1、Direct reduced iron Determination of carbon and/or sulfur High-frequency combustion method with infrared measurement PD ISO/TR 9686:2017 BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017 Direct reduced iron Determination of carbon and/or sulfur High- frequen
2、cy combustion method with infrared measurement Minerais de fer prrduits Dosage du carbone et/ou du soufre Mthode par combustion haute frquence et mesurage par infrarouge TECHNICAL REPORT ISO/TR 9686 Reference number ISO/TR 9686:2017(E) First edition 2017-05 National foreword This Published Document
3、is the UK implementation of ISO/TR 9686:2017. It supersedes BS ISO 9686:2006, which is withdrawn. The UK participation in its 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 pu
4、blication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017 ISBN 978 0 580 97807 4 ICS 73.060.10 Compliance with a British Standard cannot confer im
5、munity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Committee on 31 July 2017. Amendments/corrigenda issued since publication Date Text affected PUBLISHED DOCUMENT PD ISO/TR 9686:2017 ISO 2017 Direct reduced iron Determination
6、 of carbon and/or sulfur High- frequency combustion method with infrared measurement Minerais de fer prrduits Dosage du carbone et/ou du soufre Mthode par combustion haute frquence et mesurage par infrarouge TECHNICAL REPORT ISO/TR 9686 Reference number ISO/TR 9686:2017(E) First edition 2017-05 PD I
7、SO/TR 9686:2017 ISO/TR 9686:2017(E)ii ISO 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Switzerland All 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 mechanica
8、l, 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 requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switz
9、erland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.org PD ISO/TR 9686:2017 ISO/TR 9686:2017(E)ii ISO 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be re
10、produced 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 reques
11、ter. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgISO/TR 9686:2017(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Principle 1 5 Reagents 1 6 Apparatus . 2
12、 7 Sampling and samples 3 7.1 Laboratory sample . 3 7.2 Preparation of predried test samples 3 8 Procedure. 3 8.1 General operating instructions . 3 8.2 Test portion 3 8.3 Blank test . 3 8.4 Calibration 4 8.4.1 Crucible preparation 4 8.4.2 Combustion 5 8.5 Determination . 5 9 Expression of results 5
13、 9.1 Calculation of mass fraction of carbon or sulfur 5 9.2 General treatment of results . 5 9.2.1 Repeatability and permissible tolerance 5 9.2.2 Determination of analytical result 6 9.2.3 Between-laboratories precision . 6 9.2.4 Check for trueness 7 9.2.5 Calculation of final result 8 10 Test repo
14、rt . 8 Annex A (informative) Crucible loading sequence . 9 Annex B (informative) Flowsheet of the procedure for the acceptance of analytical values for test samples .10 Annex C (informative) Features of commercial HF combustion/infrared sulfur analysers .11 Annex D (informative) Derivation of repeat
15、ability and permissible tolerance formulae .12 Annex E (informative) Precision data obtained by international analytical trials .13 Bibliography .15 ISO 2017 All rights reserved iii Contents Page PD ISO/TR 9686:2017 ISO/TR 9686:2017(E) Foreword ISO (the International Organization for Standardization
16、) 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 which a technical committee has been established has the right to be repr
17、esented 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 matters of electrotechnical standardization. The procedures used to dev
18、elop 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. This document was drafted in accordance with the editorial rules of the IS
19、O/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 or all such patent rights. Details of any patent rights identified dur
20、ing 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 users and does not constitute an endorsement. For an explanation on th
21、e 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 Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ forewo
22、rd .html. This document was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis. This first edition Technical Report cancels and replaces the second edition International Standard (ISO 9686:2006), which has been technically revised and h
23、as been converted to a Technical Report because it is not suitable for determination of carbon or sulfur as a referee method.iv ISO 2017 All rights reserved PD ISO/TR 9686:2017 ISO/TR 9686:2017(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national
24、 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
25、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. The procedures used to develop this document and those intended f
26、or 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. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso
27、.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 or all such patent rights. Details of any patent rights identified during the development of the document wil
28、l 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 users and does not constitute an endorsement. For an explanation on the voluntary nature of standards, the me
29、aning 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 Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html. This document was prepared by
30、 Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis. This first edition Technical Report cancels and replaces the second edition International Standard (ISO 9686:2006), which has been technically revised and has been converted to a Technical Report
