ASTM E1999-99(2004)
(Test Method)Standard Test Method for Analysis of Cast Iron Using Optical Emission Spectrometry
Standard Test Method for Analysis of Cast Iron Using Optical Emission Spectrometry
SIGNIFICANCE AND USE
The chemical composition of cast iron alloys must be determined accurately in order to insure the desired metallurgical properties. This procedure is suitable for manufacturing control and inspection testing.
SCOPE
1.1 This test method covers the optical emission spectrometric analysis of cast iron by use of the point-to-plane technique for the following elements in the concentration ranges shown (Note 1):
Concentration Ranges, %ElementsApplicable Range, % Quantitative Range, %ACarbon1.9 to 3.81.90 to 3.8Chromium0 to 2.0 0.025 to 2.0Copper0 to 0.750.015 to 0.75Manganese0 to 1.8 0.03 to 1.8Molybdenum0 to 1.2 0.01 to 1.2Nickel0 to 2.0 0.02 to 2.0Phosphorus0 to 0.4 0.005 to 0.4Silicon0 to 2.5 0.15 to 2.5Sulfur0 to 0.080.01 to 0.08Tin0 to 0.140.004 to 0.14Titanium0 to 0.12 0.003 to 0.12Vanadium0 to 0.22 0.008 to 0.22
AQuantitative range in accordance with Practice E1601.
Note 1--The concentration ranges of the elements listed have been established through cooperative testing of reference materials. These concentration ranges can be extended by the use of suitable reference materials.
1.2 This test method covers analysis of specimens having a diameter adequate to overlap the bore of the spark stand opening (to effect an argon seal). The specimen thickness should be sufficient to prevent overheating during excitation. A heat sink backing may be used. The maximum thickness is limited only by the height that the stand will permit.
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.
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Designation:E1999–99 (Reapproved 2004)
Standard Test Method for
Analysis of Cast Iron Using Optical Emission Spectrometry
This standard is issued under the fixed designation E1999; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the optical emission spectro- 2.1 ASTM Standards:
metric analysis of cast iron by use of the point-to-plane E135 Terminology Relating to Analytical Chemistry for
technique for the following elements in the concentration Metals, Ores, and Related Materials
ranges shown (Note 1): E158 Practice for Fundamental Calculations to Convert
Intensities into Concentrations in Optical Emission Spec-
Concentration Ranges, %
A
Elements Applicable Range, % Quantitative Range, %
trochemical Analysis
E172 Practice for Describing and Specifying the Excitation
Carbon 1.9 to 3.8 1.90 to 3.8
Source in Emission Spectrochemical Analysis
Chromium 0 to 2.0 0.025 to 2.0
Copper 0 to 0.75 0.015 to 0.75
E305 Practice for Establishing and Controlling Atomic
Manganese 0 to 1.8 0.03 to 1.8
Emission Spectrochemical Analytical Curves
Molybdenum 0 to 1.2 0.01 to 1.2
E351 Test Methods for Chemical Analysis of Cast Iron—
Nickel 0 to 2.0 0.02 to 2.0
Phosphorus 0 to 0.4 0.005 to 0.4
All Types
Silicon 0 to 2.5 0.15 to 2.5
E406 Practice for Using Controlled Atmospheres in Spec-
Sulfur 0 to 0.08 0.01 to 0.08
Tin 0 to 0.14 0.004 to 0.14 trochemical Analysis
Titanium 0 to 0.12 0.003 to 0.12
E826 Practice for Testing Homogeneity of a Metal Lot or
Vanadium 0 to 0.22 0.008 to 0.22
Batch in Solid Form by SparkAtomic Emission Spectrom-
______________
A etry
Quantitative range in accordance with Practice E1601.
