ASTM E351-93(2006)
(Test Method)Standard Test Methods for Chemical Analysis of Cast Iron-All Types
Standard Test Methods for Chemical Analysis of Cast Iron-All Types
SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended as referee methods to test such materials for compliance with compositional specifications, particularly those under the jurisdiction of ASTM Committee A04 on Iron Castings. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory under appropriate quality control practices such as those described in Guide E 882.
SCOPE
1.1 These test methods cover the chemical analysis of pig iron, gray cast iron (including alloy and austenitic), white cast iron, malleable cast iron, and ductile (nodular) iron having chemical compositions within the following limits:
1.2 The test methods in this standard are contained in the sections indicated below:
1.3 Procedures for the determination of several elements not included in these test methods can be found in Test Methods E 30 and Test Methods E 1019.
1.4 Some of the concentration ranges given in are too broad to be covered by a single method and therefore this standard contains multiple methods for some elements. The user must select the proper method by matching the information given in the Scope and Interference sections of each method with the composition of the alloy to be analyzed.
1.5 The values stated in SI units are to be regarded as standard. In some cases, exceptions allowed in Practice E 380 are also used.
This 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 and in special "Warning" paragraphs throughout these Methods.
1.6 This test method covers the determination of manganese in concentrations from 0.10 to 2.00 %.
1.7 This method covers the determination of phosphorus in concentrations from 0.02 to 0.90 %.
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Designation: E351 − 93(Reapproved 2006)
Standard Test Methods for
Chemical Analysis of Cast Iron—All Types
This standard is issued under the fixed designation E351; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Carbon, Graphitic, by the Direct Combustion Gravimetric Method (1
1.1 These test methods cover the chemical analysis of pig
to 3 %) 108
iron, gray cast iron (including alloy and austenitic), white cast Carbon, Total by the Combustion Gravimetric Method (1.25 to
4.50 %) 97
iron, malleable cast iron, and ductile (nodular ) iron having
Cerium and Lanthanum by the D-C Plasma Optical Emission
chemical compositions within the following limits:
Method (Ce: 0.003 to 0.5 %; La: 0.001 to 0.30 %) 237
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 208
Element Concentration Range, %
Chromium by the Peroxydisulfate Oxidation—Titration Method
4 (0.006 to 1.00 %) 218
Aluminum 0.003 to 0.50
Chromium by the Peroxydisulfate-Oxidation Titrimetric Method (0.05
Antimony 0.005 to 0.03
4 a
4 to 30.0 %)
Arsenic 0.02 to 0.10
4 Cobalt by the Ion-Exchange—Potentiometric Titration Method (2.0 to
Bismuth 0.001 to 0.03
4 4.5 %) 53
Boron 0.001 to 0.10
Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 4.50 %) 61
Cadmium 0.001 to 0.005
Copper by the Neocuproine Photometric Method (0.03 to 7.5 %) 116
Carbon 1.25 to 4.50
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric
Cerium 0.005 to 0.05
Method (0.03 to 7.5 %) 81
Chromium 0.01 to 30.00
4 Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to
Cobalt 0.01 to 4.50
0.15 %) 126
Copper 0.03 to 7.50
4 Magnesium by the Atomic Absorption Method (0.002 to 0.10 %) 71
Lead 0.001 to 0.15
Manganese by the Periodate Photometric Method (0.10 to 2.00 %) 8
Magnesium 0.002 to 0.10
Manganese by the Peroxydisulfate-Arsenite Titrimetric Method (0.10
Manganese 0.06 to 2.50
to 3.5 %) 152
Molybdenum 0.01 to 5.00
Molybdenum by the Ion Exchange–8-Hydroxyquinoline Gravimetric
Nickel 0.01 to 36.00
Method 257
Phosphorus 0.01 to 0.90
4 Molybdenum by the Photometric Method (0.01 to 1.5 %) 196
Selenium 0.001 to 0.06
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Silicon 0.10 to 6.0
36.00 %) 168
Sulfur 0.005 to 0.25
Nickel by the Ion Exchange-Atomic Absorption Method (0.005 to
Tellurium 0.001 to 0.35
4 1.00 %) 176
Tin 0.001 to 0.35
Phosphorus by the Alkalimetric Method (0.02 to 0.90 %) 160
Titanium 0.001 to 0.20
Phosphorus by the Molybdenum Blue Photometric Method (0.02 to
Tungsten 0.001 to 0.20
0.90 %) 18
Vanadium 0.005 to 0.50
Silicon by the Gravimetric Method (0.1 to 6.0 %) 46
Zinc 0.005 to 0.20
Sulfur by the Gravimetric Method 30
1.2 The test methods in this standard are contained in the Sulfur by the Combustion-Iodate Titration Method (0.005 to 0.25 %) 37
4 b
Sulfur by the Chromatographic Gravimetric Method
sections indicated below:
Tin by the Solvent Extraction-Atomic Absorption Method (0.002 to
Sections
0.10 %) 186
Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.35 %) 89
Titanium, Total, by the Diantipyrylmethane Spectrophotometric
Method (0.006 to 0.35 %) 246
These test methods are under the jurisdiction of ASTM Committee E01 on
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 227
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
1.3 Proceduresforthedeterminationofseveralelementsnot
Current edition approved June 1, 2006. Published June 2006. Originally
ε1
approved in 1968. Last previous edition approved in 2000 as E351–93(2000) . included in these test methods can be found in Test Methods
DOI: 10.1520/E0351-93R06.
