1、BS ISO 4689-3:2017Iron ores Determination ofsulfur contentPart 3: Combustion/infrared methodBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 4689-3:2017 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 4689-3:2017. It super
2、sedes BS ISO 4689-3:2015 which is withdrawn. The UK participation in its preparation was entrusted to TechnicalCommittee ISE/58, Iron ores.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessarypr
3、ovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2017. Published by BSI Standards Limited 2017ISBN 978 0 580 95542 6ICS 73.060.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was publis
4、hed under the authority of theStandards Policy and Strategy Committee on 31 March 2017.Amendments/corrigenda issued since publicationDate Text affectedBS ISO 4689-3:2017 ISO 2017Iron ores Determination of sulfur content Part 3: Combustion/infrared methodMinerais de fer Dosage du soufre Partie 3: Mth
5、ode par combustion et infrarougeINTERNATIONAL STANDARDISO4689-3Third edition2017-03Reference numberISO 4689-3:2017(E)BS ISO 4689-3:2017ISO 4689-3:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no p
6、art 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 the address below or ISOs member
7、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.orgBS ISO 4689-3:2017ISO 4689-3:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and defin
8、itions . 14 Principle 25 Reagents 26 Apparatus . 27 Sampling and samples 57.1 Laboratory sample . 57.2 Preparation of predried test samples 58 Procedure. 58.1 Number of determinations . 58.2 Test portion 58.3 Blank test and check test 58.4 Determination . 68.5 Preparation of calibration graph . 69 E
9、xpression of results 79.1 Calculation of sulfur content . 79.2 General treatment of results . 79.2.1 Repeatability and permissible tolerance 79.2.2 Determination of analytical result 79.2.3 Between-laboratories precision . 89.2.4 Check for trueness 89.2.5 Calculation of final result 910 Test report
10、. 9Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples 11Annex B (informative) Derivation of repeatability and permissible tolerance equations 12Annex C (informative) Precision data obtained by international analytical trial 13Bibliography .14 ISO
11、2017 All rights reserved iiiContents PageBS ISO 4689-3:2017ISO 4689-3:2017(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
12、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 and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates clo
13、sely with the International Electrotechnical Commission (IEC) on all 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
14、 needed for the different types of ISO documents should be noted. This 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
15、patent rights. ISO shall not be held responsible for identifying any 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 nam
16、e used in this document is information given for the convenience of 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 t
17、o the World Trade Organization (WTO) principles in the Technical Barriers 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 2, Chemical analysis.This third edition c
18、ancels and replaces the second edition (ISO 4689-3:2015), of which it constitutes a minor revision, with the following changes: “0,001 %” has been inserted before “sulfur” in 5.1; in 6.7: under “Combustion crucible”, “Length” has been changed to “Height”; under “Combustion crucible”, outer diameter
19、has been changed from “10 mm” to “26 mm”; under “Combustion crucible”, inner diameter has been changed from “26 mm” to “10 mm”; “0,2 g” has been added after “sulfur” in 8.2; Formula (7) and the relevant descriptions in 9.2.4 have been modified to harmonize this clause across all standards for which
20、ISO/TC 102/SC 2 is responsible.A list of all parts in the ISO 4689 series can be found on the ISO website.iv ISO 2017 All rights reservedBS ISO 4689-3:2017ISO 4689-3:2017(E)IntroductionISO 4689-2 was originally published as ISO 4690:1986. Under a policy of rationalization of the numbering system use
21、d in ISO/TC 102, it has been decided to re-designate ISO 4690:1986 as ISO 4689-2. It was further decided to introduce a combustion/infrared method, numbered ISO 4689-3, i.e. this document.When next revised, ISO 4689:1986 will be re-designated as ISO 4689-1. ISO 2017 All rights reserved vBS ISO 4689-
22、3:2017BS ISO 4689-3:2017Iron ores Determination of sulfur content Part 3: Combustion/infrared methodWARNING This document may involve hazardous materials, operations, and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility
23、 of the user of this document to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use.1 ScopeThis document specifies a combustion/infrared method, using a high-frequency induction furnace, for the determination of the sulfur content
24、 of iron ores.This method is applicable to sulfur contents between 0,002 % (mass fraction) and 0,25 % (mass fraction) in natural iron ores, iron ore concentrates and agglomerates, including sinter products. The method is not applicable to iron ores containing more than 1,0 % (mass fraction) of combi
25、ned water. The apparatus, of which the metal filter is equipped with a heating device, can be applied to iron ores containing less than 3,0 % (mass fraction) of combined water.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content co
26、nstitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory glassware One-mark volumetr
27、ic flasksISO 2596, Iron ores Determination of hygroscopic moisture in analytical samples Gravimetric, Karl Fischer and mass-loss methodsISO 3082, Iron ores Sampling and sample preparation proceduresISO 7764, Iron ores Preparation of predried test samples for chemical analysisISO Guide 35, Reference
28、materials General and statistical principles for certification3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .
