ASTM E1019-00
(Test Method)Standard Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel and in Iron, Nickel, and Cobalt Alloys
Standard Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel and in Iron, Nickel, and Cobalt Alloys
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:ElementConcentration Range, %Aluminum0.001 to 18.00Antimony0.002 to 0.03Arsenic 0.0005 to 0.10Beryllium0.001 to 0.05Bismuth 0.001 to 0.50Boron 0.0005 to 1.00Cadmium 0.001 to 0.005Calcium 0.001 to 0.05Carbon 0.001 to 4.50Cerium 0.005 to 0.05Chromium0.005 to 35.00Cobalt 0.01 to 75.0Columbium0.002 to 6.00Copper 0.005 to 10.00Hydrogen0.0001 to 0.0030Iron 0.01 to 100.0Lead 0.001 to 0.50Magnesium0.001 to 0.05Manganese0.01 to 20.0Molybdenum0.002 to 30.00Nickel 0.005 to 84.00Nitrogen0.0005 to 0.50Oxygen 0.0005 to 0.03Phosphorus0.001 to 0.90Selenium0.001 to 0.50Silicon 0.001 to 6.00Sulfur (Metal Standards)0.002 to 0.35Sulfur (Potassium Sulfate)0.001 to 0.600Tantalum0.001 to 10.00Tellurium0.001 to 0.35Tin 0.002 to 0.35Titanium0.002 to 5.00Tungsten0.005 to 21.00Vanadium0.005 to 5.50Zinc 0.005 to 0.20Zirconium0.005 to 2.500
1.2 The test methods appear in the following order: SectionsCarbon, Total, by the Combustion-Instrumental Measurement Method9-19Nitrogen by the Inert Gas Fusion-Thermal Conductivity Method31-41Oxygen by the Inert Gas Fusion Method42-53Sulfur by the Combustion-Infrared Absorption Method (Calibration with Metal Standards) 54-64Sulfur by the Combustion-Infrared Absorption Method (Potassium Sulfate Calibration) 20-30
1.3This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 5.
General Information
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Standards Content (Sample)
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Designation: E 1019 – 00
Standard Test Methods for
Determination of Carbon, Sulfur, Nitrogen, and Oxygen in
Steel and in Iron, Nickel, and Cobalt Alloys
This standard is issued under the fixed designation E 1019; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
Carbon, Total, by the Combustion–Instrumental Measurement
Method 9-19
1.1 These test methods cover the determination of carbon,
Nitrogen by the Inert Gas Fusion–Thermal Conductivity Method 31-41
sulfur, nitrogen, and oxygen, in steel and in iron, nickel, and
Oxygen by the Inert Gas Fusion Method 42-53
Sulfur by the Combustion-Infrared Absorption Method (Calibration
cobalt alloys having chemical compositions within the follow-
with Metal Standards) 54-64
ing limits:
Sulfur by the Combustion–Infrared Absorption Method (Potassium
Sulfate Calibration) 20-30
Element Concentration Range, %
Aluminum 0.001 to 18.00
Antimony 0.002 to 0.03
1.3 This standard does not purport to address all of the
Arsenic 0.0005 to 0.10
Beryllium 0.001 to 0.05
safety concerns, if any, associated with its use. It is the
Bismuth 0.001 to 0.50
responsibility of the user of this standard to establish appro-
Boron 0.0005 to 1.00
priate safety and health practices and determine the applica-
Cadmium 0.001 to 0.005
Calcium 0.001 to 0.05
bility of regulatory limitations prior to use. Specific hazards
Carbon 0.001 to 4.50
statements are given in Section 5.
