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1、INTERNATIONAL STANDARD ISO 15353 First edition 2001-03-15 Reference number ISO 15353:2001(E) ISO 2001 Steel and iron Determination of tin content Flame atomic absorption spectrometric method (extraction as Sn-SCN) Aciers et fontes Dosage de ltain Mthode par spectromtrie dabsorption atomique dans la
2、flamme (extraction comme Sn-SCN) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15353:2001
3、(E) ii ISO 2001 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the
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6、t at the address given below. ISO 2001 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, elec- tronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the addres
7、s below or ISOs mem- ber body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland Copyright International Organization for Standardization Provided by IHS und
8、er license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15353:2001(E) ISO 2001 All rights reserved iii ContentsPage 1Scope .1 2Normative references .1 3Principle 1 4Reagents 1
9、 5Apparatus .3 6Sampling .3 7Procedure .4 8Plotting the calibration graph 6 9Expression of results 6 10Test report 7 Annexes AAdditional information on the international co-operative test 8 BGraphical representation of precision data .9 Copyright International Organization for Standardization Provid
10、ed by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15353:2001(E) iv ISO 2001 All rights reserved Foreword ISO (the International Organization for Standardiza
11、tion) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical com- mittees. Each member body interested in a subject for which a technical committee has been established has the right to b
12、e represented on that committee. International organizations, governmental and non-governmental, in liai- son with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Stan
13、dards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies c
14、asting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 15353 was prepared by Technical Committee ISO
15、/TC 17,Steel, Subcommittee SC 1, Methods of determination of chemical composition. Annexes A and B of this International Standard are for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 N
16、ot for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 15353:2001(E) ISO 2001 All rights reserved 1 Steel and iron Determination of tin content Flame atomic absorption spectrometric method (extraction as Sn-SCN) 1Scope T
17、his International Standard specifies a method for the determination of tin in steel and iron by means of flame atomic absorption spectrometry. The method is applicable to tin contents in the rangeby mass toby mass. 2Normative references The following normative documents contain provisions which, thr
18、ough reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publica- tions do not apply. However, parties to agreements based on this International Standard are encouraged to investi- gate the possib
19、ility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain reg- isters of currently valid International Standards. ISO 648:1977,Laboratory glassware O
20、ne-mark pipettes. ISO 1042:1998,Laboratory glassware One-mark volumetric flasks. ISO 3696:1987,Water for analytical laboratory use Specification and test methods. ISO 5725-1:1994,Accuracy (trueness and precision) of measurement methods and results Part 1: General prin- ciples and definitions. ISO 57
21、25-2:1994,Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. ISO 5725-3:1994,Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate m
22、easures of the precision of a standard measurement method. ISO 14284:1996,Steel and iron Sampling and preparation of samples for the determination of chemical composi- tion. 3Principle Dissolution of a test portion in hydrochloric and nitric acids. Formation of Sn-SCN complex and extraction of the c
23、om- plex into 4-methyl-2-pentanone (isobutyl methyl ketone). Aspiration of the organic solution into a dinitrogen monoxide-acetylene flame. Spectrometric measurement of the atomic absorption of thespectral line emitted by a tin hollow cathode lamp. High purity tin metal dissolved as standard solutio
24、n is used as reference material for calibration graphs. 4Reagents Use only reagents of recognized analytical grade, unless otherwise stated. 4.1Water, complying with grade 2 as defined in ISO 3696. 0,001 %0,1 % 224,6 nm Copyright International Organization for Standardization Provided by IHS under l
25、icense with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15353:2001(E) 2 ISO 2001 All rights reserved 4.2Hydrochloric acid, HCl,approximately. 4.3Hydrochloric acid, HCl, diluted. 4
26、.4Nitric acid, HNO3,approximately. 4.5Formic acid, HCOOH,approximately. 4.6Hydrochloric acid, HCl, diluted. 4.7Ascorbic acid, C6H8O6. 4.8Potassium thiocyanate solution. Dissolveof potassium thiocyanate (KSCN) in water (4.1), dilute toand mix. Prepare the solution shortly before use. 4.94-methyl-2-pe
27、ntanone (isobutyl methyl ketone), (CH3)2CHCH2COCH3. 4.10Washing solution. Dissolveof ascorbic acid (4.7) andof potassium thiocyanate inof hydrochloric acid (4.6). Prepare the solution shortly before use. 4.11Tin, standard reference solution. 4.11.1Stock solution, corresponding toof tin per litre. We
28、igh, to the nearest, approximatelyof tin metal (minimumby mass). Transfer to a beaker and dissolve inof hydrochloric acid (4.2) andof nitric acid (4.4). Warm gently. Remove from the hot plate immediately after complete dissolution and allow to cool. Transfer the solution to aone-mark volumetric flas
29、k containinghydrochloric acid (4.2). Dilute to the mark with water and mix. of this stock solution containsof tin. 4.11.2Standard reference solution A, corresponding toof tin per litre. Transferof the stock solution (4.11.1) to aone-mark volumetric flask and addof hydrochloric acid (4.2). Dilute to
