Unknown INTERNATIONAL STANDARD IS0 9556 First edition 1989 07 15 Corrected and reprinted 1989 11 15 Steel and iron Determination of total carbon content Infrared absorption method after combustion in[.]
INTERNATIONAL STANDARD IS0 9556 First edition 1989-07-15 w co m Corrected and reprinted 1989-11-15 fx of total carbon Steel and iron - Determination content - Infrared absorption method after combustion in an induction furnace par absorption dans ww w bz Aciers et fontes - Dosage du carbone total - M6thode l’infrarouge apr&s combustion dans un four B induction Reference number IS0 9556 : I!389 (E) 9556 : 1999 (El Foreword IS0 (the International Organization for Standardization) is a worldwide federation co m IS0 of body interested in a subject for which a technical committee w national standards bodies (IS0 member bodies) The work of preparing International Standards is normally carried out through IS0 technical committees Each member 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 IS0 closely with the International matters of electrotechnical Draft International Electrotechnical standardization Standards adopted by the technical the member bodies for approval before their acceptance the IS0 Council They are approved in accordance least 75 % approval by the member bodies voting International Standard IS0 9556 was prepared A, B and C of this International ww (IEC) on all are circulated Standards to by with IS0 procedures requiring at by Technical Committee ISO/TC Standard w Annexes committees as International bz Steel Commission fx collaborates are for information only 17, IS0 9558 : 1989 (E) STANDARD co m INTERNATIONAL of total carbon content Steel and iron - Determination Infrared absorption method after combustion in an induction furnace Scope This International Standard specifies an infrared absorption method after combustion in an induction furnace for the determination of the totai carbon content in steel and iron The method (rnlm) is applicable to carbon contents between 0,003 % and 4.5 % (m/m) Reagents w During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity 4.1 free from carbon dioxide Water, for 30 min, cool to room temperature fx Boil water with oxygen The Normative following reference references standards Standard 4.2 contain in this text, constitute provisions At the time of publication, through the editions indicated are subject to revision, and parties to bz were valid All standards which, provisions of this International agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards listed below Members of IEC and IS0 maintain registers of currently valid International Standards IS0 377 : 1985, Wrought steel - IS0 385-l : 1984, Laboratory General requirements IS0 648 : 1977, Laboratory IS0 Selection 1042 : 1983, Laboratory glassware glassware glassware ww flasks - - and reproducibility inter-laboratory Burettes One-mark - One-mark IS0 5725 : 1986, Precision of test methods repeatability and preparation w samples and test pieces - for a standard - of Part I: Combustion 99,5 % (m/m) minimum An oxidation catalyst [copper(N) to a temperature ing unit (see annex 4.3 Pure oxide or platinum] tube heated above 450 OC must be used prior to a purifyC), when is suspected iron, of the presence of organic con- in the oxygen known low carbon content less than 0,001 % (m/m) 4.4 Suitable solvent, dirty test samples, 4.5 Magnesium appropriate for example, for washing greasy or acetone perchlorate IMg(ClO&J, particle size: pipettes 4.6 volumetric Determination of test method by Barium carbonate Dry barium carbonate (minimum assay: 99,5 %I at 105 OC to 110 OC for h and cool in a desiccator before use 4.7 Sodium carbonate tests Dry anhydrous sodium carbonate (minimum 285 ‘C for h and cool in a desiccator assay: 99,9 %) at before use 4.8 Accelerator : copper, tungsten-tin mixture or tungsten of known low carbon content less than 0,001 % (m/m) of a test portion in a high-frequency of pure oxygen and/or Oxygen, taminants and bubble (4.2) for 15 Prepare just before use from 0,7 mm to I,2 mm Principle temperature - Transformation with accelerator induction furnace at a high in a current of carbon into carbon dioxide 4.9 Sucrose, per litre standard solution, corresponding to 25 g of C carbon monoxide Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide carried by a current of oxygen Weigh, to the nearest mg, 14,843 g of sucrose (C12H22011) (analytical standards grade) previously dried at 100 OC to 105 OC for 2.5 h and cooled in a desiccator ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - IS0 9556 : 1969 (E) Dissolve in about 100 ml of water (4.11, transfer to a 250 ml one-mark volumetric flask quantitatively, dilute to the mark with water SAFETY INSTRUCTIONS tion