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1、INTERNATIONAL STANDARD IS0 13310 First edition 1997-08-01 Iron ores - Determination of zinc content - Flame atomic absorption spectrometric method Minerais de fer - Dosage du zinc - Mkthode par spectromktrie dabsorptior? atomique dans la flamme This material is reproduced from IS0 documents under In
2、ternational Organization for Standardization (ISO) Copyright License number IHSIICCI1996. Not for resale. No part of these IS0 documents may be reproduced in any form, electronic retrieval system or otherwise, except as allowed in the copyright law of the country of use, or with the priorwritten con
3、sent of IS0 (Case postale 56,121l Geneva 20, Switzerland, Fax +41 22 734 10 79) IHS or the IS0 Licensers members. Reference number IS0 13310:1997(E) IS0 13310:1997(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member
4、bodies). The work of preparing international Standards is normally carried out through IS0 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
5、and non- governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member
6、 bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard IS0 13310 was prepared by Technical Committee ISO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis. Together with IS0 13311, it cancels a
7、nd replaces IS0 8753:1987, of which it constitutes a technical revision. Annex A forms an integral part of this International Standard. Annexes B and C are for information only. Q IS0 1997 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in a
8、ny form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 l CH-1211 Geneve 20 l Switzerland Internet centralOiso.ch x.400 c=ch; a=4OOnet; p=iso; o=isocs; s=
9、central Printed in Switzerland ii -,-,- INTERNATIONAL STANDARD Q 1s0 IS0 13310:1997(E) Iron ores - Determination of zinc content - Flame atomic absorption spectrometric method WARNING - This International Standard may involve hazardous materials, operations and equipment. This International Standard
10、 does not purport to address all of the safety issues associated with its use. It is the responsibility of the user to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifies a flame atomi
11、c absorption spectrometric method for the determination of the zinc content of iron ores. This method is applicable to zinc contents between 0,001 % (m/m) and 0,5 % (m/m) in natural iron ores, iron ore concentrates and agglomerates, including sinter products. 2 Normative references The following sta
12、ndards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged t
13、o investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 648: 1977, Laboratory glassware - One-mark pipettes. IS0 1042:i 983, Laboratory glassware - One-mark volumetr
14、ic flasks. IS0 3081 :1986, iron ores - Increment sampling - Manual method. IS0 3082:1987, Iron ores - Increment sampling and sample preparation - Mechanical method. IS0 3083:1986, Iron ores - Preparation of samples - Manual method. IS0 3696:1987, Water for analytical laboratory use - Specification a
15、nd test methods. IS0 7764:1985, iron ores - Preparation of predried test samples for chemical analysis. 3 Principle Decomposition of the test portion and removal of silica by treatment with hydrochloric acid and hydrofluoric acid. Oxidation with nitric acid. -,-,- IS0 13310:1997(E) Q IS0 Evaporation
16、 to dryness, followed by dilution and filtration. Ignition of the residue. Fusion with sodium carbonate. Dissolution of the cooled melt with hydrochloric acid. Reservation of the solution. Extraction of iron in the filtrate with 4-methyl-2-pentanone. Recovery of zinc extracted. Decomposition of 4-me
17、thyl- 2-pentanone with nitric acid. Evaporation to dryness and dissolution of salts with the reserved solution and hydrochloric acid. Aspiration of the solution into the flame of an atomic absorption spectrometer using an air-acetylene burner. Comparison of absorbance values obtained for zinc with t
18、hose obtained from the calibration solutions. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only water that complies with grade 2 of IS0 3696. 4.1 Sodium carbonate (Na AC is the reference/certified value for the CRM/RM; C is a value dependent on the type of CRM
19、/RM used. NOTE 1 Certified reference materials used for this purpose should be prepared and certified in accordance with IS0 Guide 35: 1989, Cettification of reference materials - General and statistical principles. For a CRM certified by an interlaboratory test programme 4 l/2 o:+V(A,) 1 where “(A,
20、) is the variance of the certified value A,. For a CRM certified by only one laboratory 4 1 l/2 c=2 a;+- n NOTE 2 This type of CRM should be avoided unless it is known to have an unbiased certified value. 8.2.5 Calculation of final result The final result is the arithmetic mean of the acceptable ana
21、lytical values for the test sample, or as otherwise determined by the operations specified in annex A, calculated to five decimal places and rounded off to the third decimal place as follows: 4 if the figure in the fourth decimal place is less than 5, it is discarded and the figure in the third deci
22、mal place is kept unchanged; b) if the figure in the fourth decimal place is 5 and there is a figure other than 0 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) if the figure in the fourth deci
23、mal place is 5 and the figure 0 is in the fifth decimal place, the 5 is discarded and the figure in the third 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. 8.3 Oxide factor WOO % (m/m) = 1,244 7 wZn % (m/m) 8 -,-,- IS0 9 Test report The te
24、st report shall include the following information: IS0 13310:1997(E) a) b) cl d) 4 f) 9) name and address of the testing laboratory; date of issue of the test report; reference to this International Standard; details necessary for the identification of the sample; result of the analysis: reference n
25、umber of the result; any characteristics noticed during the determination, and any operations not specified in this International Standard, which may have had an influence on the result, for either the test sample or the certified reference material(s). -,-,- IS0 13310:1997(E) IS0 Annex A (normative
26、) Flowsheet of the procedure for the acceptance of analytical values for test samples Start with independent duplicate results P= Xl +x2 2 One more determination ermination 1 = Median (x1, x2, x3, x4) R,: as defined in 8.2.1. 10 -,-,- 0 IS0 IS0 13310:1997(E) Annex B (informative) Derivation of repea
27、tability and permissible tolerance equations The regression equations in 8.2.1 were derived from the results of international analytical trials carried out in 1981 and 1982 on five iron ore samples, involving 22 laboratories in nine countries. Graphical treatment of the precision data is given in an
28、nex C. The test samples used are listed in table B.l. Table 8.1 - Zinc content of test samples Sample Zinc content % (mlm) Sishen iron ore (76-l 6) Robe River (76-21) Stollberg (79-l) Whyalla Ore (79-l 3) Purpur Ore (80-l) 0,001 6 0,009 9 0,139 8 0,477 a 0,164 9 NOTES 1 A report of the international
29、 trial and a statistical analysis of the results (Documents ISOnC 102&C 2 N 702, September 1982 and N 740 E, May 1983) are available from either the Secretariat of lSO/TC 102KC 2 or the Secretariat of ISO/TC 102. 2 The statistical analysis was performed in accordance with the principles embodied in
30、IS0 57251986, Precision of test methods - Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (now withdrawn). 11 -,-,- IS0 13310:1997(E) IS0 Annex C (informative) Precision data obtained by international analytical trials NOTE - Figure Cl is a gra
31、phical presentation of the equations in 8.2.1. ae ,$ 0,06 .Y 8 & 0.05 0.04 0.03 0.02 0.01 0 0 = Rd A=/ + = Cd x = UL I I I I 1 I I I I I I I 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55 Zinc content,% h/ml Figure C-1 - Least-squares fit of precision against X for zinc 12 -,-,- IS0 13310:1997(E) ICS 73.060.10 Descriptors: minerals and ores, metalliferous minerals, iron ores, chemical analysis, determination of content, zinc, atomic absorption spectrometric method. Price based on 12 pages -,-,-