31、 because it is not suitable for determination of carbon or sulfur as a referee method.iv ISO 2017 All rights reserved TECHNICAL REPORT ISO/TR 9686:2017(E) Direct reduced iron Determination of carbon and/or sulfur High-frequency combustion method with infrared measurement WARNING This document may in
32、volve 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 of the user of this document to establish appropriate health and safety practices. 1 Scope This document specifies a method for
33、the determination of the mass fraction of carbon and/or sulfur in direct reduced iron by infrared measurement after high-frequency combustion. This method is applicable to mass fractions of carbon between 0,05 % and 2,5 %, and/or mass fractions of sulfur between 0,001 % and 0,05 % in direct reduced
34、iron. 2 Normative references There are no normative references in this document. 3 T erms an d definiti ons No 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
35、p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp 4 Principle The test portion is combusted in a refractory crucible in a flow of oxygen in the presence of an accelerator, the crucible being inserted in the combustion tube of a high-frequency (HF)
36、furnace. The carbon present is converted into carbon dioxide and the sulfur into sulfur dioxide. Each gas is measured by infrared absorption, with calibration using barium carbonate and potassium sulfate. 5 Reagents During analysis, use only reagents of recognized analytical grade and only distilled
37、 water or water of equivalent purity. 5.1 Oxygen, minimum purity 99,5 % (mass fraction). The pressure in the furnace should be controlled by a pressure regulator designed especially for the purpose and complying with the manufacturers specification. 5.2 Magnesium perchlorate, grain size 0,7 mm to 1,
38、2 mm. ISO 2017 All rights reserved 1 PD ISO/TR 9686:2017 ISO/TR 9686:2017(E) 5.3 Accelerator, tungsten (granular form) with known low mass fractions of carbon (0,002 %) and sulfur (0,000 5 %). 5.4 Pure iron, or iron of known low mass fractions of carbon and sulfur, as in 5.3. 5.5 Tin capsules, of ca
39、pacity 0,3 ml, diameter 5 mm, length 17 mm. 5.6 Barium carbonate (BaCO 3 ), fine powder. Dry at 105 C for 3 h and cool in a desiccator. 5.7 Sulfur standard solutions. Dry potassium sulfate (K 2 SO 4 ) at 105 C for 1 h and cool in a desiccator. Weigh, to the nearest 0,000 2 g, the amounts of potassiu
40、m sulfate specified in Table 1. Transfer to five 100 ml one-mark volumetric flasks, dissolve with 50 ml of water, dilute to volume and mix. 5.8 Ascarite, used only for carbon determination. Table 1 Sulfur standard solutions Sulfur standard solution Mass of K 2 SO 4 Sulfur concentration g mg/ml SS 1
41、0,217 4 0,4 SS 2 0,434 8 0,8 SS 3 0,652 2 1,2 SS 4 0,869 6 1,6 SS 5 2,174 0 4,0 6 Apparatus Ordinary laboratory apparatus, including micropipettes and one-mark volumetric flasks complying with the specifications of ISO 7550 and ISO 1042, respectively, and the following. 6.1 Commercial carbon/sulfur
42、apparatus The apparatus required for HF combustion of the samples and the subsequent infrared absorption measurement of evolved carbon dioxide and/or sulfur dioxide may be obtained commercially from a number of manufacturers. Common features of such systems are discussed in Annex C. The manufacturer
43、s instruction for the operation of their equipment should be followed. 6.2 Ceramic combustion crucibles, required for containing the sample and any additions that may be necessary for the subsequent combustion. The crucibles should be of precise dimensions for the system, and should adapt to the sup
44、porting pedestal post, so that the sample in the crucible will be positioned at the correct height within the induction coil when it is in the raised position. These crucibles should be pre-ignited in an oxygen flow, in a furnace, for not less than 2 h at 1 350 C (or at 1 100 C if only sulfur is to
45、be determined), and then stored in a desiccator or closed container before use. For pre-ignition, a resistance furnace may be used.2 ISO 2017 All rights reserved PD ISO/TR 9686:2017 ISO/TR 9686:2017(E) 5.3 Accelerator, tungsten (granular form) with known low mass fractions of carbon (0,002 %) and su
46、lfur (0,000 5 %). 5.4 Pure iron, or iron of known low mass fractions of carbon and sulfur, as in 5.3. 5.5 Tin capsules, of capacity 0,3 ml, diameter 5 mm, length 17 mm. 5.6 Barium carbonate (BaCO 3 ), fine powder. Dry at 105 C for 3 h and cool in a desiccator. 5.7 Sulfur standard solutions. Dry pota
47、ssium sulfate (K 2 SO 4 ) at 105 C for 1 h and cool in a desiccator. Weigh, to the nearest 0,000 2 g, the amounts of potassium sulfate specified in Table 1. Transfer to five 100 ml one-mark volumetric flasks, dissolve with 50 ml of water, dilute to volume and mix. 5.8 Ascarite, used only for carbon
48、determination. Table 1 Sulfur standard solutions Sulfur standard solution Mass of K 2 SO 4 Sulfur concentration g mg/ml SS 1 0,217 4 0,4 SS 2 0,434 8 0,8 SS 3 0,652 2 1,2 SS 4 0,869 6 1,6 SS 5 2,174 0 4,0 6 Apparatus Ordinary laboratory apparatus, including micropipettes and one-mark volumetric flas
49、ks complying with the specifications of ISO 7550 and ISO 1042, respectively, and the following. 6.1 Commercial carbon/sulfur apparatus The apparatus required for HF combustion of the samples and the subsequent infrared absorption measurement of evolved carbon dioxide and/or sulfur dioxide may be obtained commercially from a number of manufacturers. Common features of such systems are discussed in Annex C. The manufacturers instruction for the operation of their equipment should be followed. 6.2 C
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