BS ISO 5418-2-2007 Iron ores - Determination of copper - Flame atomic absorption spectrometric method《铁矿石 铜的测定 燃烧原子吸收光谱测定法》.pdf

1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Part 2: Flame atomic absorption spectrometric methodICS 73.060.10Iron ores Determination of copper

2、BRITISH STANDARDBS ISO 5418-2:2006BS ISO 5418-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2007 BSI 2007ISBN 978 0 580 50487 7Amendments issued since publicationAmd. No. Date Commentscontract. Users are responsible for its c

3、orrect application.Compliance with a British Standard cannot confer immunity from legal obligations. National forewordThis British Standard was published by BSI. It is the UK implementation of ISO 5418-2:2006. It supersedes BS 7020-10-2:1988 which is withdrawn.The UK participation in its preparation

4、 was entrusted to Technical Committee ISE/58, Iron ores.A list of organizations represented on ISE/58 can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a Reference numberISO 5418-2:2006(E)INTERNATIONAL STANDARD ISO5418-2First edi

5、tion2006-12-01Iron ores Determination of copper Part 2: Flame atomic absorption spectrometric method Minerais de fer Dosage du cuivre Partie 2: Mthode par spectromtrie dabsorption atomique dans la flamme BS ISO 5418-2:2006ii iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Principle

6、1 4 Reagents.2 5 Apparatus .3 6 Sampling and samples3 6.1 Laboratory sample.3 6.2 Preparation of predried test samples 4 7 Procedure .4 7.1 Number of determinations 4 7.2 Blank test and check test4 7.3 Test portion 4 7.4 Determination.4 7.4.1 Decomposition of the test portion .4 7.4.2 Treatment of t

7、he solution5 7.4.3 Preparation of the set of calibration solutions .5 7.4.4 Adjustment of atomic absorption spectrometer 5 7.4.5 Atomic absorption measurements.6 8 Expression of results 6 8.1 Calculation of mass fraction of copper .6 8.2 General treatment of results.6 8.2.1 Repeatability and permiss

8、ible tolerance.6 8.2.2 Determination of analytical result7 8.2.3 Between-laboratories precision .7 8.2.4 Check for trueness 8 8.2.5 Calculation of final result8 8.3 Oxide factor 9 9 Test report 9 Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples.

9、10 Annex B (informative) Derivation of repeatability and permissible tolerance equations 11 Annex C (informative) Precision data obtained by international analytical trials 12 BS ISO 5418-2:2006iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national

10、 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 on that committee. Internationa

11、l 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 drafted in accordance with the rules

12、given in the ISO/IEC Directives, Part 2. 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 Standard requires approval by at lea

13、st 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 5418-2 was prepared by Technical Committee ISO/TC 10

14、2, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis. This first edition cancels and replaces ISO 4693:1986, which has been technically revised. It has been updated to alter the manner in which precision data are presented. ISO 5418 consists of the following parts, under the gen

15、eral title Iron ores Determination of copper: Part 1: 2,2-Biquinolyl spectrophotometric method Part 2: Flame atomic absorption spectrometric method BS ISO 5418-2:20061Iron ores Determination of copper Part 2: Flame atomic absorption spectrometric method WARNING This part of ISO 5418 may involve haza

16、rdous materials, operations and equipment. This part of ISO 5418 does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this part of ISO 5418 to establish appropriate health and safety practices and determine the applicability of regul

17、atory limitations prior to use. 1 Scope This part of ISO 5418 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of copper in iron ores. This method is applicable to a mass-fraction range of 0,004 % to 0,8 % of copper in natural iron ores, and iron or

18、e concentrates and agglomerates, including sinter products. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (i

19、ncluding any amendments) applies. ISO 648, Laboratory glassware One-mark pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 3082, Iron ores Sampling and sample preparation procedures ISO 3696, Water for analytical laboratory use Specification and test methods ISO 7764, Iron ores

20、Preparation of predried test samples for chemical analysis 3 Principle A test portion is decomposed by treatment with hydrochloric, nitric and hydrofluoric acids. The solution is evaporated with perchloric acid and diluted, and any insoluble residue is filtered. The copper concentration of the solut

