ASTM E1999-99e1
(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
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
Standard Test Method for
Analysis of Cast Iron Using Optical Emission Spectrometry
This standard is issued under the fixed designation E 1999; 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.
e NOTE—Editorial changes were made in October 2000.
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 E 135 Terminology Relating to Analytical Chemistry for
technique for the following elements in the concentration Metals, Ores, and Related Materials
ranges shown (Note 1): E 158 Practice for Fundamental Calculations to Convert
Intensities into Concentrations in Optical Emission Spec-
Concentration Ranges, %
A
Elements Applicable Range, % Quantitative Range, %
trochemical Analysis
E 172 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
E 305 Practice for Establishing and Controlling Spectro-
Manganese 0 to 1.8 0.03 to 1.8
chemical Analytical Curves
Molybdenum 0 to 1.2 0.01 to 1.2
E 351 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
E 406 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
E 826 PracticeforTestingHomogeneityofMaterialsforthe
Vanadium 0 to 0.22 0.008 to 0.22
Development of Reference Materials
______________
E 1019 Test Methods for Determination of Carbon, Sulfur,
A
Quantitative range in accordance with Practice E 1601.
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
NOTE 1—The concentration ranges of the elements listed have been
Cobalt Alloys
established through cooperative testing of reference materials. These
E 1059 Practice for Designating Shapes and Sizes of Non-
concentration ranges can be extended by the use of suitable reference
graphite Counter Electrodes
materials.
E 1329 Practice for Verification and Use of Control Charts
1.2 This test method covers analysis of specimens having a
in Spectrochemical Analysis
diameter adequate to overlap the bore of the spark stand
E 1601 Practice for Conducting an Interlaboratory Study to
opening (to effect an argon seal). The specimen thickness
Evaluate the Performance of an Analytical Method
should be sufficient to prevent overheating during excitation.A
E 1763 Guide for Interpretation and Use of Results from
heat sink backing may be used. The maximum thickness is
Interlaboratory Testing of Chemical Analysis Methods
limited only by the height that the stand will permit.
E 1806 Practice for Sampling Steel and Iron for Determi-
1.3 This standard does not purport to address all of the
nation of Chemical Composition
safety concerns, if any, associated with its use. It is the
2.2 Other Documents:
responsibility of the user of this standard to establish appro-
MNL 7 Manual on Presentation of Data and Control Chart
priate safety and health practices and determine the applica-
Analysis
bility of regulatory limitations prior to use.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee E-01 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analytical Chemistry for Metals, Ores and Related Materials and is the direct Standards volume information, refer to the standard’s Document Summary page on
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. the ASTM website.
Current edition approved Jan. 10, 1999. Published March 1999. ASTM Manual Series, ASTM, 6th Edition, 1990.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
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3. Terminology 7.3 Excitation Chamber, automatically flushed with argon
or other inert support gas. Gases and electrodes are described
3.1 Definitions— For definitions of terms used in this test
in 8.1 and 8.2.
method, refer to Terminology E 135.
NOTE 2—Clean the excitation chamber when the counter electrode is
4. Summary of Test Method
replaced. Clean the lens or protective window after approximately 200 to
300 excitations, or at a statistically determined time based on intensity
4.1 The most sensitive lines for carbon, phosphorus, sulfur
loss, to minimize transmission losses.
and tin lie in the ultraviolet region. The absorption of the
radiation by air in this region is overcome by flushing the spark 7.4 Spectrometer, having sufficient resolving power and
linear dispersion to separate clearly the analytical lines from
chamber with argon or argon-hydrogen gas mixture and either
evaluating all or portions of the spectrometer or filling all or other lines in the spectrum in the spectral region 170.0 to 500.0
nm. The spectrometers used to test this method had a disper-
portions of the spectrometer with an inert gas. A capacitor
discharge is produced between the flat, ground surface of the sion of 0.3 to 0.6 nm/mm and a focal length of 0.5 to 0.75 m.
