1、Cast irons Determination of non-combined carbon content lnfrared absorption method after combustion in an induction furnace PD ISO/TS 10719:2016 BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06National foreword This Published Document is the UK implementation of ISO
2、/TS 10719:2016. The UK participation in its preparation was entrusted to Technical Committee ISE/102, Methods of Chemical Analysis for Iron and Steel. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all t
3、he necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016 ISBN 978 0 580 90632 9 ICS 77.080.10 Compliance with a British Standard cannot confer immunity from legal obligations. This Publis
4、hed Document was published under the authority of the Standards Policy and Strategy Committee on 31 December 2016. Amendments/corrigenda issued since publication Date Text affected PUBLISHED DOCUMENT PD ISO/TS 10719:2016 ISO 2016 Cast irons Determination of non- combined carbon content lnfrared abso
5、rption method after combustion in an induction furnace Fontes Dtermination du carbone non combin Mthode par absorption dans linfrarouge aprs combustion dans un four induction TECHNICAL SPECIFICATION ISO/TS 10719 Reference number ISO/TS 10719:2016(E) First edition 2016-12-01 PD ISO/TS 10719:2016 ISO/
6、TS 10719:2016(E)ii ISO 2016 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2016, 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 mechanical, including photoc
7、opying, 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, Switzerland Tel. +41 22
8、749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.org PD ISO/TS 10719:2016 ISO/TS 10719:2016(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Principle 1 5 Reagents 2 6 Apparatus . 2 7 Sampling 3 8 Procedure. 3 8.1 General operating instructions . 3 8.2 Test po
9、rtion 4 8.3 Blank test . 4 8.4 Determination . 4 8.4.1 Dissolution of the test portion . 4 8.4.2 Filtration of the non-combined carbon 4 8.4.3 Measurements 4 8.5 Establishing the calibration curve 5 8.5.1 Primary product calibration 5 8.5.2 Calibration by means of certified reference materials 5 9 E
10、xpression of results 6 9.1 Primary product calibration 6 9.2 Calibration by means of certified reference materials . 6 10 Precision . 6 11 Notes on the procedure . 7 11.1 Preliminary blank tests . . 7 11.2 Preliminary tests on certified reference materials 7 12 Test report . 7 Annex A (informative)
11、Additional information on the international interlaboratory test8 Annex B (informative) C omparison betw een the r esults of the first and the sec ond precision tests 10 Annex C (informative) Effect of fine mat erial in a sample on the det ermination of non- combined carbon content 11 Bibliography .
12、14 ISO 2016 All rights reserved iii Contents Page PD ISO/TS 10719:2016 ISO/TS 10719:2016(E) Foreword ISO (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
13、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. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO
14、collaborates closely 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 a
15、pproval 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.org/directives). Attention is drawn to the possibility that some of the elements of this document may be t
16、he 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 will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). A
17、ny 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 meaning of ISO specific terms and expressions related to conformit y assessment, as well as information about ISOs adherence to the World Trade Orga
18、nization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html. The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition. This first edition Technical Specification re
19、places the first edition Technical Report (ISO/TR 10719:1994), which has been technically revised. The following changes have been made: steels have been deleted from the scope; the possibility to establish the calibration curve by means of certified reference materials has been added; assessment of
20、 the precision data has been revised.iv ISO 2016 All rights reserved PD ISO/TS 10719:2016 TECHNICAL SPECIFICATION ISO/TS 10719:2016(E) Cast irons Determination of non-combined carbon content lnfrared absorption method after combustion in an induction furnace 1 Scope This document specifies an infrar