21、ion is measured by atomic absorption spectrometry using an air-acetylene flame. BS ISO 5418-2:20062 4 Reagents During the analysis, use only reagents of recognized analytical grade, and only water that complies with grade 2 of ISO 3696. The distillation apparatus used should not contain any copper,

22、and deionized water should not come into contact with copper tubing or taps. 4.1 Iron metal powder, mass fraction of copper C in which case, the difference between the reported result and the reference/certified value is statistically significant. where cis the analytical result for the CRM/RM; Acis

23、 the certified/reference value for the CRM/RM; C is a value dependent on the type of CRM/RM used. Certified reference materials used for this purpose should be prepared and certified in accordance with ISO Guide 35:2006, Reference materials General and statistical principles for certification. For a

24、 CRM/RM certified by an interlaboratory test programme 21/ 2d2cL2 )C = + + V(Anwhere V(Ac) is the variance of the certified/reference value Ac(= 0 for a CRM/RM certified by only one laboratory); n is the number of replicate determinations carried out on the CRM/RM. CRMs certified by only one laborat

25、ory should be avoided, unless they are known to have an unbiased certified value. 8.2.5 Calculation of final result The final result is the arithmetic mean of the acceptable analytical values for the test sample, or as otherwise determined by the operations specified in Annex A, is calculated to fiv

26、e decimal places and rounded off to the third decimal place as follows: a) where the figure in the fourth decimal place is less than 5, it is discarded and the figure in the third decimal place is kept unchanged; b) where the figure in the fourth decimal place is 5 and there is a figure other than 0

27、 in the fifth decimal place, or if the figure in the fourth decimal place is greater than 5, the figure in the third decimal place is increased by one; c) where the figure in the fourth decimal place is 5 and the figure 0 is in the fifth decimal place, the 5 is discarded and the figure in the third

28、decimal place is kept unchanged if it is 0, 2, 4, 6 or 8 and is increased by one if it is 1, 3, 5, 7 or 9. BS ISO 5418-2:200698.3 Oxide factor The oxide factor, expressed as a percent, is given by the following equation: wCuO= 1,251 8 wCu9 Test report The test report shall include the following info

29、rmation: a) name and address of the testing laboratory; b) date of issue of the test report; c) a reference to this part of ISO 5418; d) details necessary for the identification of the sample; e) result of the analysis; f) reference number of the result; g) any characteristics noticed during the det

30、ermination and any operations not specified in this part of ISO 5418 which may have had an influence on the result, either for the test sample or for the certified reference material(s). BS ISO 5418-2:200610 Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for t

31、est samples Rd: as defined in 8.2.1. BS ISO 5418-2:200611Annex B (informative) Derivation of repeatability and permissible tolerance equations The regression equations in 8.2.1 were derived from the results of international analytical trials carried out in 1972/1973 on five iron ore samples, involvi

32、ng 45 laboratories in nine countries. The graphical treatment of the precision data is given in Annex C. The test samples used are listed in Table B.1. Table B.1 Mass fraction of copper in test samples Sample Mass fraction of copper % Malmberget concentrate (72-1) 0,001 1 Kiruna R (72-2) 0,011 3 Roa

33、sting residue (Purpurerz) (72-3) 0,072 Russian pyrite cinder (Russ Abbrnde (72-4) 0,378 Forsbo ore (72-5) 0,781 NOTE 1 A report of the international trial and a statistical analysis of the results (Document ISO/TC 102/SC 2 N306E, May 1973) is available from the Secretariat of ISO/TC 102/SC 2. NOTE 2

34、 The statistical analysis was performed in accordance with the principles embodied in ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. BS ISO 5418-2:

35、200612 Annex C (informative) Precision data obtained by international analytical trials Key X Mass fraction of copper, % Y Precision, % Figure C.1 Least-squares fit of precision against X for copper BS ISO 5418-2:2006blankBS ISO BSI389 Chiswick High RoadLondonW4 4AL5418-2:2006BSI British Standards I

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