Cerium 0.005 to 0.05
Chromium 0.005 to 35.00
2. Referenced Documents
Cobalt 0.01 to 75.0
Columbium 0.002 to 6.00
2.1 ASTM Standards:
Copper 0.005 to 10.00
E 29 Practice for Using Significant Digits in Test Data to
Hydrogen 0.0001 to 0.0030
Iron 0.01 to 100.0 Determine Conformance with Specifications
Lead 0.001 to 0.50
E 50 Practices for Apparatus, Reagents, and Safety Precau-
Magnesium 0.001 to 0.05
tions for Chemical Analysis of Metals
Manganese 0.01 to 20.0
Molybdenum 0.002 to 30.00
E 1806 Practice for Sampling Steel and Iron for Determi-
Nickel 0.005 to 84.00
nation of Chemical Composition
Nitrogen 0.0005 to 0.50
E 173 Practice for Conducting Interlaboratory Studies of
Oxygen 0.0005 to 0.03
Phosphorus 0.001 to 0.90
Methods for Chemical Analysis of Metals
Selenium 0.001 to 0.50
Silicon 0.001 to 6.00
3. Significance and Use
Sulfur (Metal Standards) 0.002 to 0.35
Sulfur (Potassium Sulfate) 0.001 to 0.600
3.1 These test methods for the chemical analysis of metals
Tantalum 0.001 to 10.00
and alloys are primarily intended to test such materials for
Tellurium 0.001 to 0.35
compliance with compositional specifications. It is assumed
Tin 0.002 to 0.35
Titanium 0.002 to 5.00
that all who use these test methods will be trained analysts,
Tungsten 0.005 to 21.00
capable of performing common laboratory procedures skill-
Vanadium 0.005 to 5.50
fully and safely. It is expected that work will be performed in
Zinc 0.005 to 0.20
Zirconium 0.005 to 2.500
a properly equipped laboratory.
1.2 The test methods appear in the following order:
4. Apparatus and Reagents
Sections
4.1 Apparatus and reagents required for each determination
are listed in separate sections preceding the procedure.
5. Hazards
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
5.1 For hazards to be observed in the use of certain reagents
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Nov. 10, 2000. Published January 2001. Originally
e1 3
published as E 1019 – 84. Last previous edition E 1019 – 94 . Annual Book of ASTM Standards, Vol 14.02.
2 4
Some of these test methods represent revisions of test methods covered by Annual Book of ASTM Standards, Vol 03.05.
ASTM Methods E 350, E 351, E 352, E 353, and E 354 which appear in the Annual Annual Book of ASTM Standards, Vol 03.06.
Book of ASTM Standards, Vol 03.05. Discontinued 1998; see 1997 Annual Book of ASTM Standards, Vol 03.06.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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E 1019
in this test method, refer to Practices E 50. TOTAL CARBON BY THE COMBUSTION
INSTRUMENTAL MEASUREMENT METHOD
5.2 Use care when handling hot crucibles and operating
furnaces to avoid personal injury by either burn or electrical
9. Scope
shock.
9.1 This test method covers the determination of carbon in
concentrations from 0.005 to 4.5 %.
6. Sampling
10. Summary of Test Method
6.1 For procedures for sampling the materials, refer to those
10.1 The carbon is converted to carbon dioxide by combus-
parts of Practice E 1806.
tion in a stream of oxygen.
10.1.1 Thermal Conductivity Method—The carbon dioxide
7. Rounding Calculated Values
is absorbed on a suitable grade of zeolite, released by heating
7.1 Calculated values shall be rounded to the desired num-
the zeolite, and swept by helium or oxygen into a chromato-
ber of places as directed in Practice E 29.
graphic column. Upon elution, the amount of carbon dioxide is
measured in a thermistor-type conductivity cell. Refer to Fig. 1.
8. Interlaboratory Studies
10.1.2 Infrared (IR) Absorption, Method A— The amount of
8.1 These test methods have been evaluated in accordance
carbon dioxide is measured by infrared (IR) absorption. Car-
with Practice E 173. bon dioxide (CO ) absorbs IR energy at a precise wavelength
A—High Purity Oxygen M—CO Collection Trap
B—Oxygen Regulator (2 Stage) N—Furnace Combustion Exhaust
C—Sodium Hydroxide Impregnated Clay/Magnesium Perchlorate O—Furnace Purge Exhaust
D—Secondary Pressure Regulator P—Metal Connector To Use Oxygen As Carrier Gas
E—Flowmeter Q—High Purity Helium
F—Induction Furnace R—Helium Regulator (2 Stage)
G—Combustion Tube S—Chromagraphic Column
H—Dust Trap T—TC Cell/Readout
I—Manganese Dioxide U—Measure Flowmeter
J—Heated CO to CO Converter V—Reference Flowmeter
K—Magnesium Perchlorate W—Furnace Power Stat
L—Valve Manifold
* May be sealed chamber if
oxygen is carrier gas.