E1019 Test Methods for Determination of Carbon, Sulfur,
NOTE 1—The concentration ranges of the elements listed have been
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
established through cooperative testing of reference materials. These
Alloys by Various Combustion and Fusion Techniques
concentration ranges can be extended by the use of suitable reference
E1059 Practice for Designating Shapes and Sizes of Non-
materials.
graphite Counter Electrodes
1.2 This test method covers analysis of specimens having a
E1329 PracticeforVerificationandUseofControlChartsin
diameter adequate to overlap the bore of the spark stand
Spectrochemical Analysis
opening (to effect an argon seal). The specimen thickness
E1601 Practice for Conducting an Interlaboratory Study to
should be sufficient to prevent overheating during excitation.A
Evaluate the Performance of an Analytical Method
heat sink backing may be used. The maximum thickness is
E1763 Guide for Interpretation and Use of Results from
limited only by the height that the stand will permit.
Interlaboratory Testing of Chemical Analysis Methods
1.3 This standard does not purport to address all of the
E1806 Practice for Sampling Steel and Iron for Determina-
safety concerns, if any, associated with its use. It is the
tion of Chemical Composition
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1 2
This test method is under the jurisdiction of ASTM Committee E01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2004. Published Nov. 2004. Originally the ASTM website.
´1 3
approved in 1999. Last previous edition approved in 1999 as E1999 – 99 . DOI: Withdrawn. The last approved version of this historical standard is referenced
10.1520/E1999-99R04. on www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
E1999–99 (2004)
2.2 Other Documents: 7.1.2 Surface Grinder or Sander with Abrasive Belts or
MNL 7 Manual on Presentation of Data and Control Chart Disks,capableofprovidingaflat,clean,uniformsurfaceonthe
Analysis reference materials and specimens.
7.2 Excitation Source, capable of providing sufficient en-
3. Terminology
ergy to sample the specimen and excite the analytes of interest.
See Practice E172. Any other excitation source whose perfor-
3.1 Definitions— For definitions of terms used in this test
mance has been proven to be equivalent may be used.
method, refer to Terminology E135.
7.3 Excitation Chamber, automatically flushed with argon
or other inert support gas. Gases and electrodes are described
4. Summary of Test Method
in 8.1 and 8.2.
4.1 The most sensitive lines for carbon, phosphorus, sulfur
and tin lie in the ultraviolet region. The absorption of the
NOTE 2—Clean the excitation chamber when the counter electrode is
radiation by air in this region is overcome by flushing the spark replaced. Clean the lens or protective window after approximately 200 to
300 excitations, or at a statistically determined time based on intensity
chamber with argon or argon-hydrogen gas mixture and either
loss, to minimize transmission losses.
evaluating all or portions of the spectrometer or filling all or
portions of the spectrometer with an inert gas. A capacitor
7.4 Spectrometer, having sufficient resolving power and
discharge is produced between the flat, ground surface of the linear dispersion to separate clearly the analytical lines from
disk specimen and a conically shaped electrode. The discharge
other lines in the spectrum in the spectral region 170.0 to 500.0
is terminated at a predetermined intensity of a selected iron nm. The spectrometers used to test this method had a disper-
line, or at a predetermined time, and the relative radiant
sion of 0.3 to 0.6 nm/mm and a focal length of 0.5 to 0.75 m.
energies of the analytical lines are recorded and converted to Spectral lines are listed in Table 1. The primary slit width is 15
concentration.
5. Significance and Use
TABLE 1 Analytical and Internal Standard Lines, Possible
Interference
5.1 The chemical composition of cast iron alloys must be
Element Wavelength, nm Reported Possible
determined accurately in order to insure the desired metallur-
Interfering
gical properties. This procedure is suitable for manufacturing
Elements
control and inspection testing.
Carbon 193.093 A1, Mo, Cu, S
6. Interferences
Chromium 267.716 Mo, S, Mn
265.859
6.1 Interferences may vary with spectrometer design and
excitation characteristics. Direct spectral interferences may be
Copper 211.209 Ni
221.81
present on one or more of the wavelengths listed in a method.
