BS ISO 15633-2017 Iron ores Determination of nickel Flame atomic absorption spectrometric method《铁矿石 镍的测定 火焰原子吸收光谱法》.pdf

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1、Iron ores Determination of nickel Flame atomic absorption spectrometric methodBS ISO 15633:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Iron ores Determination of nickel Flame atomic absorption spectrometric methodMinerais de fer Dosage du nickel Mtho

2、de par spectromtrie dabsorption atomique dans la flammeINTERNATIONAL STANDARDISO15633Third edition2017-07Reference numberISO 15633:2017(E)National forewordThis British Standard is the UK implementation of ISO 15633:2017. It supersedes BS ISO 15633:2015, which is withdrawn.The UK participation in its

3、 preparation was entrusted to Technical Committee ISE/58, Iron ores.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct applica

4、tion. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 98400 6ICS 73.060.10Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Commit

5、tee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 15633:2017 ISO 2017Iron ores Determination of nickel Flame atomic absorption spectrometric methodMinerais de fer Dosage du nickel Mthode par spectromtrie dabsorption atomique dans la flamm

6、eINTERNATIONAL STANDARDISO15633Third edition2017-07Reference numberISO 15633:2017(E)BS ISO 15633:2017ISO 15633:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be repr

7、oduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requeste

8、r.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 15633:2017ISO 15633:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved.

9、 Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at

10、the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 15633:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 T

11、erms and definitions . 14 Principle 15 Reagents 26 Apparatus . 27 Sampling and samples 37.1 Laboratory sample . 37.2 Preparation of predried test samples 38 Procedure. 48.1 Number of determinations . 48.2 Test portion 48.3 Blank test and check test 48.4 Determination . 48.4.1 Decomposition of the te

12、st portion 48.4.2 Removal of iron . 58.4.3 Treatment of the residue 58.4.4 Preparation of the calibration solutions 58.4.5 Adjustment of the atomic absorption spectrometer. 68.4.6 Atomic absorption measurements . 69 Expression of results 69.1 Calculation of nickel content . 69.2 General treatment of

13、 results . 79.2.1 Repeatability and permissible tolerance 79.2.2 Determination of analytical result 79.2.3 Between-laboratories precision . 79.2.4 Check for trueness 89.2.5 Calculation of final result 99.3 Oxide factor 910 Test report . 9Annex A (normative) Flowsheet of the procedure for the accepta

14、nce of analytical values for test samples 11Annex B (informative) Derivation of repeatability and permissible tolerance formulae 12Annex C (informative) Precision data obtained by international analytical trial 13Bibliography .14 ISO 2017 All rights reserved iiiContents PageBS ISO 15633:2017ISO 1563

15、3:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide 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 w

16、hich 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. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all

17、 matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. Th

18、is document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).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

19、 or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade name used in this document is information given for the convenience of

20、users and does not constitute an endorsement. For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Bar

21、riers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 02, Chemical analysis.This third edition cancels and replaces the second edition (ISO 15633:2015), of which i

22、t constitutes a minor revision with the following changes: in Clause 1 “0,1 %” has been replaced by “0,10 %”; in 7.1 “ 99,9 % (mass fraction) (see Note of 5.15) in 30 ml of nitric acid (5.9). After cooling, transfer quantitatively to a 1 000 ml one-mark volumetric flask, dilute to volume with water

23、and mix.5.15 Nickel standard solution B, 10 g Ni/ml.Transfer 100,0 ml of nickel standard solution A (5.14) to a 1 000 ml one-mark volumetric flask. Dilute to volume with water and mix.NOTE The purity of the metals stated on the certificates does not generally take into account the presence of absorb

24、ed gases such as oxygen, carbon monoxide, etc.6 ApparatusOrdinary laboratory apparatus including one-mark pipettes and one-mark volumetric flasks complying with the specifications of ISO 648, ISO 1042 and the following.2 ISO 2017 All rights reservedBS ISO 15633:2017ISO 15633:2017(E)6.1 Platinum cruc

25、ible, of minimum capacity 25 ml.6.2 Muffle furnace.6.3 Atomic absorption spectrometer, equipped with an air-acetylene burner.WARNING Follow the manufacturers instructions for igniting and extinguishing the air-acetylene flame to avoid possible explosion hazards. Wear tinted safety glasses whenever t

26、he burner is in operation.The atomic absorption spectrometer used in this method shall meet the following criteria.a) Minimum sensitivity: the absorbance of the most concentrated calibration solution (see 8.4.4) is at least 0,3.b) Graph linearity: the slope of the calibration graph covering the top

27、20 % of the concentration range (expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bottom 20 % of the concentration range determined in the same way.c) Minimum stability: the standard deviation of the absorbance of the most concentrated calibration solution

28、and that of the zero calibration solution each being calculated from a sufficient number of repetitive measurements are less than 1,5 % and 0,5 %, respectively of the mean value of the absorbance of the most concentrated solution.The use of a strip-chart recorder and/or digital readout device is rec

29、ommended to evaluate criteria a), b) and c) and for all subsequent measurements.NOTE Instrument parameters vary with each instrument. The following parameters were successfully used in several laboratories and they can be used as guidelines. An air-acetylene flame was used.Hollow-cathode lamp, mA 10

