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1、BRITISH STANDARD BS ISO 17053:2005 Steel and iron Determination of oxygen Infrared method after fusion under inert gas ICS 77.080.01 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 17053:2005 This British Standard was published unde
2、r the authority of the Standards Policy and Strategy Committee on 30 March 2005 BSI 30 March 2005 ISBN 0 580 45704 4 National foreword This British Standard reproduces verbatim ISO 17053:2005 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Tech
3、nical Committee ISE/18, Sampling and analysis of iron and steel, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this d
4、ocument may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contra
5、ct. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for
6、 change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 9 and a back cover. The BSI copyright noti
7、ce displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 17053:2005(E) OSI 5002 INTERNATIONAL ST
8、ANDARD ISO 17053 First edition 2005-02-01 Steel and iron Determination of oxygen Infrared method after fusion under inert gas Acier et fonte Dosage de loxygne Mthode par infrarouge aprs fusion sous gaz inerte BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00
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14、sed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:35071 O5002(E) I SO 5002 All irthgs ersedevr iii Contents Page Forewordiv 1 Scope1 2 Normative references .1 3 Principle.1 4 Reagents and materials1 5 Apparatus.3 6 Sampling3 7 Procedure.3 8 Expr
15、ession of results6 9 Test report7 Annex A (informative) Additional information on international cooperative test8 Annex B (informative) Graphical representation of precision data.9 BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c
16、) BSI IS:35071 O5002(E) iv I SO 5002 All irthgs ersedevr 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 out through ISO technical committee
17、s. 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 closely with the Inter
18、national Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International St
19、andards 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 casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the sub
20、ject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 17053 was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition. BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, M
21、on Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADR IS:35071 O5002(E) I SO 5002 All irthgs ersedevr 1 Steel and iron Determination of oxygen Infrared method after fusion under inert gas 1 Scope This International Standard specifies an infrared method after fusion und
22、er inert gas for the determination of oxygen in steel and iron. The method is applicable to mass fractions of oxygen between 0,000 75 % and 0,01 %. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition
23、 cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions ISO 5725-2:1994, Accuracy (trueness and precision
24、) 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 measures of the precision of a standard mea
25、surement method ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemical composition 3 Principle Fusion of a test portion in a single-use graphite crucible under helium gas at a minimum temperature of 2 000 C. Combination of the oxygen from the sample with
26、 carbon from the crucible to form carbon monoxide. Eventually, transformation of carbon monoxide into carbon dioxide. Measurement of infrared absorption of the carbon monoxide or dioxide, against a calibration curve made of potassium nitrate. 4 Reagents and materials 4.1 General During the analysis,
27、 unless otherwise stated, use only reagents of recognized analytical grade. 4.2 Helium, of high purity, total impurity content 0,000 5 % (mass 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 the pres
28、ence of organic contaminants is suspected in the helium. BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:35071 O5002(E) 2 I SO 5002 All irthgs ersedevr 4.3 Magnesium perchlorate, Mg (ClO4)2, (commercial designation: anhy
29、drone), particle size from 1,2 mm to 2,0 mm, or anhydrous calcium sulfate, (commercial designation: drierite), particle size from 0,6 mm to 0,85 mm. 4.4 Sodium hydroxide, on granulated support, (commercial designation: ascarite), particule size from 0,7 mm to 1,2 mm. 4.5 Copper oxide, CuO. 4.6 Tin o
30、r nickel capsules, for example diameter 5 mm, length 13 mm, mass 160 mg, with low mass fraction of oxygen, less than 0,1 g/mg of oxygen. Cut off the upper part of the tin capsule to reduce the mass to 50 mg or the length to 8 mm in order to remove the contaminated part. 4.7 Water of high purity, dei
31、onised, prepared just before use. 4.8 Potassium nitrate, KNO3, of high purity, maximum total impurity content 0,000 5 % by mass. Dry before use at 100C to 105C for 2 h, and allow to cool in a dessicator. 4.9 Potassium nitrate stock solution, corresponding to 4 mg/ml of oxygen. Weigh, to the nearest
32、0,1 mg, 8,416 g of potassium nitrate (4.8). Place in a 100 ml beaker and dissolve in about 50 ml of water (4.7). Transfer quantitatively to a 1 000 ml volumetric flask, dilute to the mark with water (4.7), and mix. 1 ml of the potassium nitrate stock solution contains 4 mg of oxygen as potassium nit
33、rate. 4.10 Potassium nitrate diluted stock solution, corresponding to 0,4 mg/ml of oxygen. This solution must be prepared freshly before use. Transfer 10 ml of the potassium nitrate stock solution to a 100 ml volumetric flask, dilute to the mark with water (4.7), and mix. 1 ml of the potassium nitra
34、te stock solution contains 0,4 mg of oxygen as potassium nitrate. 4.11 Potassium nitrate standard solutions These solutions must be prepared freshly before use. Transfer the volume listed in Table 1 of the potassium nitrate stock solution (4.9) and of the potassium nitrate diluted stock solution (4.