327.4 Mo, P
Frequently, these interferences must be determined and proper
510.5 V
correctionsmadebytheuseofvariousreferencematerials.The
Manganese 293.306 Cr, Mo, W
composition of the sample being analyzed should match
closely the composition of one or more of the reference
Molybdenum 202.03 Ni
materials used to prepare and control the calibration curve 281.61 Mn
which is employed. Alternatively, mathematical corrections
Nickel 243.789 Mn
may be used to solve for interelement effects (refer to Practice
231.604 Mn
E158). Various mathematical correction procedures are com- 341.4
352.45 Mo
monly utilized. Any of these is acceptable, which will achieve
analytical accuracy equivalent to that provided by this test
Phosphorus 178.287 Cr, Mn, Mo, Cu
method.
Silicon 212.411 Mo, Cu, Ni
251.612
7. Apparatus
288.16 Mo, Cr
7.1 When required, use sample preparation equipment as
Sulfur 180.731 Mn, Cu, Cr
follows:
7.1.1 Sample Mold, to produce graphite-free white chilled
Tin 189.989 Mn, Mo, Fe
iron samples that are homogeneous, free of voids or porosity in
Titanium 334.904 Cr
theregiontobeexcited,andrepresentativeofthematerialtobe
337.2 Fe
analyzed. A chill-cast disk approximately 40 mm (1 ⁄2 in.) in
334.2
1 1
diameter and 3 to 12-mm ( ⁄8 to ⁄2-in.) thick is satisfactory. A
Vanadium 310.23 Ni
sample mold made from copper with a low oxygen content has
311.07
proventobeoptimumforthispurpose.RefertoPracticeE1806
A
Iron 273.074
for iron sampling procedures.
271.4
281.33
360.89
4 A
ASTM Manual Series, ASTM, 6th Edition, 1990. Internal standard.
E1999–99 (2004)
to 50 µm. Secondary slit width is 15 to 200 µm. The chemical analysis of iron base alloys. Refer to Practice E826
spectrometer shall be provided with one or more of the for information on homogeneity testing of reference materials.
following: 9.2.1 In selecting calibrants, use caution with compositions
7.4.1 Anair/gasinletandavacuumoutlet.Thespectrometer that are unusual. One element may influence adversely the
radiant energy of another element or its uniformity of distri-
shall be operated at a vacuum of 25 µm of mercury or below.
bution within the material. Tests should be made to determine
7.4.2 A gas inlet and a gas outlet.
if interrelations exist between elements in the calibrants. To
7.4.3 Sealed with nitrogen or other inert gas.
compensate for interelement effects, it is suggested that the
7.5 Measuring System, consisting of photomultipliers hav-
calibrants approximate the composition of the material to be
ing individual voltage adjustment, capacitors on which the
tested.
output of each photomultiplier is stored and an electronic
system to measure voltages on the capacitors either directly or
10. Preparation of Calibrants and Specimens
indirectly, and the necessary switching arrangements to pro-
vide the desired sequence of operation.
10.1 Cast graphite-free specimens from molten metal into a
7.6 Readout Console, capable of indicating the ratio of the
suitable mold and cool. The molten metal must be at a high
analytical lines to the internal standard with sufficient precision enoughtemperatureforallcarbontobeinsolution.Preparethe
to produce the accuracy of analysis desired.
surface to be analyzed on a suitable belt or disk grinder.
Prepare the surface of the specimens and reference materials in
7.7 Flushing System, consisting of argon tanks or an argon-
hydrogen gas mixture, a pressure regulator, and a gas flowme- a similar manner. All specimens must be moisture-free for
ter.Automatic sequencing shall be provided to actuate the flow proper excitation in the argon atmosphere.
of argon or argon-hydrogen mixture at a given flow rate for a
NOTE 5—Specimen porosity is undesirable because it leads to the
given time interval and to start the excitation at the end of the
“diffuse-type” rather than the desired “concentrated-type” discharge. The
flush period. Means of changing the flow rate of argon or
specimen surface should be kept clean because the specimen is the
argon-hydrogenmixtureshallbeprovided.Theflushingsystem
electron emitter, and electron emission is inhibited by oily, dirty surfaces.