21、ed absorption method after combustion in an induction furnace for the determination of non-combined carbon content in cast irons. The method is applicable to non-combined carbon contents between 1,0 % (mass fraction) and 3,0 % (mass fraction). Elements ordinarily present do not interfere. However, s
22、ome alloyed cast irons, when extensively heat treated, contain carbides that are not soluble when using this method and may give high values for non- combined carbon. 2 Normative references The following documents are referred to in the text in such a way that some or all of their content constitute
23、s 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 3696, Water for analytical laboratory use Specification and test methods ISO 14284, Steel and iron Samp
24、ling and preparation of samples for the determination of chemical composition 3 T erms a nd definiti ons For the purposes of this document, the following terms and definitions apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia
25、: available at http:/ /www.electropedia.org/ ISO Online browsing platform: available at http:/ /www.iso.org/obp 3.1 non-combined carbon graphitic carbon carbon that is not dissolved by methanol and nitric and hydrofluoric acids 4 Principle Decomposition of a test portion with nitric acid in the pres
26、ence of methanol and treatment with hydrofluoric acid. Removal of the non-combined carbon by filtering through a glass-fibre filter. Combustion of the glass-fibre filter containing the non-combined carbon in a flow of oxygen at a high temperature, using a high-frequency induction furnace, in the pre
27、sence of pure iron and an accelerator. Transformation of carbon into carbon dioxide and/or carbon monoxide. Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide, carried by the current of oxygen. ISO 2016 All rights reserved 1 PD ISO/TS 10719:2016 ISO/TS 10719:2016(E) 5 Re
28、agents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only water with a low content of organic matter, i.e. grade 2 or grade 1 water as specified in ISO 3696. 5.1 Water, free from carbon dioxide. Boil water for 30 min, cool to room temperature and
29、allow oxygen (5.2) to bubble through it for 15 min. Prepare just before use. 5.2 Oxygen, minimum purity 99,5 % (volume fraction). An oxidation catalyst copper(II) oxide or platinum tube heated to a temperature above 450 C shall be used prior to a purifying unit, when oxygen is suspected for the pres
30、ence of organic contaminants. 5.3 Iron, containing less than 0,001 0 % of carbon (mass fraction). 5.4 Solvent, appropriate for cleaning greasy or dirty test samples, for example, acetone. 5.5 Methanol, minimum purity 99,5 % (volume fraction). 5.6 Barium carbonate. Dry barium carbonate minimum purity
31、 99,5 % (mass fraction) at 105 C to 110 C for 3 h and cool in a desiccator before use. 5.7 Cast ir on c ertified r efer enc e mat erials (CRMs), containing 1 % to 3 % (mass fraction) carbon. The cast irons to be used for this purpose shall have white structure. 5.8 Accelerator. Copper, tungsten-tin
32、mixture or tungsten containing less than 0,001 0 % carbon (mass fraction). 5.9 Nitric acid, about 1,40 g/ml. 5.10 Hy dr ofluoric acid, about 1,15 g/ml. 5.11 Hydrochloric acid, about 1,19 g/ml, diluted 1 + 1. 5.12 Sodium hydroxide, 120 g/l solution. Cautiously dissolve 60 g of sodium hydroxide in abo
33、ut 200 ml of water (5.1). When dissolution is complete, cool, dilute to 500 ml with water, mix and store in a plastic bottle. 5.13 Magnesium perchlorate Mg(ClO 4 ) 2 , particle size from 0,7 mm to 1,2 mm. 5.14 Inert ceramic (attapulgus clay), impregnated with sodium hydroxide, particle size from 0,7
34、 mm to 1,2 mm. 6 Apparatus The apparatus required for combustion in a high frequency induction furnace and the subsequent infrared absorption measurement of the evolved carbon dioxide and/or carbon monoxide may be obtained commercially from a number of manufacturers. Follow the manufacturers instruc
35、tions for 2 ISO 2016 All rights reserved PD ISO/TS 10719:2016 ISO/TS 10719:2016(E) the operation of the instrument. A pressure regulator is required to control the oxygen pressure to the furnace according to the manufacturers specification. Ordinary laboratory apparatus and the following shall be us
