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 0305Gh & 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
2Qh & 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