1、BSI Standards PublicationBS ISO 2597-2:2015Iron ores Determination oftotal iron contentPart 2: Titrimetric methods after titanium(III)chloride reductionBS ISO 2597-2:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 2597-2:2015.It supersedes BS ISO 2597-2:20
2、08 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee ISE/58, Iron ores.A list of organizations represented on this committee can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 necessaryprovisions of a contract.
3、 Users are responsible for its correctapplication. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 79561 9ICS 73.060.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority
4、of theStandards Policy and Strategy Committee on 30 November 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 2597-2:2015 ISO 2015Iron ores Determination of total iron content Part 2: Titrimetric methods after titanium(III) chloride reductionMinerais de fer Dosag
5、e du fer total Partie 2: Mthodes titrimtriques aprs rduction au chlorure de titane(III)INTERNATIONAL STANDARDISO2597-2Second edition 2015-11-01Reference numberISO 2597-2:2015(E)BS ISO 2597-2:2015ISO 2597-2:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in Swit
6、zerlandAll rights reserved. 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 re
7、quested from either ISO at 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.orgBS ISO 2597-2:2015ISO 2597-2:2015(E)Foreword iv1 Scop
8、e . 12 Normative references 13 Principle 13.1 Decomposition of the test portion . 13.1.1 Acid decomposition . 13.1.2 Fusion-filtration 23.2 Titration of iron 24 Reagents 25 Apparatus . 36 Sampling and samples 46.1 Laboratory sample . 46.2 Preparation of test samples . 46.2.1 General 46.2.2 Ores havi
9、ng significant contents of combined water or oxidizable compounds 46.2.3 Ores outside the scope of 6.2.2 47 Procedure. 57.1 Number of determinations . 57.2 Blank test and check test 57.3 Determination of hygroscopic moisture content. 57.4 Test portion 57.5 Determination . 57.5.1 Decomposition of the
10、 test portion 57.5.2 Reduction . 78 Expression of results 88.1 Calculation of total iron content 88.2 General treatment of results . 88.2.1 Repeatability and permissible tolerance 88.2.2 Determination of analytical result 98.2.3 Between-laboratories precision . 98.2.4 Check for trueness 98.2.5 Calcu
11、lation of final result . 108.3 Oxide factors 109 Test report 10Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples 12Annex B (normative) Procedure of Japanese weighing method .13Bibliography .14 ISO 2015 All rights reserved iiiContents PageBS ISO 2
12、597-2:2015ISO 2597-2:2015(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
13、 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 closely with the International Electrotechnical Comm
14、ission (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 needed for the different types of ISO documents s
15、hould 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 patent rights. ISO shall not be held responsible for
16、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 name used in this document is information given for the con
17、venience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Forewor
18、d - Supplementary informationThe committee responsible for this document is ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis.This second edition cancels and replaces the first edition (ISO 2597-2:2008), which has been technically revised.ISO 2597 consists of the fol
19、lowing parts, under the general title Iron ores Determination of total iron content: Part 1: Titrimetric method after tin(II) chloride reduction Part 2: Titrimetric methods after titanium(III) chloride reductioniv ISO 2015 All rights reservedBS ISO 2597-2:2015INTERNATIONAL STANDARD ISO 2597-2:2015(E
20、)Iron ores Determination of total iron content Part 2: Titrimetric methods after titanium(III) chloride reductionWARNING This part of ISO 2597 may involve hazardous materials, operations and equipment. This part of ISO 2597 does not purport to address all of the safety problems associated with its u
