《ISO-TR-15349-1-1998.pdf》由会员分享，可在线阅读，更多相关《ISO-TR-15349-1-1998.pdf（20页珍藏版）》请在三一文库上搜索。
1、TECHNICAL REPORT ISO/TR 15349-l First edition 1998-10-15 Unalloyed steel - Determination of low carbon content - Part 1: Infrared absorption method after combustion in an electric resistance furnace (by peak separation) Acier non al/i6 - Dktermination des faibles teneurs en carbone - Partie 1: M - t
2、ype 2, when the subject is still under technical development or where for any other reason there is the future but not immediate possibility of an agreement on an International Standard; - type 3, when a technical committee has collected data of a different kind from that which is normally published
3、 as an International Standard (“state of the art”, for example). Technical Reports of types 1 and 2 are subject to review within three years of publication, to decide whether they can be transformed into International Standards. Technical Reports of type 3 do not necessarily have to be reviewed unti
4、l the data they provide are considered to be no longer valid or useful. ISO/TR 15349-1, which is a Technical Report of type 2, was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition. This document is being issued in the Technical Rep
5、ort (type 2) series of publications (according to subclause G.3.2.2 of part 1 of the lSO/IEC Directives, 1995) as a “prospective standard for provisional application” in the field of determination of carbon content in steel because there is an urgent need for guidance on how standards in this field
6、should be used to meet an identified need. This document is not to be regarded as an “International Standard”. It is proposed for provisional application so that information and experience of its use in practice may be gathered. Comments on the content of those documents should be sent to the IS0 Ce
7、ntral Secretariat. A review of this Technical Report (type 2) will be carried out not later than three years after its publication with the options of: extension for another three years; conversion into an International Standard; or withdrawal. ISOmR 15349 consists of the following parts, under the
8、general title Unalloyed steel - Determination of low carbon content: - Part I: Infrared absorption method after combustion in an electric resistance furnace (by peak separation) - Par? 2: Infrared absorption method after combustion in an induction furnace (with preheating) Part 3: Infrared absorptio
9、n method after combustion in an electric resistance furnace (with preheating) Annexes A to C of this part of lSO/TR 15349 are for information only. . . . III Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001
10、 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted without license from IHS -,-,- This page intentionally left blank Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Res
11、ale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted without license from IHS -,-,- TECHNICAL REPORT o IS0 ISO/rR 15349-l :1998(E) Unalloyed steel - Determination of low carbon content - Part 1: Infrared absorption method after combustion in an electric resistance furnace (by peak sep
12、aration) 1 Scope This part of IS0 15349 describes an infrared absorption method with peak separation procedure after combustion in an electric resistance furnace for the determination of the low carbon content in unalloyed steel. The method is applicable to carbon contents between 0,000 3 % (m/m) an
13、d 0,010 % (m/m). 2 Normative references The following standards contain provisions which, through references in this text, constitute provisions of this part of IS0 15349. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements
14、based on this part of IS0 15349 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 1042:1998, Laboratory glassware - One-mark volumetric f/asks.