29、org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obpINTERNATIONAL STANDARD ISO 4689-3:2017(E) ISO 2017 All rights reserved 1BS ISO 4689-3:2017ISO 4689-3:2017(E)4 PrincipleThe sample is mixed with a flux containing iron, tin and tungsten and heated in a high-frequency inducti
30、on furnace, using oxygen as a supporting fuel and carrier gas.The evolved sulfur dioxide is carried by oxygen into the cell of an infrared detector, where the absorption scale is read.5 ReagentsDuring analysis, use only reagents of recognized analytical grade, and only distilled water or water of eq
31、uivalent purity.5.1 Metallic iron, particle size 0,2 mm to 1,2 mm containing less than 0,001 % sulfur.5.2 Magnesium perchlorate, Mg(ClO4)2, anhydrous, free flowing, particle size 0,5 mm to 2 mm.5.3 Iron(III) oxide, containing less than 0,003 % sulfur.5.4 Metallic tin, particle size 0,2 mm to 1,2 mm,
32、 containing less than 0,001 % sulfur.5.5 Metallic tungsten, particle size 0,2 mm to 1,2 mm containing less than 0,001 % sulfur.5.6 Sodium hydroxide coated silica, particle size 0,5 mm to 2 mm.5.7 Sodium hydroxide, particle size 0,5 mm to 2 mm.5.8 Standard sulfur solution, prepared as follows.Dry 8 g
33、 of potassium sulfate purity 99,99 % (mass fraction) to constant mass at 105 C to 110 C and cool in a desiccator. Weigh the dried masses of potassium sulfate specified in Table 1 and dissolve each portion in water. Cool, transfer each portion to separate volumetric flasks and dilute to volume with w
34、ater.Table 1 Sulfur standard solution (calibration series)Solution no. Mass of potassium sulfate gConcentration of sulfur mg/ml1 0,543 5 1,002 1,087 0 2,003 1,902 2 3,504 2,717 4 5,006 ApparatusOrdinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with t
35、he specifications of ISO 648 and ISO 1042, respectively, as well as the following. See Figure 1.6.1 Oxygen supply.6.2 Absorption tower, containing soda-asbestos (5.6) or sodium hydroxide (5.7).6.3 Drying tower, containing magnesium perchlorate (5.2).2 ISO 2017 All rights reservedBS ISO 4689-3:2017IS
36、O 4689-3:2017(E)6.4 High-frequency induction furnace, having a heating induction coil (height 30 mm to 55 mm, 4 to 5 rolls), capable of heating to a temperature of 1 200 C.An example of a combustion furnace, with combustion gas-refining section, is given in Figure 1.6.5 Combustion tube, quartz.6.6 R
37、efractory combustion crucible.Key1 metal filter2 heating device3 quartz combustion tube4 dust trap5 high-frequency induction coil6 crucible7 holderaOxygen.bCombustion gas.Figure 1 Example of combustion furnace with combustion gas-refining section ISO 2017 All rights reserved 3BS ISO 4689-3:2017ISO 4
38、689-3:2017(E)6.7 Tin capsule.The following dimensions may be used as guidelines.Combustion tube Combustion crucible Tin capsuleLength 140 m to 220 m Height 26 mm Diameter 6 mmOuter diameter 30 mm to 44 mm Outer diameter 26 mm Height 18 mmInner diameter 26 mm to 37 mm Inner diameter 10 mm Mass 0,3 gV
39、olume 0,4 ml6.8 Metal filter.6.9 Dust trap, containing glass wool.6.10 Detector for infrared absorption, an example of which is shown in Figure 2.6.11 Micro-pipette, capacity 100 l, accurate to 1 l.Key1 chopper2 measuring cell3 infrared detector4 motor5 infrared source6 filter cell7 reference cellaC
40、ombustion gas.bOxygen.Figure 2 Example of an infrared detection system4 ISO 2017 All rights reservedBS ISO 4689-3:2017ISO 4689-3:2017(E)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 308
41、2. 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 ISO 7764.7.2 Preparation of predried test samplesThoroughly mix the labora
42、tory 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.For ores having significant content of combined water or
43、oxidizable compounds, an air-equilibrated test sample shall be prepared in accordance with ISO 2596.8 Procedure8.1 Number of determinationsCarry out the analysis at least in duplicate in accordance with Annex A, independently, on one predried test sample.NOTE The expression “independently” means tha
44、t the second and any subsequent result are not affected by the previous result(s). For this 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, a
45、ppropriate recalibration.8.2 Test portionTaking several increments, weigh to the nearest 0,000 2 g, approximately 0,5 g of the predried test sample obtained in accordance with 7.2. For samples containing in excess of 0,1 % (mass fraction), sulfur 0,2 g should be taken.The test portion should be take
46、n and weighed quickly to avoid re-absorption 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 t
47、est sample of the certified 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
48、in the analytical procedure will become necessary.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 are from the same reagent bottles.Where the analysis is carried out on sev
49、eral samples of the same type of ore at the same time, the analytical value of one certified reference material may be used. ISO 2017 All rights reserved 5BS ISO 4689-3:2017ISO 4689-3:2017(E)8.4 DeterminationConnect the furnace (6.4) with components (6.1, 6.2, 6.3, 6.5, 6.8, 6.9, and 6.10) and switch on the power. Set the condition for heating in accordance with the manufacturers instructions after stabilization of the apparatus.Analyse a standardization sample as follows.a) Adjust the readin