analysis are mainly (4.1) and mix solution contains 25 mg of C 4.10 Sodium carbonate, to 25 g of C per litre standard solution, crucibles and in the fusions Use crucible tongs times and suitable containers for the used crucibles mal corresponding precautions taken to the nearest (4.71, dissolve mg, in about 250 ml one-mark g of sodium 200 ml of water volumetric mark with water 55,152 solution effectively to a dilute to the (4.1) and mix ml of this standard 7.1 contains 25 mg of C General the from oxygen cylinders shall be process shall be in a confined space using tubes w clay) impregnated (4.11) and magnesium since a high concan present a instructions supply (attapulgus at all Nor- combustion the apparatus operating Purify the oxygen ceramic 4.11 Inert ceramic (attapulgus clay) impregnated with sodium hydroxide, particle size: from 0,7 mm to I,2 mm handling from centration of oxygen fire hazard carbonate (4.11, transfer flask quantitatively, for Oxygen removed Weigh, - The risks related to combusburns in pre-igniting the ceramic co m ml of this standard Procedure perchlorate cent flow rate whilst on standby packed with the inert with sodium hydroxide (4.51, and maintain a quiesMaintain a glass wool filter or a stainless steel net as a dust collector Clean and change as necessary The furnace chamber, pedestal post and filter trap shall be cleaned frequently Apparatus to remove oxide build-up laboratory stated, fx Allow each item of equipment During the analysis, unless otherwise use only ordinary apparatus mended by the equipment supply is switched to stabilize for the time recom- manufacturers when the main on after being out of action for any length of time IS0 385-1, glassware shall be class A, in accordance IS0 648 or IS0 1042 as appropriate with After cleaning the furnace after the equipment duction required for combustion furnace measurement and the of the evolved in a high-frequency subsequent infrared carbon dioxide monoxide may be obtained commercially manufacturers Follow the manufacturer’s operation of the instrument 5.1 pl instruments and/or Micropipette, from a number of instructions for the are given in annex C Ceramic in an induction Ignite crucibles filters or by burning several 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 of carbon, used provides a direct reading in percentage adjust the instrument reading for each calibration range as follows Select the certified reference material with a carbon content close to the maximum carbon content in the calibration series, measure the carbon content of the certified reference material in the manner specified in 7.4 less than 0,001 % (m/m) ww 5.3 changing for a period, stabilize 100 ul, limit of error shall be less than 5.2 Tin capsule, about mm in diameter, 18 mm in height, 0.3 g in mass and approximately 0,4 ml in volume, of known low carbon content the apparatus and/or carbon w Features of commercial in- absorption bz The apparatus chamber has been inoperative crucible, capable of withstanding Adjust the reading of the instrument NOTE furnace - specified in an electric furnace to the certified value combustion in air or in a current This adjustment in 7.5 shall be made before the calibration It cannot replace or correct the calibration of oxygen for not less than h at 100 OC and store in a desicTest as cator before use 7.2 NOTE - For the determination of low carbon contents it is advisable to ignite crucibles at 350 OC in a current of oxygen Degrease the test sample by washing in a suitable solvent (4.4) Evaporate Weigh, portion ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - All volumetric the last traces of the washing to the nearest mg, approximately ple for carbon Sampling Carry out sampling national standards contents less than imately 0,5 g for carbon contents in accordance for iron with IS0 377 or appropriate I,0 liquid by heating g of the test sam- % (m/m) greater than I,0 NOTE - The mass of the test portion may be dependent instrument used and approx% (m/m) on the type of IS0 7.3 Blank Using test the micropipette (5.1), transfer 9556 : 1989 (E) 100 ul of each of the diluted solutions to five tin capsules (5.2) and dry at 90 “C for Prior to the determination, carry out the following blank tests in h duplicate ble (5.3), press the tin capsule lightly against the bottom of the crucible Add the same quantity of pure iron (4.3) as that of the test portion (7.21, and the same quantity of the accelerators Table (4.8) (see note 2) as will be added to the test portion Volume Treat the crucible and contents third paragraphs Obtain the milligrams as specified in the second and reading Mass of of the blank tests and convert of carbon by means of the calibration the standard ml it to graph (7.5) 0”) by