Spectral lines are listed in Table 1. The primary slit width is 15
disk specimen and a conically shaped electrode. The discharge
is terminated at a predetermined intensity of a selected iron to 50 µm. Secondary slit width is 15 to 200 µm. The
spectrometer shall be provided with one or more of the
line, or at a predetermined time, and the relative radiant
following:
energies of the analytical lines are recorded and converted to
7.4.1 Anair/gasinletandavacuumoutlet.Thespectrometer
concentration.
shall be operated at a vacuum of 25 µm of mercury or below.
5. Significance and Use
7.4.2 A gas inlet and a gas outlet.
7.4.3 Sealed with nitrogen or other inert gas.
5.1 The chemical composition of cast iron alloys must be
determined accurately in order to insure the desired metallur-
gical properties. This procedure is suitable for manufacturing
TABLE 1 Analytical and Internal Standard Lines, Possible
control and inspection testing.
Interference
Element Wavelength, nm Reported Possible
6. Interferences
Interfering
6.1 Interferences may vary with spectrometer design and
Elements
excitation characteristics. Direct spectral interferences may be
Carbon 193.093 A1, Mo, Cu, S
present on one or more of the wavelengths listed in a method.
Chromium 267.716 Mo, S, Mn
Frequently, these interferences must be determined and proper
265.859
correctionsmadebytheuseofvariousreferencematerials.The
Copper 211.209 Ni
composition of the sample being analyzed should match
221.81
closely the composition of one or more of the reference
327.4 Mo, P
materials used to prepare and control the calibration curve
510.5 V
which is employed. Alternatively, mathematical corrections
Manganese 293.306 Cr, Mo, W
may be used to solve for interelement effects (refer to Practice
E 158). Various mathematical correction procedures are com-
Molybdenum 202.03 Ni
281.61 Mn
monly utilized. Any of these is acceptable, which will achieve
analytical accuracy equivalent to that provided by this test
Nickel 243.789 Mn
method.
231.604 Mn
341.4
352.45 Mo
7. Apparatus
Phosphorus 178.287 Cr, Mn, Mo, Cu
7.1 When required, use sample preparation equipment as
follows:
Silicon 212.411 Mo, Cu, Ni
7.1.1 Sample Mold, to produce graphite-free white chilled
251.612
288.16 Mo, Cr
iron samples that are homogeneous, free of voids or porosity in
theregiontobeexcited,andrepresentativeofthematerialtobe
Sulfur 180.731 Mn, Cu, Cr
analyzed. A chill-cast disk approximately 40 mm (1 ⁄2 in.) in
1 1
diameter and 3 to 12-mm ( ⁄8 to ⁄2-in.) thick is satisfactory. A Tin 189.989 Mn, Mo, Fe
sample mold made from copper with a low oxygen content has
Titanium 334.904 Cr
proven to be optimum for this purpose. Refer to Practice
337.2 Fe
334.2
E 1806 for iron sampling procedures.
7.1.2 Surface Grinder or Sander with Abrasive Belts or
Vanadium 310.23 Ni
Disks,capableofprovidingaflat,clean,uniformsurfaceonthe
311.07
reference materials and specimens.
A
Iron 273.074
7.2 Excitation Source, capable of providing sufficient en-
271.4
ergy to sample the specimen and excite the analytes of interest.
281.33
360.89
See Practice E 172. Any other excitation source whose perfor-
A
mance has been proven to be equivalent may be used. Internal standard.
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E1999–99
7.5 Measuring System, consisting of photomultipliers hav- compensate for interelement effects, it is suggested that the
ing individual voltage adjustment, capacitors on which the calibrants approximate the composition of the material to be
output of each photomultiplier is stored and an electronic tested.
system to measure voltages on the capacitors either directly or
indirectly, and the necessary switching arrangements to pro-
10. Preparation of Calibrants and Specimens
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
enough temperature for all carbon to be in solution. Prepare the
to produce the accuracy of analysis desired.
surface to be analyzed on a suitable belt or disk grinder.