30、Wavelength, nm 232,0Air flow rate, l/min 10Acetylene flow rate, l/min 2,5In systems where the values shown above for gas flow rates do not apply, the ratio of the gas flow rates can still be a useful guideline.7 Sampling and samples7.1 Laboratory sampleFor analysis, use a laboratory sample of 100 m

31、particle size which has been taken and prepared in accordance with ISO 3082. In the case of ores having significant contents of combined water or oxidizable compounds, use a particle size of 160 m.NOTE A guideline on significant contents of combined water and oxidizable compounds is incorporated in

32、ISO 7764.Ensure that the sample has not been pulverized in a nickel/chromium pot.7.2 Preparation of predried test samplesThoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner that it is representative of the entire contents of the container. Dry

33、 the test sample at 105 C 2 C as specified in ISO 7764. This is the predried test sample. ISO 2017 All rights reserved 3BS ISO 15633:2017ISO 15633:2017(E)6.1 Platinum crucible, of minimum capacity 25 ml.6.2 Muffle furnace.6.3 Atomic absorption spectrometer, equipped with an air-acetylene burner.WARN

34、ING Follow the manufacturers instructions for igniting and extinguishing the air-acetylene flame to avoid possible explosion hazards. Wear tinted safety glasses whenever the burner is in operation.The atomic absorption spectrometer used in this method shall meet the following criteria.a) Minimum sen

35、sitivity: the absorbance of the most concentrated calibration solution (see 8.4.4) is at least 0,3.b) Graph linearity: the slope of the calibration graph covering the top 20 % of the concentration range (expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bott

36、om 20 % of the concentration range determined in the same way.c) Minimum stability: the standard deviation of the absorbance of the most concentrated calibration solution and that of the zero calibration solution each being calculated from a sufficient number of repetitive measurements are less than

37、 1,5 % and 0,5 %, respectively of the mean value of the absorbance of the most concentrated solution.The use of a strip-chart recorder and/or digital readout device is recommended to evaluate criteria a), b) and c) and for all subsequent measurements.NOTE Instrument parameters vary with each instrum

38、ent. The following parameters were successfully used in several laboratories and they can be used as guidelines. An air-acetylene flame was used.Hollow-cathode lamp, mA 10Wavelength, nm 232,0Air flow rate, l/min 10Acetylene flow rate, l/min 2,5In systems where the values shown above for gas flow rat

39、es do not apply, the ratio of the gas flow rates can still be a useful guideline.7 Sampling and samples7.1 Laboratory sampleFor analysis, use a laboratory sample of 100 m particle size which has been taken and prepared in accordance with ISO 3082. In the case of ores having significant contents of c

40、ombined water or oxidizable compounds, use a particle size of 160 m.NOTE A guideline on significant contents of combined water and oxidizable compounds is incorporated in ISO 7764.Ensure that the sample has not been pulverized in a nickel/chromium pot.7.2 Preparation of predried test samplesThorough

41、ly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner that it is representative of the entire contents of the container. Dry the test sample at 105 C 2 C as specified in ISO 7764. This is the predried test sample. ISO 2017 All rights reserved 3 ISO 1563

42、3:2017(E)8 Procedure8.1 Number of determinationsCarry out the analysis at least in duplicate, in accordance with Annex A and independently on one predried test sample.NOTE The expression “independently” means that the second and any subsequent result is not affected by the previous result(s). For th

43、is particular analytical method, this condition implies that the repetition of the procedure is carried out either by the same operator at a different time or by a different operator including, in either case, appropriate recalibration.8.2 Test portionTaking several increments, weigh, to the nearest

44、 0,000 2 g, approximately 1 g of the predried test sample in accordance with 7.2. For ores having significant content of combined water or oxidizable compounds, an air-equilibrate test sample shall be prepared in accordance with ISO 2596.The test portion should be taken and weighed quickly, in order

45、 to avoid reabsorption of moisture.8.3 Blank test and check testIn each run, one blank test and one analysis of a certified reference material of the same type of ore shall be carried out in parallel with the analysis of the ore sample(s) under the same conditions. A predried test sample of the cert

46、ified reference material shall be prepared as specified in 7.2.The certified reference material should be of the same type as the sample to be analysed and the properties of the two materials should be sufficiently similar to ensure that in either case, no significant changes in the analytical proce

47、dure become necessary. Where a certified reference material is not available, a reference material can be used (see 9.2.4).Where the analysis is carried out on several samples at the same time, the blank value may be represented by one test provided that the procedure is the same and the reagents us

48、ed are from the same reagent bottles.Where the analysis is carried out on several samples of the same type of ore at the same time, the analytical value of one certified reference material can be used.8.4 Determination8.4.1 Decomposition of the test portionTransfer the test portion (8.2) to a 250 ml

49、 tall-form beaker. Moisten with a few millilitres of water. Add 25 ml of hydrochloric acid (5.4), cover with a watch-glass and heat for about 1 h on a hotplate adjusted to give a temperature of 100 C in a test beaker containing a similar volume and depth of sulfuric acid (5.11).If the amount of insoluble reside is high, continue heating on a higher temperature zone of the hotplate without boiling the solution.After heating the volume of the solution should have decreased to about 10 ml.Add 5 ml of nitric