subtracting the mass of carbon in the pure iron used (4.3) from the mass of carbon in the blank tests The mean blank value (??z,) is calculated from the two blank values (see note 3) 2.0 54 10.0 l) Carbon of content in the test portion in the tin capsule S”~~~~t$er % h/m) mg mg 0 0.10 0,010 0,001 0,20 0,020 0,002 0,50 l,oo 0,050 0,100 0,005 0,010 Zero member fx NOTES Mass carbon taken w 1,o The blank value is obtained of carbon in the diluted solution ((4.91 or (4.1O)l of 7.4 in a desiccator co m Cool to room temperature Transfer the tin capsule (5.2) (see note 1) to the ceramic cruci- 7.5.1.2 Measurements Prepare the tin capsule; using the micropipette (5.11, transfer 100 pl of water (4.1) to a tin capsule (5.2) and dry at 90 “C for h Transfer the tin capsule The quantity of accelerators will depend on the individual characteristics of the instrument and the type of material being analysed The amount used shall be sufficient for complete combustion ly against the bottom of the ceramic crucible, add 1,000 g of pure iron (4.31 and cover with the same quantity of the ac- The mean blank value and the difference between the two blank values shall both not exceed 0,Ol mg of carbon If these values are abnormally high, investigate and eliminate the source of contamination Determination Transfer one tin capsule (5.2) to the ceramic w 7.4 press the tin capsule lightly against the bottom crucible, add the test portion propriate mass of the accelerators (7.2) crucible and cover with ww At the end of the combustion discard the crucible, 7.5 the ap- (4.8) (see note of 7.3) Place the ceramic crucible and contents sucrose or sodium car- bonate to the ceramic crucible (5.31, press the tin capsule light- celerators portion (4.8) (see note of 7.3) as will be added to the test Treat the crucible and contents third paragraphs of 7.4 7.5.1.3 Plotting the calibration as specified in the second and graph of the ceramic on the pedestal raise to the combustion position and lock the system the furnace in accordance with the manufacturer’s tions (5.31, containing ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - bz In cases where the calibration graphs of 7.5.1 or 7.5.2 are applied, use the following prepared capsule post, Operate instruc- and measuring cycle, remove and Obtain the net reading by subtracting the reading of the zero member from that of each member of the calibration series Prepare a calibration graph by plotting the milligrams of carbon for each member 7.5.2 Samples (m/m) and 0,l having carbon net reading against of the calibration contents between series 0,Ol % (4.9) or % (m/m) and record the analyser reading Establishment of the calibration 7.5.1 Samples having carbon (m/m) and 0,Ol % (m/m) contents 7.5.2.1 Preparation Transfer the volumes between 0,003 % sodium carbonate Preparation Transfer the volumes of sucrose standard to five 50 ml one-mark with water 7.5.1.1 of the calibration of the calibration volumetric standard solution (4.10) indicated flasks in table Dilute to the mark series standard solution (4.9) or (5.11, transfer 100 pl of each of the diluted solutions to five tin capsules (5.2) and dry at 90 OC for sodium carbonate standard solution (4.10) indicated in table to five 250 ml one-mark volumetric flasks Dilute to the mark h with water Cool to room temperature (4 I) and mix solution (4.1) and mix Using the micropipette of sucrose series graph in a desiccator 9558 : 1989 (El Table \‘-l me ““l”l of the str rndard solu Ition :(4.9) 01r (4.1O)l ml 7.5.4.1 Mass of carbon in the diluted solution, per millilitre Mass of :arbon taken in the tin capsule Carbon content in the test portion w mg % b-n/m) I 0 zo 1.0 0,010 4,o zo 0.10 0,20 10,o 5.0 09 0,020 0,050 20,o 10.0 l,@J 0,100 0') Preparation Weigh, to the nearest 0,l Table Mass of the reference Sodium carbonate (4.7) 0') in 7.5.1.2 7.5.3 graph in 7.5.1.3 *) Samples having carbon contents between 0,l % (m/m) 4.1 5.0 l,O 88.2 10,o 2.0 246.4 369.7 132,3 198.6 15.0 22,5 3,o 4,5 Zero member 7.5.4.2 Measurements Transfer the tin capsule containing 7.5.3.1 Preparation of the calibration Weigh, to the nearest 0,l (4.6) or sodium carbonate series carbonate to the ceramic lightly against the bottom mg, the masses of barium carbonate (4.7) indicated in table and transfer to five tin capsules (5.2) material -Tiq-Gq carbonate (4.6) Mass of I carbon taken i:$$ carbonate (4.7) 0") W3 Carbon content in the test portion % (m/m) 1.0 0,lO 17,7 28 M,l 50 10.0 0,20 0,50 88.2 1.00 Zero member of pure iron (4.3) and cover with the same quantity of the accelerators (4.8) (see note of 7.3) as will be added to the test Treat the crucible and contents third paragraphs of 7.4 7.5.4.3 As specified 8.1 Method of results of calculation graph (7.5) Measurements celerators The carbon wc (%I, content, expressed as a percentage by mass, is given by the equation : (rno - ii,) ~m x 103 x loo (4.8) (see note of 7.3) as will be added to the test portion Treat the crucible and contents third paragraphs = (m as specified - ~72~) IOm in the second and of 7.4 Plotting the calibration As specified where graph m is the mass, expressed test portion; in milligrams of carbon, in the ml is the mass, expressed blank test (7.3); in milligrams of carbon, in the in 7.5.1.3 Samples having carbon contents between and 4,5 % (m/ml graph in 7.5.1.3 Expression lightly against the bottom of the ceramic crucible, add 1,000 g of pure iron (4.3) and cover with the same quantity of the ac- 7.5.4 Plotting the calibration in the second and Convert the analyser reading of the test portion to milligrams of Transfer the tin capsule containing barium carbonate or sodium carbonate to the ceramic crucible (5.31, press the tin capsule 7.5.3.3 as specified carbon (m,-,) by means of the calibration ww 7.5.3.2 or sodium w 0") 16,4 32,9 a,1 164.3 *) bz of the reference ma barium carbonate crucible (5.31, press the tin capsule of the ceramic crucible, add 0,500 g portion Table Mass 82,l 164,3 fx and 1,0 % (m/m) Carbon content in the test portion % (m/m) mg 0") w As specified Mass of carbon taken in the tin capsule material n-4 Plotting the calibration in table and transfer NOTE - If the weighed barium carbonate cannot be transferred to the tin capsule, it may be placed directly on the bottom of the ceramic crucible Measurements 7.5.2.3 (4.7) indicated to five tin capsules (5.2) Barium carbonate (4.6) As specified series mg, the masses of barium carbonate (4.6) or sodium carbonate l) Zero member 7.5.2.2 of the calibration co m IS0 1,0 % (m/m) m is the mass, in grams, of the test portion (7.2) IS0 A Precision planned laboratories, three NOTES trial of this method was at 12 levels of carbon, determinations of carbon carried out each laboratory content at each by 22 making level Two of the three determinations ty conditions (see were treated statistically carbon content showed a logarithmic and repeatability relationship (r) and reproducibility (R and R 0,005 0,000 53 0,000 69 0,Ol 0,000 99 0,002 40 0.02 0,05 0,001 42 0,002 29 0,003 0,006 59 12 0.1 0,003 29 0,004 72 0,009 17 02 0,5 18 zo 62 19 0,001 60 0,013 0,023 0,035 0,052 0,084 + I RW 0,000 77 0,001 02 one operator, same same calibration, ap- and 0,001 50 the within-laboratory reproducibility was report The test report shall include the following a) (R,) all information necessary sample, the laboratory b) method the information for the identification : of the and the date of the analysis; used, by reference to this International Standard ; 0,002 20 0,003 65 c) the results, and the form in which they are expressed; 0,005 36 0,007 85 d) any unusual features 0,013 0,019 0,028 0,043 a noted during the determination; e) any operation not specified in this International Standard, or any optional operation which may have influenced the results ww w 4.5 0,007 0,011 0,015 0,024 0,001 Test fx (m/m) 0,003 bz % Reproducibility Repeatability day 2, w R,) of the test results (see note 3) as summarized in table The graphical representation of the figures is given in annex Carbon content on calculated between Table i.e From the two values obtained on day the repeatability (r) and reproducibility (R) were calculated using the procedure specified in IS0 5725 From the first value obtained on day and the value ob- in accordance tained The data obtained conditions, The third determination was carried out at a different time (on a different day) by the same operator as in note using the same apparatus with a new calibration are listed in table A The results obtained with IS0 5725 were carried out under repeatabili- in IS0 5725, paratus, identical operating minimum period of time notes and 2) The test samples used and mean results obtained as defined co m 8.2 9558 : 1989 (El ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - IS0 9558 : 1989 (E) Annex A (informative) on the international Table was derived from the results of international eight countries involving 22 laboratories The results of the trials were reported in document co-operative analytical trials carried out in 1985 on seven steel samples and five iron samples in 17/l N 888, April 1988 The graphical representation in annex B of the precision data is given w The test samples used are listed in table A.1 Table A.1 Carbon content % (m/m) Sample fx Certified High-purity iron High-purity Electrolytic iron iron BCS 43111 Carbon steel JSS 171-3 NBS SRM 159 JSS 030-4 Mild steel Carbon steel Carbon steel EURO F 080-l NBS SRM bz EURO B 097-l JSS 001-2 NBS SRM 365 14f EURO B 063-l