30、the mark with water and mix. of this solution containsof tin. 4.11.3Standard solution B, corresponding toof tin per litre. Transferof the standard solution A (4.11.2) to aone-mark volumetric flask and addof hydrochlo- ric acid (4.2). Dilute to the mark with water and mix. of this solution containsof
31、 tin. 4.12Iron, free from tin (less thanby mass). 4.13Solution for optimization of the atomic absorption spectrometer. Dissolveof ascorbic acid (4.7) inof HCl (4.6). Allow to cool and addof the standard stock solution (4.11.1). Proceed exactly as specified in 7.3.2 but transfer the organic phase to
32、avolumetric flask, dilute with 4-methyl-2-pentanone (4.9) to the mark and mix. The solution is stable for several weeks if the flask is properly closed. 1,19 g/ml 1+1 1,40 g/ml 1,21 g/ml 1+24 25 g50 ml 45 g25 g500 ml 1 g 0,000 1 mg0,25 g99,9 %250 ml 20 ml5 ml 250 ml 100 ml 1 ml1 mg 50 mg 25 ml500 ml
33、90 ml 1 ml0,05 mg 5 mg 25 ml250 ml50 ml 1 ml0,005 mg 0,000 1 % 4 g40 ml3 ml 100 ml Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:49:58 MDTNo reproduction or networking permi
34、tted without license from IHS -,-,- ISO 15353:2001(E) ISO 2001 All rights reserved 3 5Apparatus All volumetric glassware shall be grade A, in accordance with ISO 648 or ISO 1042, as appropriate. Use ordinary laboratory apparatus. 5.1Atomic absorption spectrometer, consisting of a tin hollow cathode
35、lamp fuelled by supplies of acetylene and dinitrogen monoxide sufficiently pure to give a steady, clear, red-feather flame, free from water and oil. The atomic absorption spectrometer used is deemed satisfactory if, after optimization according to 7.3.5, the limit of detection and characteristic con
36、centration are in reasonable agreement with the values given by the manufacturer and if it meets the precision criteria given in 5.1.1 to 5.1.3. It is also desirable that the instrument conform to the ad- ditional performance requirement given in 5.1.4. 5.1.1Short term stability The standard deviati
37、on of ten measurements of the absorbance of the most concentrated calibration solution shall not exceedof the mean absorbance of the same solution. 5.1.2Limit of detection This is determined by taking three times the standard deviation of ten measurements of the absorbance of a solution containing t
38、he appropriate element at a concentration level selected to give an absorbance just above that of the zero member. The limit of detection of tin in a matrix similar to the final test portion solution shall be better than of tin in organic solution. 5.1.3Graph linearity The slope of the calibration g
39、raph covering the topof the concentration range (expressed as a change in ab- sorbancy) shall be not less than 0,7 times the value of the slope for the bottomof the concentration range de- termined in the same way. For instruments with automatic calibration using two or more standards, it shall be e
40、stablished prior to the analysis, by obtaining absorbance readings, that the above requirements for graph linearity are fulfilled. 5.1.4Characteristic concentration The characteristic concentration for tin in a matrix similar to the final test portion solution shall be better than of tin in organic
41、solution. 5.2Ancillary equipment, consisting of a strip chart recorder and/or digital readout device recommended to evalu- ate the criteria listed for 5.1 and for all subsequent measurements. Scale expansion can be used until the noise observed is greater than the readout error and is always recomme
42、nded for absorbances below 0,1. If scale expansion has to be used and the instrument does not have the means to read the value of the scale expansion factor, the value can be calculated by measuring a suitable solution with and without scale expansion and simply dividing the signal obtained. 6Sampli
43、ng Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel. 1,5 % 0,1g/ml 20 % 20 % 0,4g/ml Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08
44、:49:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15353:2001(E) 4 ISO 2001 All rights reserved 7Procedure 7.1Test portion Weigh, to the nearest, a test portion of the sample according to Table 1. 7.2Blank test In parallel with the determination and following the sa
45、me procedure, carry out a blank test using the same quantities of all the reagents but omitting the test portion. 7.3Determination 7.3.1Preparation of the test solution Place the test portion (see 7.1) in abeaker. Addof hydrochloric acid (4.3) andof nitric acid (4.4) then cover the beaker. Heat gent
46、ly. After complete dissolution, immediately remove the beaker from the hot plate and allow to cool. Rinse the lid with water and addof formic acid (4.5). Heat gently (without lid) until the reaction has ceased, then immediately remove the beaker from the hot plate. Dilute withof hydrochloric acid (4
47、.6). Addof ascorbic acid (4.7) and dissolve by gentle heating. Remove immediately from the hot plate and cool to am- bient temperature. 7.3.2Extraction Transfer the sample solution quantitatively to aseparating funnel and dilute with hydrochloric acid (4.6) to . Addpotassium thiocyanate solution (4.
48、8) and4-methyl-2-pentanone (4.9). Shake vigorously for . Let the phases separate completely. This normally takes approximately, but in the case of samples containing graphite, or elements that precipitate, it may take up toto. Discard the lower aqueous phase. Addof washing solution (4.10). Shake vigorously for. Let the phases separate completely. Discard the lower aqueous phase. It is not necessary to separate the organic phase quantitatively. Discard approximately of this together with the aqueous phase. Make sure t