21、se. It is the responsibility of the user of this part of ISO 2597 to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use.1 ScopeThis part of ISO 2597 specifies a titrimetric method, free from mercury pollution, for the determinatio
22、n of total iron content in iron ores, using potassium dichromate as titrant after reduction of the iron(III) by tin(II) chloride and titanium(III) chloride. The excess reductant is then oxidized by either dilute potassium dichromate.This method is applicable to a concentration range of 30 % mass fra
23、ction to 72 % mass fraction of iron in natural iron ores, iron ore concentrates and agglomerates, including sinter products.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references,
24、 only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 80000-1:2009, Quantities and unit Part 1: GeneralISO 385, Laboratory glassware BurettesISO 648, Laboratory glassware Single-volume pipettesISO 1042, Laborator
25、y glassware One-mark volumetric 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 procedures3 Principle3.1 Decomposition of the test portion3.1.1 Acid decompositionF
26、or samples containing not more than 0,05 % mass fraction of vanadium, the test portion is treated with hydrochloric acid in the presence of tin chloride.The residue is filtered, ignited and treated with hydrofluoric and sulfuric acids. The mixture is fused with potassium disulfate and the cold melt
27、is dissolved in water more hydrochloric acid and combined with the main iron solution, which is treated with potassium permanganate and evaporated. ISO 2015 All rights reserved 1BS ISO 2597-2:2015ISO 2597-2:2015(E)3.1.2 Fusion-filtrationFor samples containing more than 0,05 % mass fraction of vanadi
28、um, the test portion is fused with a mixture of fluxes, the cold melt is leached with water and the precipitate is filtered, washed in sodium hydroxide solution, dissolved in hydrochloric acid and evaporated.3.2 Titration of ironThe major portion of the iron(III) is reduced by tin(II) chloride and t
29、he remainder of the iron(III) is reduced by titanium(III) chloride. The excess reductant is oxidized with either dilute potassium dichromate solution. The reduced iron is titrated with potassium dichromate solution using the sodium diphenylaminesulfonate indicator.4 ReagentsDuring the analysis, use
30、only reagents of recognized analytical reagent grade, and only distilled water or water of equivalent purity.4.1 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml. (Methods 1 and 2).4.2 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 1 + 1. (Methods 1 and 2).4.3 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml,
31、 diluted 1 + 12. (Methods 1 and 2).4.4 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 2 + 100. (Methods 1 and 2).4.5 Hydrofluoric acid, 40 % mass fraction ( 1,13 g/ml) or 48 % mass fraction ( 1,19 g/ml). (Methods 1 and 2).4.6 Sulfuric acid, 1,84 g/ml. (Methods 1 and 2).4.7 Sulfuric acid, 1,84 g/
32、ml, diluted 1 + 1, carefully pour 1 volume of reagent 4.6 into one volume of cold water. (Methods 1 and 2).4.8 Orthophosphoric acid, 1,7 g/ml. (Methods 1 and 2).4.9 Perchloric acid, 72 % mass fraction ( 1,7 g/ml), diluted 1 + 1. (Method 2).4.10 Sulfuric acidorthophosphoric acid mixture, pour 150 ml
33、of orthophosphoric acid (4.8) into about 400 ml of water while stirring, add 150 ml of sulfuric acid (4.6), cool in a water bath, dilute with water to 1 l and mix well. (Methods 1 and 2).4.11 Sodium hydroxide (NaOH), solution, 20 g/l. (Methods 1 and 2).4.12 Hydrogen peroxide (H2O2), 30 % by volume s
34、olution. (Methods 1 and 2).4.13 Hydrogen peroxide (H2O2), 30 % by volume solution, diluted 1 + 9. (Method 1).4.14 Tin(II) chloride solution, 100 g/l, dissolve 100 g of crystalline tin(II) chloride (SnCl22H2O) in 200 ml of hydrochloric acid (4.1) by heating the solution in a water bath. Cool the solu
35、tion and dilute with water to 1 l. This solution should be stored in a brown glass bottle with a small quantity of granular tin metal. (Methods 1 and 2).2 ISO 2015 All rights reservedBS ISO 2597-2:2015ISO 2597-2:2015(E)4.15 Potassium permanganate (KMnO4) solution, 25 g/l. (Methods 1 and 2).4.16 Pota
