Normative references to International Standards are listed in annex ZA (normative). STD.BSI
20、BS EN IS0 hb9-ENGL 2001 R 1624669 iJ8970L4 352 EN IS0 6869:2000 INTERNATIONAL STANDARD IS0 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 Alim
21、ents des animaux - Dtermination des teneurs en calcium, cuivre, fer, magnsium, manganse, potassium, sodium et zinc - Mthode par spectromtrie dabsorption atomique Reference number IS0 6869:2000(E) STD.BiI BS EN IS0 b69-ENGL 2001 II Lb24669 0897025 297 EN IS0 6869:2000 Contents Foreword . iv 1 2 3 4 5
22、 6 7 8 8.1 8.2 8.3 8.4 8.5 8.6 8.7 9 10 10.1 10.2 10.3 11 Scope 1 Principle 1 Apparatus . 3 Sampling . 4 Preparation of test sample 4 Procedure . 4 Detection of presence of organic matter . 4 Test portion 4 Dry ashing 4 Decomposition . 4 Blank solution 5 Normative references 1 Reagents and materials
23、 1 Determination of copper. iron. manganese and zinc . 5 Determination of calcium, magnesium. potassium and sodium 6 Expression of results 6 Precision . 7 Interlaboratory tests 7 Repeatability . 7 Reproducibility . 8 Test report 8 Annex A (informative) Results of interlaboratory tests . 9 Bibliograp
24、hy 15 Previous page is blank . iii . Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical cornmittees. Each member body
25、 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. IS0 collaborates closely with the International Electrotec
26、hnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISOAEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publi
27、cation 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 may be the subject of patent rights. IS0 shall not be held responsible for identifying any or all
28、 such patent rights. International Standard IS0 6869 was prepared by Technical Committee ISOITC 34, Food products, Subcommittee SC 1 O, Animal feeding stuffs. Annex A of this International Standard is for information only. iv STD*BSI BS EN IS0 bb7-ENGL 2001 II 1624669 0877017 Ob% I EN IS0 6869:2000
29、Animal feeding stuffs - Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc - Method using atomic absorption spectrometry 1 Scope This International Standard specifies an atomic absorption spectrometric method for the determination of the contents
30、 of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn) 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 Na 500 mgkg; Ca and Mg 50 mg;
31、 Cu, Fe, Mn and Zn 5 mgkg. 2 Normative references The following normative documents contain 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.
32、 However, parties to agreements based on this International Standard are encouraged to investigate the possibility 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 IS
33、0 and IEC maintain registers of currently valid International Standards. IS0 3696:1907, Water for analytical laboratory use - Specification and test methods. IS0 6498, Animal feeding stuffs - Preparation of test samples. 3 Principle A test portion is dissolved in hydrochloric acid, if necessary afte
34、r aching in a muffle furnace at (550 f 15) OC. Any silica compounds present are removed by precipitation and filtration. 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 absorba
35、nce of each element is measured by comparison with the absorbance of calibration solutions for the same element. 4 Reagents and materials Use only reagents of recognized analytical grade. 4.1 Water, complying with at least grade 3 in accordance with IS0 3696. 1 STD.BSI BS EN IS0 b8bS-ENGL 2001 1b24b
36、b9 08970l,8 TT8 EN IS0 6869:2000 4.2 4.3 4.4 4.5 Lanthanum nitrate solution. Dissolve 133 g of La(N03)3.6H20 in 1 litre of water (4.1). Another lanthanum salt may be used if the lanthanum content of the prepared solution is the same. 4.6 Caesium chloride solution. Dissolve 100 g of CsCI in 1 litre o
37、f water (4.1). Another caesium salt may be used if the caesium content of the obtained solution is the same. 4.7 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(l1) sulfate pentahydrate (CuS04-5
38、H20); - 702,2 mg of ammonium iron(1l) sulfate hexahydrate (NH4)2S04-FeS04.6H20; - 307,7 mg of manganese sulfate monohydrate (MnS04.HzO); - 439,8 mg of zinc sulfate heptahydrate (ZnS04.7H20). Transfer the weighed salts to the volumetric flask and dissolve them in water (4.1). Dilute to the mark with
39、water. The contents of Cu, Fe, Mn and Zn of this stock solution are each 100 pg/ml. NOTE Ready-prepared commercially available solutions may be used. 4.8 Dilute 20,O 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 ar
40、e each 20 pg/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 (KCI); - 2,028 g of magnesium sulfate heptahydrate (MgS04.7H20); - 2,542 g of sodium chloride (NaCI). Transfer the weighed salts to a 1 litr
41、e volumetric flask. Concentrated hydrochloric acid, c(HCI) = 12 moVI (p = 1,19 g/ml). Hydrochloric acid, c(HCI) = 6 moVI. Dilute hydrochloric acid, c(HCI) = 0,6 molh. Stock solution of Cu, Fe, Mn and Zn. Standard solution of Cu, Fe, Mn and Zn. 2 STD-RSI BS EN IS0 bb9-ENGL 2001 I 1624bb9 OB97019 934
42、EN IS0 6869:2000 Add 50 ml of hydrochloric acid (4.3) to a beaker. Weigh into the beaker 2,497 g of calcium carbonate (CaC03). 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
43、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/rnl; the content of Mg of the solution is 200 pg/ml. NOTE Ready-prepared commercially available solutions may be used. 4.10 Standard
44、 solution of Ca, K, Mg and Na. Dilute 25,O 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 pg/ml; the content of Mg of the solution is 20 pg/ml. Prepare the solution fresh in the week of use an
45、d store it in a polyethylene bottle. 4.1 1 Lanthanudcaesium 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). 5 Apparatus Rinse all volumetric war
46、e, 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 necessary to boil with hydrochloric acid each time before use. Usual laboratory apparatus and, in particular, the fol
47、lowing. 5.1 Analytical balance, capable of weighing to the nearest 0,l rng. 5.2 Incineration 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 ab
48、out 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 or gas burner. 5.5 Boiling water bath. 5.6 Electric muffle furnace, capable of being maintained at (550 f 15) “
49、C. 5.7 Atomic absorption spectrometer (see IS0 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 correction for, or measurement of, background absorption. 5.8 Mn, Na or Zn. Hollow cathode lamps or electrode-less discharge lamps, for the determination of Ca, Cu, Fe, K, Mg, 5.9 Filter paper which does not release minerals. 3 STD-BSI BS EN IS0 b869-ENGL ZOO Fe: 248,3 nm; Mn: 279,5 nm; Zn: 213,8 nm. 8.6.2 Preparation of calibration curve Prepare a series of appropriate