E30 and Test Methods E1019.
These test methods represent revisions of methods covered by Test Methods
E30, which appear in this publication. Typical alloy specification numbers for this
1.4 Some of the concentration ranges given in 1.1 are too
category are listed in the Appendix.
3 broad to be covered by a single method and therefore this
As typified by compositions listed in Cast Metals Handbook, 1957, pp.
196–197. standard contains multiple methods for some elements. The
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E351 − 93 (2006)
user must select the proper method by matching the informa- 2.2 Other Document:
tion given in the Scope and Interference sections of each ISO 5725Precision of Test Methods—Determination of
method with the composition of the alloy to be analyzed. Repeatability and Reproducibility for Inter-Laboratory
Tests
1.5 The values stated in SI units are to be regarded as
standard. In some cases, exceptions allowed in Practice E380
3. Significance and Use
are also used.
3.1 These test methods for the chemical analysis of metals
1.6 This standard does not purport to address all of the
and alloys are primarily intended as referee methods to test
safety concerns, if any, associated with its use. It is the
such materials for compliance with compositional
responsibility of the user of this standard to establish appro-
specifications, particularly those under the jurisdiction of
priate safety and health practices and determine the applica-
ASTM CommitteeA04 on Iron Castings. It is assumed that all
bility of regulatory limitations prior to use. Specific hazards
who use these test methods will be trained analysts capable of
statements are given in Section 5 and in special “Warning”
performing common laboratory procedures skillfully and
paragraphs throughout these Methods.
safely. It is expected that work will be performed in a properly
equippedlaboratoryunderappropriatequalitycontrolpractices
2. Referenced Documents
such as those described in Guide E882.
2.1 ASTM Standards:
D1193Specification for Reagent Water
4. Apparatus, Reagents, and Instrumental Practices
E29Practice for Using Significant Digits in Test Data to
4.1 Apparatus—Specialized apparatus requirements are
Determine Conformance with Specifications
listed in the Apparatus section in each method. In some cases
E30TestMethodsforChemicalAnalysisofSteel,CastIron,
reference may be made to Practices E50.
Open-Hearth Iron, and Wrought Iron.
4.2 Reagents:
E50Practices for Apparatus, Reagents, and Safety Consid-
4.2.1 Purity of Reagents—Unless otherwise indicated, all
erations for Chemical Analysis of Metals, Ores, and
reagents used in these test methods shall conform to the
Related Materials
Reagent Grade Specifications of theAmerican Chemical Soci-
E60Practice for Analysis of Metals, Ores, and Related
ety. Other chemicals may be used, provided it is first ascer-
Materials by Spectrophotometry
tained that they are of sufficiently high purity to permit their
E173Practice for Conducting Interlaboratory Studies of
use without adversely affecting the expected performance of
Methods for Chemical Analysis of Metals
thedetermination,asindicatedinthesectionon“Precisionand
E350Test Methods for Chemical Analysis of Carbon Steel,
Bias.”
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
4.2.2 Purity of Water—Unless otherwise indicated, refer-
Wrought Iron
ences to water shall be understood to mean reagent water as
E352TestMethodsforChemicalAnalysisofToolSteelsand
defined by Type II of Specification D1193.
Other Similar Medium- and High-Alloy Steels
E353Test Methods for Chemical Analysis of Stainless,
4.3 Photometric Practice—Photometric practice prescribed
Heat-Resisting, Maraging, and Other Similar Chromium-
in these test methods shall conform to Practice E60.
Nickel-Iron Alloys
E380Practice for Use of the International System of Units
5. Hazards
(SI) (Modernized Metric System)
5.1 For precautions to be observed in the use of certain
E882Guide for Accountability and Quality Control in the
reagents and equipment in these methods, refer to Practices
Chemical Analysis Laboratory
E50.
E1019Test Methods for Determination of Carbon, Sulfur,
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
6. Sampling
Alloys by Various Combustion and Fusion Techniques
6.1 For procedures for sampling the material, reference
E1024Guide for Chemical Analysis of Metals and Metal
shall be made to Practice E1806.
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry (Withdrawn 2004)
7. Interlaboratory Studies and Rounding Calculated
E1806Practice for Sampling Steel and Iron for Determina-
Values
tion of Chemical Composition
7.1 These test methods have been evaluated using Practice
E173 or ISO 5725.
4 7
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4th Floor, New York, NY 10036, http://www.ansi.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Reagent Chemicals, American Chemical Society Specifications , American
Standards volume information, refer to the standard’s Document Summary page on
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
the ASTM website.
listed by the American Chemical Society, see Analar Standards for Laboratory
Withdrawn. The last approved version of this historical standard is referenced
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
on www.astm.org.
