ap Designation: E 1019 - 94° Standard Test Methods for \1rtm cama sanore nen pear 9 tt Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel and in fron, Nickel, and Cobalt Alloys* ‘This standards ioe wade he Fined degraion E1019; he number immesiney following the designation inate the yea of ‘fal adoption orn the eae of ein the year of ut revion number i parentheses Soperseiptepan eae au ear chage sac he lat revlon orapw 1. Scope 1.1 These test_methods? cover the determination of carbon, sulfur, nitrogen, and oxygen, in steel and in iron, nickel, and cobalt alloys having chemical compositions ‘within the following limits Bienen [Concentron Rar, Avasinuss 0.001 1800 ‘ieony 9.002 1 003 ‘Anenie. 2.0005 60.10 Benim Gon! w 005, Bismuth Bani 1080 Boros ‘3.0008 100 Cedi ‘001 0005, acum 001 008, Cabos 2001 430 Cesar Dns wens Sromium 00s 038.00 conat| 091 730. Columbine 9002 06.00 Cooper 8.005 9 000 Hyrogen 0001 t.020 tree 801 10 1000 tend 0001 2030 Niagnenum Soni 00 Manganese O01 9200, Moiydenam 002 0 3090 Niet 00s to 6400 Ngee :00$ 19 030 Ones 0.0005 19 6.03 Poors dare Seen S001 18030 Siicon 0001 18609 Sal (Meal Sard 0402 wo3s Sor (rots Sate) {8001 16 400 Tantalane 001 te 1400 Telus 0001 19038 Tin Go02 e035 Titania 002 te 5. Tumse ‘8005 fe 34-00 Yeeadiom ‘0005 $30 Zine 0008 0.29 Zirconium 0.008 1 2500 1.2 The test methods appear in the following order: Secon Catton, Tou, ty the Comburion-Inirvmestl Measurement “Metis Nitrope by the loc Gas Fusign- Thermal Cnty Meda "These test methods ae under the jrdiion of ASTM Comite Eom Analytal Chemisty foe Meal, Orc, tnd Related Material and ae the diet ‘esponsibty of Sobeommaitee £0101 on iro, Sel and Feral ‘Curect eto approved July 1S, 998, Pblsod September 199, Orginal vb as E1013 84 Las revicus ion 1019838, Some of thew text methods represent reson of test methods covered by ASTI Mets E 350, E38), £952, £388, and E384 whachappeas inthe Arnal Bove of ASTI Senda, Vol 0305. 205 ‘Oxygen ty the Inet Gas Fusion Method Sule by te Combustee-afeed ADerpion Method (Caivation wh Meu) Sanda) Sut by the Combusticenfared Abrortoe Method (Potassium ‘Sulla Cabeason) S410 64 200% 1.3 This standard does not purport 10 address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appro- priate sajety and health practices and determine the applica- bility of regulatory limitations prior 10 use. Specific hazards statements are given in Section 8, 2, Referenced Documents 21 ASTM Standards: E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications? E 50 Practices for Apparatus, Reagents, and Safety Pre- ‘cautions for Chemical Analysis of Metals* E 59 Practice for Sampling Steel and Iron for Determina- tion of Chemical Composition* E 173 Practice for Conducting interlaboratory Studies of ‘Methods for Chemical Analysis of Metals* 3. Significance and Use 3.1 These test methods forthe chemical analysis of metals and alloys are primarily intended to test such materials for ‘compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts, capable of performing common laboratory procedures skill fully and safely. I is expected that work will be performed ia 4 property equipped laboratory 4, Apparatus and Reagents 4.1 Apparatus and reagents required for each determina- tion are listed in separate sections preceding the procedure, 5. Sampling 3.1 For procedures for sampling the materials, refer to those parts of Practice E 59 pertaining to solid form samples of the type used for instrumental analysis. 6. Rounding Calculated Values 6.1 Caleulated values shall be rounded to the desired ‘number of places as directed in Practice E 29. 7. Interlaboratory Studies 7.1 ‘These test methods have been evaluated in accordance with Practice E173. 3 anmel Book of ASTM Standards, Vol W402 ‘annual Book of ASTM Standards, Vo 0305Gh & 1019 8. Hazards 8.1 For hazards to be observed in the use of certain reagents in this test method, refer to Practices E 50. 