15、 IS0 3696:1987, Water for analytical laboratory use - Specification and test methods. IS0 5725-l :I 994, Accuracy (trueness and precision) of measurement methods and results - Part 1: Genera principles and definitions. IS0 5725-211994, Accuracy (trueness and precision) of measurement methods and res
16、ults - Par? 2: Basic methoc for the determination of repeatability and reproducibility of a standard measurement method. IS0 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results - Part 3: Intermediate measures of the precision of a standard measurement method. IS0 14284:
17、1996, Steel and iron - Sampling and preparation of samples for the determination of chemical composition. IS0 15349-2:- I) Unalloyed steel - , Determination of low carbon content - Part2: Infrared absorption method after combustion in an induction furnace (with preheating). 3 Principle Combustion of
18、 a test portion with accelerator at a high temperature in an electric resistance furnace in a current of pure oxygen. Transformation of carbon into carbon dioxide and/or carbon monoxide. Measurement, by peak separation process, of infrared absorption of the carbon dioxide and carbon monoxide evolved
19、 from steel and carried by a current of pure oxygen. I) To be published. 1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted wit
20、hout license from IHS -,-,- ISO/TR 15349-l : 1998(E) 0 IS0 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 3 water as specified in IS0 3696. 4.1 Water, free from carbon dioxide. Boil water for 30 min, cool to room temperature a
21、nd bubble with oxygen (4.2) for 15 min. Prepare just before use. 4.2 Oxygen, 9995 % (m/m) minimum. An oxidation catalyst copper(ll)o or platinum tube heated to a temperature above 450 “C must be used prior to a purifying unit, when the presence in the oxygen of organic contaminants is suspected. 4.3
22、 Suitable solvent, appropriate for washing greasy or dirty test samples; e.g. acetone. 4.4 Accelerator, copper plate(see note 1) or granular tin (see note 2) of known very low carbon content less than 0,000 1 % (m/m). NOTE 1 Copper plate (about 0,l g/plate) should be used after the following treatme
23、nt: heat the copper plate at 450 OC to 600 “C for IO min in a current of oxygen and cool in a desiccator without grease. This treatment shall be carried out just before use. NOTE 2 Granular tin should be used after the following treatment: rinse the granular tin in hydrochloric acid (p about 1 ,I 9
24、g/ml, diluted 1 + 1) for 5 min using an ultrasonic wave washer, wash it thoroughly with water and dry. Stock it in a clean glass bottle with ground-in stopper. 4.5 Standard substances 4.5.1 Sucrose, standard solution Weigh, to the nearest 0,l mg, the masses of sucrose, indicated in table 1, (analyti
25、cal standard grade) previously dried at 100 OC to 105 “C for 2,5 h then cooled in a desiccator and transfer to seven 100 ml beakers. Add 30 ml of water (4.1) to dissolve, transfer to seven 100 ml one-mark volumetric flasks quantitatively, dilute to the mark with water (4.1) and mix. 4.52 Calcium car
26、bonate Dry calcium carbonate minimum assay 99,9 % (m/m) at 180 OC for 1 h and cool in a desiccator before use. 4.6 Magnesium perchlorate Mg(CIO,), particle size: from 0,7 mm to I,2 mm. 4.7 Inert ceramic (attapulgus clay) impregnated with sodium hydroxide, particle size: from 0,7 mm to I,2 mm. Table
27、1 - Standard solution series of sucrose Standard solution reference number 1 2 3 4 5 6 7 1) Zero member. Mass of sucrose g 0 ) 0,010 0 0,025 0 0,060 0 0,120 0 0,180 0 0,240 0 Corresponding mass Carbon content in 1 g of carbon added of the test portion ICI % (m/m) 0 0 4,21 0,000 42 IO,53 0,001 05 25,
28、26 0,002 53 50,53 0,005 05 75,79 0,007 58 101,l 0,010 11 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted without license from
29、IHS -,-,- 0 IS0 ISO/TR 15349-l :1998(E) 5 Apparatus During the analysis, unless otherwise stated, use only ordinary laboratory apparatus. All laboratory glassware shall be class A, in accordance with IS0 1042 as appropriate. The apparatus required for combustion in an electric resistance furnace and
30、 subsequent infrared absorption measurement with peak separation procedure of the evolved carbon dioxide and/or carbon monoxide from steel may be obtained commercially, for example, Trace carbon analyser Model EMIA - U610, HORIBA, LTD*). Follow the manufacturers instructions for the operation of the
31、 instrument. 5.1 Ceramic boat, 80 mm x 13,5 mm X 10 mm Ignite a ceramic boat in an electric store in a desiccator withou t grease resistance fu mace in a current of oxygen for not less than 2 h at 1 200 OC and Just before use, ignite the ceramic boat at 1 300 OC for several minutes and use the hot b
32、oat. 5.2 Quartz boat, 30 mm x 9 mm x 8 mm Rinse a quartz boat in the washing solution mix nine volumes of nitric acid (p about I,40 g/ml, diluted 1 + 6) and one volume of hydrogen peroxide (30 % V/V) for 2 h to 3 h, wash it thoroughly with water and dry. Stock in a desiccator without grease. Just be
33、fore use, place the quartz boat on the ceramic boat, ignite it at 1 200 “C for IO min and cool in a desiccator without grease. 5.3 Micropipette, 100 1, limit of error shall be less than 1 1. 6 Sampling and preparation of the test samples Sampling and preparation of the samples shall be carried out i
34、n accordance with IS0 14284. Prepare the chip size of test sample between 0,75 mm and 2,0 mm. 7 Procedure SAFETY INSTRUCTIONS - The risks related to combustion analysis are mainly burns in pre-igniting the ceramic boats and in the combustion. Use boat tongs at all times and suitable containers for t
35、he used boats. Normal precautions for handling oxygen cylinders shall be taken. Oxygen from the combustion process shall be effectively removed from the apparatus since a high concentration of oxygen in a confined space can present a fire hazard. 7.1 Preparation of the apparatus Raise the temperatur
36、e of the combustion furnace to 1 300 “C. After having verified the highest temperature (more than 1 200 “C) at the centre of the heating zone in the combustion tube by use of a thermocouple, measure the distance, L, from the inlet of combustion tube to the centre of the heating zone in millimetres.