** Not required if oxygen is
carrier gas.
FIG. 1 Apparatus for Determination of Carbon by the Combustion Thermal Conductivity Method
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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E 1019
within the IR spectrum. Energy of this wavelength is absorbed pass the appropriate IR wavelength to each detector. In the
as the gas passes through a cell body in which the IR energy is absence of CO and CO , the energy received by each detector
transmitted. All other IR energy is eliminated from reaching is maximum. During combustion, the IR absorption properties
the detector by a precise wavelength filter. Thus, the absorption of CO and CO gases in the chamber cause a loss of energy;
of IR energy can be attributed to only CO and its concentra- therefore a loss in signal results which is proportional to
tion is measured as changes in energy at the detector. One cell concentrations of each gas in the closed loop. Total carbon, as
is used as both a reference and a measure chamber. Total CO plus CO, is monitored and measured over a period of
carbon, as CO , is monitored and measured over a period of time. Refer to Fig. 4.
time. Refer to Fig. 2. 10.2 This test method is written for use with commercial
10.1.3 Infrared (IR) Absorption, Method B— The detector analyzers, equipped to carry out the above operations automati-
consists of an IR energy source, a separate measure chamber cally and calibrated using steels of known carbon content.
and reference chamber, and a diaphragm acting as one plate of
11. Interferences
a parallel plate capacitor. During specimen combustion, the
11.1 The elements ordinarily present do not interfere.
flow of CO with its oxygen gas carrier is routed through the
measure chamber while oxygen alone passes through the
12. Apparatus
reference chamber. Energy from the IR source passes through
12.1 Combustion and Measurement Apparatus—See Figs.
both chambers, simultaneously arriving at the diaphragm
1-4.
(capacitor plate). Part of the IR energy is absorbed by the CO
12.2 Crucibles—Use crucibles that meet or exceed the
present in the measure chamber while none is absorbed passing
through the reference chamber. This creates an IR energy specifications of those recommended by the manufacturer of
the instrument used and preheat in a suitable furnace for not
imbalance reaching the diaphragm, thus distorting it. This
distortion alters the fixed capacitance creating an electric signal less than 40 min at more than 1000°C. Remove from the
furnace and cool in air for 90 6 15 s before use. Crucibles may
change that is amplified for measurement as CO . Total carbon,
as CO , is monitored and measured over a period of time. be placed in a desiccator for periods of 1 h prior to use.
12.3 Crucible Tongs—Capable of handling recommended
Refer to Fig. 3.
10.1.4 Infrared (IR) Absorption, Method C, Closed Loop— crucibles.
The combustion is performed in a closed loop, where CO and
13. Reagents
CO are detected in the same infrared cell. Each gas is
13.1 Acetone—The residue after evaporation must be
measured with a solid state energy detector. Filters are used to
<0.0005 %.
13.2 Copper (Low Carbon), granular (10 to 30 mesh) (Note
1).
13.3 Oxygen, Ultra High Purity (purity: 99.95 %
minimum)—Other grades of oxygen may be used if low and
consistent blank readings are obtained, or the oxygen may be
purified as described in Practices E 50.
13.4 Platinum or Platinized Silica, heated to 350°C for the
conversion of carbon monoxide to carbon dioxide.
13.5 Tungsten (Low Carbon), 12 to 20 mesh (Note 1).
13.6 Tungsten-Tin (Low Carbon), 20 to 40 mesh.
NOTE 1—The accelerator should contain no more than 0.001 % carbon.
If necessary, wash three times with acetone by decantation to remove
organic contaminants and dry at room temperature. The mesh size is
critical to the inductive coupling which heats the sample.
14. Preparation of Apparatus
14.1 Assemble the apparatus as recommended by the manu-
facturer.
14.2 Test the furnace and analyzer to ensure the absence of
leaks and make the required electrical power connections.