36、ed. 6.1 Filter, made of glass fibre, 47 mm in diameter, pore size 0,3 m. 6.2 V acuum filt ering appar atus, for use with 47 mm glass-fibre filters (6.1) and suitable for use with acids. 6.3 Ceramic crucible, capable of withstanding combustion in an induction furnace. Ignite crucibles in an electric
37、furnace in air or in a current of oxygen, for not less than 2 h at 1 100 C, and store in a desiccator before use. 7 Sampling Sampling shall be carried out in accordance with ISO 14284 or with an appropriate national standard for cast irons (see Annex C). NOTE For cast irons, use drillings with lengt
38、hs of more than 2 mm. For spheroidal graphite cast irons, use solid portions, approximately 10 mm x 10 mm x 0,3 mm. 8 Procedure SAFETY INSTRUCTIONS The risks related to combustion analysis are mainly burns in pre-igniting the ceramic crucibles and in the fusions. Use crucible tongs at all times and
39、suitable containers for the used crucibles. Normal precautions for handling oxygen cylinders shall be taken. Oxygen from the combustion process shall be removed effectively from the apparatus, since a high concentration of oxygen in a c o n f i n e d s p a c e c a n p r e s e n t a f i r e h a z a r
40、 d . Take care not to mix methanol with concentrated nitric acid because of the risk of explosion. 8.1 General operating instructions Purify the oxygen supply (5.2) using tubes packed with the inert ceramic (5.14) impregnated with sodium hydroxide (5.12) and magnesium perchlorate (5.13), and maintai
41、n a quiescent flow rate while on standby. Maintain a glass-fibre filter or a stainless steel filter screen as a dust collector. Clean and change as necessary. The furnace chamber, pedestal post and filter trap shall be cleaned frequently to remove oxide build-up. When the main supply is switched on
42、after being out of action for any length of time, allow the equipment to stabilize for the time recommended by the equipment manufacturers. After cleaning the furnace chamber and/or changing filters, or after the equipment has been inoperative for a period, stabilize the apparatus by burning several
43、 samples, of similar type to the samples to be analysed, prior to setting up for analysis. Flush oxygen through the apparatus and adjust the instrument controls to give a zero reading. If the instrument used provides a direct reading in percentage of carbon, adjust the instrument reading for the cal
44、ibration range as follows. Select a cast iron certified reference material with a carbon content close to the maximum carbon content in the calibration series, measure the corresponding carbon content in accordance with the manufacturers instructions and adjust the reading of the instrument to the c
45、ertified value. ISO 2016 All rights reserved 3 PD ISO/TS 10719:2016 ISO/TS 10719:2016(E) 8.2 Test portion If necessary, degrease the test sample by cleaning in a suitable solvent (5.4). Cautiously evaporate the last traces of the solvent by warming. Weigh, to the nearest 1 mg, approximately 0,50 g o
46、f the test sample. 8.3 Blank test In parallel with the determination and following the same procedure, carry out two blank tests using the same quantities of all the reagents, including the same quantity of the pure iron (5.3) as used for the test portion (8.2). Obtain the reading of the blank tests
47、 and convert it to milligrams of carbon by means of the calibration curve (see 8.5). The mean blank value (m 1 ) is calculated from the two blank values. The mean blank value and the difference between the two blank values shall both not exceed 0,15 mg of carbon. If these values are abnormally high,
48、 investigate and eliminate the source of contamination. 8.4 Determination 8.4.1 Dissolution of the test portion Place the test portion (8.2) in a 250 ml beaker. Add 25 ml of methanol (5.5), 50 ml of water (5.1) and 5 ml of nitric acid (5.9). Immediately cover the beaker with a watch glass and allow
49、to stand for 12 h to 16 h at room temperature. Add 20 ml of nitric acid (5.9) and allow to stand until further reaction ceases. Place the beaker on a hot plate heated between 50 C and 60 C. When vigorous reaction ceases, add 4 drops to 5 drops of hydrofluoric acid (5.10). Continue heating until dissolution is completed. If necessary, add water (5.1) to maintain the original volume. 8.4.2 Filtration of the non-combined carbon Place two glass-fibre filters (6.1) in a vacuum filtering apparatus (6.2)