7.7 Flushing System, consisting of argon tanks or an argon-
Prepare the surface of the specimens and reference materials in
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
given time interval and to start the excitation at the end of the
NOTE 5—Specimen porosity is undesirable because it leads to 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.
shall be in accordance with Practice E 406.
NOTE 6—Reference materials and specimens shall be refinished dry on
7.8 Vacuum Pump, if required, capable of maintaining a
a belt or disc sander before being re-excited on the same area.
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
3/min) is usually adequate.
11.1 Operate the spectrometer according to the manufactur-
er’s instructions.
8. Reagents and Materials
NOTE 7—When parameters are established, maintain them carefully.
8.1 Inert gas, argon, nitrogen, and hydrogen, as required,
The variation of the power supply voltage shall not exceed 65 % and
must be of sufficient purity to permit proper excitation of the
preferably should be held within 62%.
analytical lines of interest in the excitation chamber or light
transmittance in the spectrometer chamber. Use in accordance
11.1.1 An example of excitation parameters for a high
with Practice E 406.
energy undirectional spark source is listed below:
8.2 Counter Electrodes—A silver or thoriated tungsten rod
Preburn Exposure
Capacitance, µF 10 10
of 2 to 6-mm diameter ground to a 30 to 90° included angle
Inductance, µH 20 20
conical tip, which conforms to Practice E 1059, has been found
Resistance, V 04.4
satisfactory.
Potential, V 550 350
Number of discharges/s 120 60
NOTE 4—Ablack deposit may build up on the tip of the electrode, thus
reducing the overall intensity of the spectral radiation. The number of 11.2 Exposure Conditions (Note 8)—An example of expo-
acceptable excitations on an electrode varies from one instrument to
sure parameters is listed below:
another and should be determined in each laboratory. With a thoriated
Preflush period, s 2 to 10
tungsten electrode, it has been reported that a hundred or more excitations
Preburn period, s 5 to 20
usually can be made before replacement. Cleaning electrodes after each
Exposure period, s 5 to 20
burn significantly reduces this buildup and gives more consistent results.
Argon Flow (Note 9) ft /h L/min
Flush 5 to 45 2.5 to 25
9. Reference Materials
Preburn 5 to 45 2.5 to 25
Exposure 5 to 30 2.5 to 15
9.1 Certified Reference Materials, used as calibrants, for
chill-cast iron alloys are available commercially.
NOTE 8—Select preburn and exposure periods after a study of volati-
9.2 Other Calibrants, shall be chemically analyzed test zation rates during specimen excitation. Once established, maintain the
parameters consistently.
specimens taken from production heats. They shall cover the
NOTE 9—A high-purity argon atmosphere is required for the analytical
concentrationrangesoftheelementstobedeterminedandshall
gap. Molecular gas impurities, nitrogen, oxygen, hydrocarbons, or water
include all of the specific types of alloys being analyzed.These
vapor, either in the gas system or from improperly prepared specimens
calibrantsshallbehomogeneousandfreeofvoidsandporosity.
should be minimized.
The metallurgical history of the calibrants should be similar to
that of the specimens being analyzed. Refer to Test Methods
11.3 Electrode System— For conventional capacitor dis-
E 351 and E 1019 or other nationally accepted test methods for
charge excitation systems, the specimen, electrically negative,
chemical analysis of iron base alloys. Refer to Practice E 826
serves as one electrode. The opposite electrode is a thoriated
for information on homogeneity testing of reference materials.
tungsten or silver rod, the tip of which has been sharpened to
9.2.1 In selecting calibrants, use caution with compositions a 30 to 90° included angle cone. Usea3to 6-mm (0.125 to
that are unusual. One element may influence adversely the 0.25-in.) gap. Once a gap size is selected, maintain a consistent
radiant energy of another element or its uniformity of distri- gap. Center the analytical gap on the optical axes of the
bution within the material. Tests should be made to determine spectrometer. Condition a fresh counter electrode with 2 to 6
if interrelations exist between elements in the calibrants. To excitations using the conditions given in 11.1 and 11.2.
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12. Preparation of Apparatus element if their difference does not exceed twice th
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