Prepare the analyzer for operation according to the manufac-
turer’s instructions. Make a minimum of two determinations
using the specimen and accelerator as directed in 17.1.2 and
17.1.3 before attempting to calibrate the system or determine
A—Oxygen Cylinder G—CO-CO Converter
B—Two Stage Regulator H—SO Trap
the blank.
C—Sodium Hydroxide Impregnated Clay I—CO IR Cell/Readout
D—Magnesium Percholorate J—Induction Furnace
15. Sample Preparation
E—Regulator K—Combustion Area
F—Flow Controller L—Dust Trap
15.1 The sample should be uniform in size, but not finer
FIG. 2 Infrared Absorption Method A than 40 mesh.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1019
A—Oxygen Cylinder G—Orifice
B—Two Stage Regulator H—Pressure Regulator
C—Sodium Hydroxide Impregnated Clay I—Combustion Chamber
D—Magnesium Percholorate J—CO to CO Converter
E—Dust Trap K—SO Trap
F—IR Cell/Readout L—Measure Flow Rotameter
FIG. 3 Infrared Absorption Method B
15.2 Wash in acetone and dry at 70 to 100°C. 16.3.2 Proceed as directed in 17.1.2 and 17.1.3.
16.3.3 Repeat 16.3.1 and 16.3.2 a sufficient number of times
16. Calibration
to establish that low (less than 0.020 mg of carbon) and
16.1 Calibration Standards (Note 2):
consistent (60.002 mg of carbon) readings are obtained. Blank
16.1.1 For Range I, 0.005 to 0.10 % carbon, select three values are equal to the total result of the accelerator and
primary standard reference materials containing approximately
Standard A minus the certified value for the primary standard
0.005, 0.05, and 0.10 % carbon and designate them as Stan- reference material.
dards A, B, and C, respectively.
16.3.4 Record the average value of at least three blank
16.1.2 For Range II, 0.10 to 1.25 % carbon, select two
determinations.
primary standard reference materials containing approximately
16.3.5 If the blank readings are too high or inconsistent,
0.12 and 1.00 % carbon and designate them as Standards BB
determine the cause, correct it, and repeat the steps as directed
and CC, respectively.
in 16.3.1-16.3.4.
16.1.3 For Range III, 1.25 to 4.50 % carbon, select two
16.3.6 Enter the average blank value in the analyzer (Note
primary standard reference materials containing approximately
3); refer to manufacturer’s instructions. This mechanism will
1.25 and 4.00 % carbon and designate them as Standards BBB
electronically compensate for the blank value.
and CCC, respectively.
NOTE 3—If the unit does not have this function, the blank value must
NOTE 2—The accuracy of this test method is dependent upon the
be subtracted from the total result prior to any calculation.
accuracy of the test methods used to certify the carbon concentration in the
16.4 Determination of Blank Reading—Range II—Proceed
calibration primary standard reference materials, as well as upon their
as directed in 16.3.
homogeneity.
16.5 Determination of Blank Reading—Range III:
16.2 Adjustment of Response of Measurement System:
16.5.1 Transfer 0.5 g of Standard A, weighed to the nearest
16.2.1 Transfer 1.0 g of Standard B, weighed to the nearest
1 mg, and 1.5 g of accelerator, weighed to the nearest 5 mg, to
1 mg, and 1.5 g of accelerator, weighed to the nearest 5 mg, to
a preburned crucible.
a preburned crucible.
16.5.2 Proceed as directed in 16.3.2-16.3.6.
16.2.2 Proceed as directed in 17.1.2 and 17.1.3.
16.6 Calibration—Range I (0.005 to 0.10 % carbon):
16.2.3 Repeat 16.2.1 and 16.2.2 until the absence of drift is
indicated. Adjust the signal to provide a reading within 60.003 16.6.1 Weigh four 1.0 g specimens of Standard C, to the
nearest 1 mg, the place in preburned crucibles. To each, add 1.5
of the certified percent carbon value for the primary standard
reference material. g of accelerator, weighed to the nearest 5 mg.
16.3 Determination of Blank Reading—Range I: 16.6.2 Follow the calibration procedure recommended by
16.3.1 Transfer 1.0 g of Standard A, weighed to the nearest the manufacturer. Use Standard C as the primary calibration
1 mg, and 1.5 g
...
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