1、BRITISH STANDARD BS ISO 17053:2005 Steel and iron Determination of oxygen Infrared method after fusion under inert gas ICS 77.080.01 BS ISO 17053:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 March 2005 BSI 30 March 2005 ISBN 0 580
2、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 Technical Committee ISE/18, Sampling and analysis of iron and steel, which has the responsibility to: A list of o
3、rganizations 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 document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence
4、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 contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself
5、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 change, and keep the UK interests informed; monitor related international and European developments and prom
6、ulgate 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 notice displayed in this document indicates when the document was last issued. Amendments issued since publicatio
7、n Amd. No. Date Comments Reference number ISO 17053:2005(E) OSI 5002INTERNATIONAL STANDARD 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 BSISO17
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13、gs ersedevr iiiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Principle . 1 4 Reagents and materials 1 5 Apparatus. 3 6 Sampling 3 7 Procedure. 3 8 Expression of results 6 9 Test report 7 Annex A (informative) Additional information on international cooperative test 8 Annex B (info
14、rmative) Graphical representation of precision data. 9 BSISO17053:2005IS:35071 O5002(E) iv I SO 5002 All irthgs ersedevrForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International St
15、andards 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. International organizations, governmental and non-governmental, in liaison with ISO, also
16、 take part in the work. ISO collaborates closely with the International 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 committee
17、s is to prepare International Standards. 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 casting a vote. Attention is drawn to the possib
18、ility 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. ISO 17053 was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition.
19、BSISO17053:2005INTENRATIONAL TSANDADR IS:35071 O5002(E)I SO 5002 All irthgs ersedevr 1Steel and iron Determination of oxygen Infrared method after fusion under inert gas 1 Scope This International Standard specifies an infrared method after fusion under inert gas for the determination of oxygen in s
20、teel 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 cited applies. For undated references, the lates
21、t 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) of measurement methods and results Part 2: Basi
22、c 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 measurement method ISO 14284:1996, Steel and iron Sa
23、mpling 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 carbon from the crucible to form carbon monoxide
24、. 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, unless otherwise stated, use only reagents of re
25、cognized 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 presence of organic contaminants is suspected in the
26、helium. BSISO17053:2005IS:35071 O5002(E) 2 I SO 5002 All irthgs ersedevr4.3 Magnesium perchlorate, Mg (ClO 4 ) 2 , (commercial designation: anhydrone), 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 Sod
27、ium 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 or 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 p
28、art 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, deionised, prepared just before use. 4.8 Potassium nitrate, KNO 3 , of high purity, maximum total impurity content 0,000 5 % by mass. Dry before use at 100C to
29、 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 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 vol
30、umetric 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 nitrate. 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
31、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 nitrate stock solution contains 0,4 mg of oxygen as potassium nitrate. 4.11 Potassium nitrate standard solutions These solutions must be prepared freshly befor
32、e use. Transfer the volume listed in Table 1 of the potassium nitrate stock solution (4.9) and of the potassium nitrate diluted stock solution (4.10) 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
33、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 content. BSISO17053:2005IS:35071 O5002(E) I SO 5002 All irthgs ersedevr 3Table 1 Potassium nitrate standard solution Potassium nitrate standard solution Volum
34、e of potassium nitrate stock solution (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 a0 mg 0 g 4.11.2 3 ml of potassium nitrate diluted stock solution (4.10) 0,0
35、12 mg 1,2 g 4.11.3 1,0 ml 0,04 mg 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 aZero member: The standard solution (4.11.1) is in fact the water (4.7) used for preparing the so
36、lutions. 5 Apparatus 5.1 General 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 cr
37、ucible, single-use. Use high-purity 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 s
38、tandards for steel. 7 Procedure SAFETY 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
39、 filters (5.4) are clean and change them as often as necessary. BSISO17053:2005IS:35071 O5002(E) 4 I SO 5002 All irthgs ersedevrIf the electricity supply has been switched off for a long time, allow the instrument to stabilize for the time recommended by the manufacturer. After changing the filters
40、(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 blank, calibration and preparation tests, as indicated in 7.3, 7.4 and 7.5, before
41、 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) of high oxygen content at various steps of heating power. The required heatin
42、g 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 Prepare the test portion of approximately 1 g in accordance with ISO 14284 or app
43、ropriate 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, entering a mass of 1 g, and setting the blank subtraction of the instrument to ze
44、ro. 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, the mean blank value and the difference between the two blank values shall b
45、oth 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, investigate and eliminate the source of contamination. If the mean value of t
46、he 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, ac
47、cording to the level of mass fraction of oxygen to be determined. Using the micropipette (5.5), transfer 100 l of each of the freshly prepared potassium nitrate standard solutions (4.11.1 to 4.11.9) to each tin or nickel capsule (4.6), respectively, and dry at 90 C to 95 C for 2 h. The drying of the
48、 calibration solutions in the tin or nickel capsules shall be done stepwise, in order to avoid splashing and loss of calibration material due to excessive heating before complete vaporisation of the water. BSISO17053:2005IS:35071 O5002(E) I SO 5002 All irthgs ersedevr 5Gently press the tin or nickel
49、 capsule and proceed as in 7.6, using the tin or nickel capsule as a test portion, entering a sample mass of one gram, and setting the sample fusion temperature to 2 000 C to limit tin vaporization. Prepare a calibration graph by plotting the reading obtained from the instrument against micrograms of oxygen from the last column of Table 1. 7.5 Preparation test Prior to the determination, carry out the