37、Prepare two rigid nickel bars. Fix the stopper of a rigid nickel bar, A at the point *) Model EMIA - U610, HORIBA is the tradename of a product supplied by HORIBA LTD. This information is given for the convenience of users of this part of ISO/TR 15349 and does not constitue an endorsement by IS0 of
38、the product named. Equivalent products may be used if they can be shown to lead to the same results. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction o
39、r networking permitted without license from IHS -,-,- ISO/rR 15349=1:1998(E) 0 IS0 where L = (the length of the ceramic boat used)/2 (mm) distance from the bar end. This is used to set the ceramic boat containing the test portion or calcium carbonate (see note below and figure 1). NOTE 1 e.g., for m
40、odel EMIA - lJ610, L is 290 mm and boat length is 80 mm. In this case the stopper is 250 mm distant from the bar end. Fix the stopper of another rigid nickel bar, B at the point where L = the length of the ceramic boat used (mm) distance from the bar end. This is used to set the ceramic boat contain
41、ing sucrose (see note below and figure 1). NOTE 2 e.g., for model EMIA - tJ610, L is 290 mm and boat length is 80 mm. In this case the stopper is 210 mm distant from the bar end. 6 7 Key: 1 Heating zone 2 Thermocouple 3 Combustion tube 4 Oxygen 5 Lmm 6 Stopper A 7 Rigid nickel bar A 8 Rigid nickel b
42、ar B 9 Evolved gases carried by oxygen to measuring system 10 Stopper B 11 L - (length of ceramic boat) /2 mm 12 Ceramic boat (test portion or calcium carbonate) 13 Ceramic boat containing quartz boat (sucrose) 14 L - (length of ceramic boat) mm Figure 1 - Combustion furnace Purify the oxygen supply
43、 using tubes packed with the inert ceramic (4.7) (attapulgus clay) impregnated with sodium hydroxide and magnesium perchlorate (4.6), and maintain a quiescent flowrate whilst on standby. Maintain a glass wool filter. Clean and charge as necessary. When the main supply is switched on after being out
44、of action for any length of time, allow each item of equipment to stabilize for the time recommended by the equipment manufacturers. After changing filters or after the equipment has been inoperative for a period, stabilize the apparatus by burning several samples of similar type to the samples to b
45、e analysed prior to setting up for analysis. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted without license from IHS -,-,- Fl
46、ush oxygen through the apparatus and adjust the instrument controls to give a zero reading. 1 :1998(E) If the instrument used provides a direct reading in percentage of carbon, adjust the instrument reading for each calibration range as follows. Make a choice of an appropriate steel-CRM (certified r
47、eference materials) carry out as described in 7.4 and obtain a time-CO insert the boat until it is stopped and lock the system. (In this case the centre of boat is at the centre of heating zone - see figure 1). Copyright International Organization for Standardization Provided by IHS under license wi
48、th ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 22:31:49 MDTNo reproduction or networking permitted without license from IHS -,-,- 0 IS0 ISO/TR 15349-l :1998(E) Operate the instrument in accordance with the manufacturers instructions. At the end of the combustion and measuring cycle (see figure 3), remove and discard the boat, and record the analyser reading. 7.523 Plotting the calibration graph Obtain the net reading by subtracting the reading of the zero member from that of each member of the calibration series. Prepare a calibration g