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
E351 − 93 (2006)
7.2 Calculated values shall be rounded to the desired num- Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
ber of places as directed in 3.4 to 3.6 of Practice E29. to a 500-mL volumetric flask, dilute to volume, and mix.
13.2 Nitric-Phosphoric Acid Mixture—Cautiously, while
stirring,add100mLofHNO and400mLofH PO to400mL
MANGANESE BY THE METAPERIODATE 3 3 4
ofwater.Cool,diluteto1L,andmix.Preparefreshasneeded.
PHOTOMETRIC METHOD
13.3 Potassium Metaperiodate Solution(7.5g/L)—Dissolve
8. Scope
7.5 g of potassium metaperiodate (KIO ) in 200 mL of hot
8.1 Thistestmethodcoversthedeterminationofmanganese HNO (1+1), add 400 mL of H PO , cool, dilute to 1 L, and
3 3 4
in concentrations from 0.10 to 2.00 %.
mix.
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
9. Summary of Method
KIO solution to 1 L of water, mix, heat at not less than 90°C
9.1 Manganous ions are oxidized to permanganate ions by
for20to30min,andcool.Usethiswatertodilutesolutionsto
reaction with metaperiodate ions. Solutions of the samples are
volume that have been treated with KIO solution to oxidize
fumed with perchloric acid so that the effect of metaperiodate
manganese, and thus avoid reduction of permanganate ions by
ion is limited to the oxidation of manganese. Photometric
any reducing agents in the untreated water. Warning—Avoid
measurement is made at approximately 545 nm.
the use of this water for other purposes.
10. Concentration Range
14. Preparation of Calibration Curve
10.1 The recommended concentration range is 0.15 to 0.8
14.1 Calibration Solutions—Usingpipets,transfer5,10,15,
mg of manganese per 50 mL of solution, using a 1-cm cell
20, and 25 mL of manganese standard solution (1 mL=0.032
(Note 1) and a spectrophotometer with a band width of 10 nm
mg Mn) to 50-mL borosilicate glass volumetric flasks, and, if
or less.
necessary, dilute to approximately 25 mL. Proceed as directed
in 14.3.
NOTE 1—This method has been written for cells having a 1-cm light
path and a narrow-band instrument. The concentration range depends
14.2 Reference Solution—Transfer approximately 25 mL of
upon band width and spectral region used as well as cell optical path
water to a 50-mL borosilicate glass volumetric flask. Proceed
length. Cells having other dimensions may be used, provided suitable
as directed in 14.3.
adjustments can be made in the amounts of sample and reagents used.
14.3 Color Development—Add 10 mL of KIO solution,
11. Stability of Color
and heat the solutions at not less than 90°C for 20 to 30 min
11.1 The color is stable for at least 24 h. (Note 2). Cool, dilute to volume with pretreated water, and
mix.
12. Interferences
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
12.1 The elements ordinarily present do not interfere. Per-
means of heating them for the specified period to ensure complete color
chloric acid treatment, which is used in the procedure, yields development.
solutionswhichcanbehighlycoloredduetothepresenceofCr
14.4 Photometry:
(VI) ions. Although these ions and other colored ions in the
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
sample solution undergo no further change in color quality
tion using the Reference Solution (14.2) in absorption cells
upon treatment with metaperiodate ion, the following precau-
with a 1-cm light path and using a light band centered at
tionsmustbeobservedwhenfilterphotometersareused:Select
approximately545nm.Usingthetestcell,takethephotometric
afilterwithmaximumtransmittancebetween545and565nm.
readings of the calibration solutions versus the Reference
The filter must transmit not more than 5% of its maximum at
Solution (14.2).
a wavelength shorter than 530 nm.The band width of the filter
14.4.2 Single-Cell Photometer—Transfer a suitable portion
should be less than 30 nm when measured at 50% of its
of the Reference Solution (14.2) to an absorption cell with a
maximum transmittance. Similar restrictions apply with re-
1-cm light path and adjust the photometer to the initial setting,
spect to the wavelength region employed when other wide-
using a light band centered at approximately 545 nm. While
band instruments are used.
maintaining this adjustment, take the photometric readings of
the calibration solutions.
12.2 The spectral transmittance curve of permanganate ions
exhibits two useful minima, one at approximately 526 nm, and
14.5 Calibration Curve—Plot the net photometric readings
the other at 545 nm. The latter is recommended when a
of the calibration solutions against milligrams of manganese
narrow-band spectrophotometer is used.
per 50 mL of solution.
13. Reagents 15. Procedure
13.1 Manganese, Standard Solution (1 mL=0.032 mg
15.1 Test Solution:
Mn)—Transfer the equivalent of 0.4000 g of assayed, high- 15.1.1 Select and weigh a sample in accordance with the
purity manganese (purity: 99.99% minimum), to a 500-mL following:
volumetric flask and dissolve in 20 mL of HNO by heating.
...
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