NBS SRM 3d JSS 110-7 Carbon steel Carbon steel Carbon steel White iron Pig iron w WI : General mean of within a day ww W2 : General mean of between days tests < Found I Wl 0,002 0,004 0,006 0,001 0,004 0,007 0,001 0,004 0,007 0,026 0,025 0,025 0,042 0,0412 0,094 0.18 0,452 0,092 0,183 0,040 0,092 0,182 0,457 0,456 0,753 0,760 1,26 254 1,267 2,556 0,760 1,266 2,559 4,12 4,095 4,095 ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - information co m Additional IS0 9556 : 1989 (El Annex B (informative) representation of precision data 0,Ol fx I ii w co m Graphical bz CL 0,005 0,001 0,0005 0,Ol w 0,005 B.l - Logarithmic 0,l Carbon content 0,5 I% (m/m)] relationship between carbon content or reproducibility (R and Z?,) 1% (m/m)1 and repeatability (r) ww Figure 0,05 ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - IS0 9556 : 1989 (E) Annex C (informative) C.1 Source of commercial high-frequency induction and infrared carbon analysers of oxygen, fitted with a fine regulating C.4.5 valve The temperature and a pressure gauge A pressure regulator is required to con- depends trol the according the characteristics oxygen manufacturer’s pressure to the specification furnace to the furnaces co m Features attained in part on the factors test portion and the mass of materials This is usually 28 kN/ms containing unit, the inert ceramic im- c.3 Flowmeter, to I/min capable of measuring a flow of oxygen of C.6 Desulfurization trioxide collector High-frequency C.4.1 The combustion and a high-frequency induction furnace generator furnace consists of an induction in inner diameter, which fits inside the induction 200 mm to 220 mm 26 mm in length) coil This tube has metal plates bz at the top and bottom which are sealed to the tube by O-rings Gas inlet and outlet points are made through the metal plates C.4.2 The generator is usually a I,5 kVA to 2,5 kVA apparent power unit, but the frequency used by certain manufac- turers may be different Values of MHz to MHz, 15 MHz, and 20 MHz have been used The power from the generator is fed to the induction coil which surrounds the silica furnace tube The w and is usually air-cooled C.4.3 crucible within containing the sample, flux and the induction ww determine coil for effective coupling The induction coil diameter, the number of turns, the chamber geometry and the power of the generator the degree of coupling which can occur These fac- tors are determined by the instrument manufacturer ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - gas analyser C.7.1 In most instruments tion are transferred of oxygen the gaseous products of combus- to the analyser system in a continuous flow The gases flow through an infrared cell, for example of the Luft type, where the absorption due to carbon dioxide and/or and integrated over a pre-programmed is amplified and converted concentration carbon of the infrared radiation monoxide is measured time period The signal to a digital display of the percentage of carbon C.7.2 In some analysers the products of combustion may be collected in oxygen in a fixed volume at controlled pressure and carbon monox- ac- when the power is supplied C.4.4 furnace infrared the mixture analysed for carbon dioxide and/or ide celerator is supported on a pedestal post which is precisely positioned so that, when raised, the metal in the crucible is correctly placed C.7 silica and a sulfur cellulose cotton The furnace chamber consists of a silica tube (e.g 30 mm to 40 mm in outer diameter, to 36 mm coil metal oxide dust consisting of a heated oxidation foil or platinized containing fx C.4 tube, a platinum but also on the form of the Certain of these factors c.5 Dust collector, capable of collecting in a current of oxygen from the furnace tube containing combustion by the operator w Purifying pregnated with sodium hydroxide in a carbon dioxide absorbing tube, and the magnesium perchlorate in a dehydration tube the in C.4.4, of the metal in the crucible, may be varied to some extent C.2 during indicated C.7.3 Electronic controls are usually provided the instrument zero, compensating slope calibration of the response line and The analyser generally for adjusting for the blank, adjusting the correcting for non-linear has a means of entering the mass of the standard or test portion for automatic correction of the read-out Instruments may also be equipped with an integrated automatic the test calculator portion balance for weighing and transferring the crucible, weighing the value of mass to the 9556 : 1999 (E) ww w bz ```````,`,`,`,``,,,``,,-`-`,,`,,`,`,,` - fx w co m Is0 UDC 669.1 : 643.422.4 Descriptors : steels, Price based on pages iron, : 646.26 chemical analysis, determination of content, carbon, infrared spectra, absorption spectra,