8.2 Use care when handling hot crucibles and operating furnaces to avoid personal injury by either burn or electrical shock. ‘TOTAL CARBON BY THE COMBUSTION INSTRUMENTAL ‘MEASUREMENT METHOD. Scope 9.1 This test method covers the determination of carbon in concentrations from 0.005 to 4.5 . 10, Summary of Test Methods 10.1 The carbon is converted to carbon dioxide by combustion in a steam of oxygen. 10.1 Thermal Conductivity Method—The carbon oxide is absorbed on a suitable grade of zeolite, released by heating the zeolite, and swept by helium or oxygen into @ chromatographic column, Upon elution, the amount of carbon dioxide is measured in a thermistor-type conductivity cel, Refer to Fig. 1. 10.1.2 Infrared (FR) Absorption, Method A—The amount of carbon dioxide is measured by infrared (IR) absorption. Carbon dioxide (CO,) absorbs IR energy at a previse wavelength within the IR spectrum. Energy of this wave- Jength is absorbed as the gas passes through a cell body in which the IR energy is transmitted. All other IR energy is climinated from reaching the detector by a precise wave- length filter. Thus, the absorption of IR energy can be attributed to only CO, and its concentration is measured as changes in energy at the detector. One cell is used as both ¢ reference and a measure chamber. Total carbon, as CO>, is ‘monitored and measured over a period of time, Refer to Fig. 2 10.1.3 Infrared (2R) Absorption, Method B—The detector consists of an IR energy source, a separate measure chamber and reference chamber, and a diaphragm acting as one plate ‘Actin Puy Oxygen ‘5—Onygen Peguater (2 Stage) FIG. 1 Apparatus for Determination of Carbon by the Combustion Thermal Conductivity Method 2Qh & 1019 Oxygen Cynder 6-60.60, convener 8 Two Stage Regubtor Te (CSodhan Hycrone Error Clay "So, CetResdout 2 atanestin Perot ‘inductor Forace| Rogue —Comeustonn768 FoAlow Conroe ‘Tous Tap FIG. 2. Infrared Absorption Method A of a parallel plate capacitor. During specimen combustion, the flow of CO, with its oxygen gas carrier is routed through the measure chamber while oxygen alone passes through the reference chamber. Energy from the IR source passes through both chambers, simultaneously arriving at the diaphragm (capacitor plate). Part of the IR energy is ab- sorbed by the CO; present in the measure chamber while none is absorbed passing through the reference chamber. ‘This creates an 1R energy imbalance reaching the diaphragm, thus distorting it. This distortion alters the fixed capecitance creating an clectric signal change that is amplified for measurement as CO,. Total carbon, as CO2, is monitored and measured over a period of time. Refer to Fig. 3. 10.1.4 Infrared (IR) Absorplion, Method C, Closed Loop—The combustion is performed in a closed loop, where CO and CO, are detected in the same infrared cell. Each gas is measured with a solid state energy detector. Filters are used to pass the appropriate IR wavelength to each detector. In the absence of CO and CO,, the energy received by each detector is maximum. During combustion, the IR absorption properties of CO and CO; gases in the chamber cause a Loss of energy; therefore a loss in signal results which is propor- tional to concentrations of each gas in the closed loop. Total carbon, 2s CO, plus CO, is monitored and measured over @ period of time, Refer to Fig. 4. 10.2 This test method is writen for use with commercial analyzers, equipped to cary out the above operations automatically and calibrated using steels of known carbon content. 11, Interferences 11.1 The elements ordinarily present do not interfere. 12, Apparatus 12.1 Combustion and Measurement Apparatus—See Figs. 1,2,3,and 4. 122 Crucibles—Use crucibles that meet or exceed the HL Preaure Roguator carton Carer 00 1660, Corverir k-80, Tro (Meese Pow Rotametar FIG. 3. Infrared Absorption Method B 3