NOTE 6—Reference materials and specimens shall be refinished dry on
shall be in accordance with Practice E406.
a belt or disc sander before being re-excited on the same area.
7.8 Vacuum Pump, if required, capable of maintaining a
vacuum of 25 µm Hg.
11. Excitation and Exposure
NOTE 3—A pump with a displacement of at least 0.23 m /min (8 ft
11.1 Operate the spectrometer according to the manufactur-
3/min) is usually adequate.
er’s instructions.
NOTE 7—When parameters are established, maintain them carefully.
8. Reagents and Materials
The variation of the power supply voltage shall not exceed 65 % and
8.1 Inert gas, argon, nitrogen, and hydrogen, as required,
preferably should be held within 62%.
must be of sufficient purity to permit proper excitation of the
11.1.1 An example of excitation parameters for a high
analytical lines of interest in the excitation chamber or light
energy undirectional spark source is listed below:
transmittance in the spectrometer chamber. Use in accordance
Preburn Exposure
with Practice E406.
Capacitance, µF 10 10
8.2 Counter Electrodes—A silver or thoriated tungsten rod
Inductance, µH 20 20
Resistance, V 04.4
of 2 to 6-mm diameter ground to a 30 to 90° included angle
Potential, V 550 350
conical tip, which conforms to Practice E1059, has been found
Number of discharges/s 120 60
satisfactory.
11.2 Exposure Conditions (Note 8)—An example of expo-
NOTE 4—Ablack deposit may build up on the tip of the electrode, thus
sure parameters is listed below:
reducing the overall intensity of the spectral radiation. The number of
Preflush period, s 2 to 10
acceptable excitations on an electrode varies from one instrument to
Preburn period, s 5 to 20
another and should be determined in each laboratory. With a thoriated
Exposure period, s 5 to 20
tungsten electrode, it has been reported that a hundred or more excitations
usually can be made before replacement. Cleaning electrodes after each Argon Flow (Note 9)ft /h L/min
Flush 5 to 45 2.5 to 25
burn significantly reduces this buildup and gives more consistent results.
Preburn 5 to 45 2.5 to 25
Exposure 5 to 30 2.5 to 15
9. Reference Materials
NOTE 8—Select preburn and exposure periods after a study of volati-
9.1 Certified Reference Materials, used as calibrants, for
zation rates during specimen excitation. Once established, maintain the
chill-cast iron alloys are available commercially.
parameters consistently.
9.2 Other Calibrants, shall be chemically analyzed test
NOTE 9—A high-purity argon atmosphere is required for the analytical
specimens taken from production heats. They shall cover the gap. Molecular gas impurities, nitrogen, oxygen, hydrocarbons, or water
vapor, either in the gas system or from improperly prepared specimens
concentrationrangesoftheelementstobedeterminedandshall
should be minimized.
include all of the specific types of alloys being analyzed.These
calibrantsshallbehomogeneousandfreeofvoidsandporosity. 11.3 Electrode System— For conventional capacitor dis-
The metallurgical history of the calibrants should be similar to charge excitation systems, the specimen, electrically negative,
that of the specimens being analyzed. Refer to Test Methods serves as one electrode. The opposite electrode is a thoriated
E351 and E1019 or other nationally accepted test methods for tungsten or silver rod, the tip of which has been sharpened to
E1999–99 (2004)
a 30 to 90° included angle cone. Usea3to 6-mm (0.125 to 14. Procedure for Excitation and Radiation Measurement
0.25-in.) gap. Once a gap size is selected, maintain a co
...
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