36、ssium dichromate (K2Cr2O7) solution, 1 g/l. (Method 1).4.17 Titanium(III) chloride (TiCl3) solution, 20 g/l, dilute one volume of titanium(III) chloride solution (about 20 % TiCl3) with nine volumes of hydrochloric acid (4.2). (Methods 1 and 2).Alternatively, dissolve 1,3 g of titanium sponge in abo
37、ut 40 ml of hydrochloric acid (4.1) in a covered beaker by heating in a water bath. Cool the solution and dilute with water to 200 ml. Prepare fresh solution as needed.4.18 Flux mixture, mix one portion of anhydrous sodium carbonate (Na2CO3) and two portions of sodium peroxide (Na2O2). (Methods 1 an
38、d 2).4.19 Iron standard solution, 0,1 mol/l, transfer 5,58 g of iron(III) oxide (purity greater than 99,9 % mass fraction) to a 500 ml beaker flask and place a small filter funnel in the neck. Add 75 ml of hydrochloric acid (4.2) in small increments and heat until dissolved. (Methods 1 and 2).Cool a
39、nd oxidize with 5 ml of hydrogen peroxide (4.13) added in small portions. Heat to boiling and boil to decompose the excess hydrogen peroxide and to expel chlorine. Cool, transfer to a 1 000 ml volumetric flask and mix well.1,00 ml of this solution is equivalent to 1,00 ml of the standard potassium d
40、ichromate solution (4.20).4.20 Potassium dichromate (99,9 % minimum purity), standard solution, 0,016 67 mol/l, pulverize about 6 g of potassium dichromate reagent in an agate mortar, dry at 140 C to 150 C for 2 h, and cool to room temperature in a desiccator. (Methods 1 and 2).Transfer 4,903 g of t
41、his material to a 300 ml beaker, dissolve in about 100 ml of water, transfer quantitatively to a 1 000 ml volumetric flask, make up to volume with water after cooling to 20 C and mix well. Record the temperature at which this dilution was made (20 C) on the stock bottle. Measure the temperature at e
42、ach use to correct the volume of titrant used.The volumetric flask should previously be calibrated by weighing the mass of water contained at 20 C and converting to volume.Water used for preparation should previously be equilibrated at room temperature.A calibrated mercury thermometer, graduated in
43、0,1 C divisions and having a marked dipping line, should be used. Take a sufficient volume of standard solution for dipping the thermometer and transfer to a suitable beaker. Measure the temperature of the solution to the nearest 0,1 C, after dipping for more than 60 s.4.21 Indigo carmine 5,5-disulf
44、onic acid disodium salt (Cl6H8O8N2S2Na2) solution, 0,1 g/100 ml, dissolve 0,1 g of indigo carmine in a cold mixture of 50 ml sulfuric acid (4.7) and 50 ml of water. (Method 1).4.22 Sodium diphenylaminesulfonate indicator solution, 0,2 g/100 ml, dissolve 0,2 g of sodium diphenylaminesulfonate (C6H5NH
45、C6H4SO3Na) in a small volume of water and dilute to 100 ml. (Method 1 and Method 2).Store the solution in a brown glass bottle.5 ApparatusThe pipette and volumetric flask specified are complying with ISO 648 and ISO 1042 respectively.Ordinary laboratory apparatus, and the following. ISO 2015 All rig
46、hts reserved 3BS ISO 2597-2:2015ISO 2597-2:2015(E)5.1 Alumina, zirconium or vitreous carbon crucible, capacity 25 ml to 30 ml, crucibles should be cleaned before use to avoid contamination with iron.5.2 Burette, class A, complying with ISO 385.5.3 Weighing bottle, of approximate volume 10 ml and app
47、roximate mass 6 g.5.4 Platinum crucible, capacity 25 ml to 30 ml and having a lid.5.5 Weighing spatula, of a non-magnetic material or demagnetized stainless steel.5.6 Muffle furnace, suitable for operation in the range 500 C to 800 C.6 Sampling and samples6.1 Laboratory sampleFor analysis, use a lab
48、oratory sample of minus 100 m 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 less than 160 m.NOTE 1 A guideline on significant contents of combined water an
49、d oxidizable compounds is incorporated in ISO 7764.NOTE 2 If the determination of total iron relates to a reducibility test, prepare the laboratory sample by crushing and pulverizing, to less than 100 m particle size, the whole of one of the reducibility test portions which has been reserved for chemical analysis. In the case of ores having significant contents of combined water or oxidizable compounds, use a particle size of less than 160 m.6.2 Preparation of test samples6.2.1 GeneralDepending o