35、10) to a series of nine 100 ml volumetric flasks, dilute to the mark with water (4.7), and mix. 100 l of each of the potassium nitrate standard solutions contain the mass of oxygen (as potassium nitrate) listed in the last column of Table 1. 4.12 Graphite powder, of high purity, with low oxygen cont
36、ent. BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:35071 O5002(E) I SO 5002 All irthgs ersedevr 3 Table 1 Potassium nitrate standard solution Potassium nitrate standard solution Volume of potassium nitrate stock soluti
37、on (4.9) added (except for solution 4.11.2) Mass of oxygen in 1 ml of the potassium nitrate standard solution Mass of oxygen in 100 l of the potassium nitrate standard solution 4.11.1 0 ml a 0 mg 0 g 4.11.2 3 ml of potassium nitrate diluted stock solution (4.10) 0,012 mg 1,2 g 4.11.3 1,0 ml 0,04 mg
38、4 g 4.11.4 2,0 ml 0,08 mg 8 g 4.11.5 3,0 ml 0,12 mg 12 g 4.11.6 5,0 ml 0,20 mg 20 g 4.11.7 10,0 ml 0,40 mg 40 g 4.11.8 20,0 ml 0,80 mg 80 g 4.11.9 30,0 ml 1,20 mg 120 g a Zero member: The standard solution (4.11.1) is in fact the water (4.7) used for preparing the solutions. 5 Apparatus 5.1 General
39、The apparatus required for fusion of the test portion, and measurement of the carbon monoxide or dioxide extracted, may be obtained commercially from a number of manufacturers. Follow the manufacturers instructions for the operation of the instrument. 5.2 Graphite crucible, single-use. Use high-puri
40、ty crucibles suited to the apparatus. 5.3 Crucible tongs, for handling the crucibles used. 5.4 Glass-wool filters. 5.5 Micropipette, 100 l, the limit of error shall be less than 1 l. 6 Sampling Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel. 7 Procedure S
41、AFETY INSTRUCTIONS The risk involved when using an apparatus for fusing the test portion are mainly risks of burns. It is therefore necessary to use crucible tongs (5.3) and appropriate containers for the used crucibles. 7.1 General instructions Check that glass-wool filters (5.4) are clean and chan
42、ge them as often as necessary. BS ISO 17053:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:35071 O5002(E) 4 I SO 5002 All irthgs ersedevr If the electricity supply has been switched off for a long time, allow the instrument to stabi
43、lize for the time recommended by the manufacturer. After changing the filters (5.4) and/or reagents (4.3, 4.4 and 4.5), or when the apparatus has been inoperative for a period, stabilize the instrument by carrying out trial analyses, the results of which are to be disregarded. Then proceed with blan
44、k, calibration and preparation tests, as indicated in 7.3, 7.4 and 7.5, before analysing the sample. If the instrument used provides a direct reading in percentage of oxygen, adjust the instrument reading for each calibration range as follows. Read the content of a certified reference material (CRM)
45、 of high oxygen content at various steps of heating power. The required heating power for the determination of test samples is that at which the reading levels off. In order to determine a high-alloy test sample, a high-alloy CRM shall be used to know the required heating power. 7.2 Test portion Pre
46、pare the test portion of approximately 1 g in accordance with ISO 14284 or appropriate national standards for steel. Weigh the test portion to the nearest 1 mg. 7.3 Blank test Prior to the determination, carry out the following blank test in duplicate. Proceed as in 7.6 without the test portion, ent
47、ering a mass of 1 g, and setting the blank subtraction of the instrument to zero. Obtain the reading of the blank test. The mean value of the blank test shall be sufficiently low when compared to the mass fraction of oxygen to be determined in the test portion. For a mean value below 8 g/g of oxygen
48、, the mean blank value and the difference between the two blank values shall both not exceed 0,5 g/g of oxygen. For a mean value above 8 g/g of oxygen, the mean blank value and the difference between the two blank values shall both not exceed 2 g/g of oxygen. If the blank values are abnormally high,
49、 investigate and eliminate the source of contamination. If the mean value of the blank is satisfactory, it may then be introduced in the blank subtraction device of the instrument. 7.4 Calibration Prior to the determination, carry out the following calibration. Prepare, according to 4.11, at least five solutions chosen among solutions 4.11.1 to 4.11.9 indicated in Table 1, according to the level of mass fraction of oxygen to b