ASTM E351-93(2000)e1
(Test Method)Standard Test Methods for Chemical Analysis of Cast Iron--All Types
Standard Test Methods for Chemical Analysis of Cast Iron--All Types
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:Element Concentration Range, %Aluminum40.003 to 0.50Antimony0.005 to 0.03Arsenic40.02 to 0.10Bismuth40.001 to 0.03Boron40.001 to 0.10Cadmium40.001 to0.005Carbon 1.25 to 4.50Cerium40.005 to 0.05Chromium0.01 to 30.00Cobalt40.01 to 4.50Copper 0.03 to 7.50Lead40.001 to 0.15Magnesium0.002 to 0.10Manganese0.06 to 2.50Molybdenum0.01 to 5.00Nickel 0.01 to 36.00Phosphorus0.01 to 0.90Selenium40.001 to 0.06Silicon 0.10 to 6.0Sulfur 0.005 to 0.25Tellurium40.001 to 0.35Tin40.001 to 0.35Titanium40.001 to 0.20Tungsten40.001 to 0.20Vanadium40.005 to 0.50Zinc40.005 to 0.20
1.2 The test methods in this standard are contained in the sections indicated below: SectionsCarbon, Graphitic, by the Direct Combustion Gravimetric Method (1 to 3 %) 108Carbon, Total by the Combustion Gravimetric Method (1.25 to 4.50 %) 97Cerium and Lanthanum by the D-C Plasma Optical Emission Method (Ce: 0.003 to 0.5 %; La: 0.001 to 0.30 %)237Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 208Chromium by the Peroxydisulfate Oxidation-Titration Method (0.006 to 1.00 %) 218Chromium by the Peroxydisulfate-Oxidation Titrimetric Method (0.05 to 30.0 %) 4a Cobalt by the Ion-Exchange-Potentiometric Titration Method (2.0 to 4.5 %) 53Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 4.50 %) 61Copper by the Neocuproine Photometric Method (0.03 to 7.5 %) 116Copper by the Sulfide Precipitation-Electrodeposition Gravimetric Method (0.03 to 7.5 %) 81Lead by the Ion-Exchange-Atomic Absorption Method (0.001 to 0.15 %) 126Magnesium by the Atomic Absorption Method (0.002 to 0.10 %) 71Manganese by the Periodate Photometric Method (0.10 to 2.00 %) 8Manganese by the Peroxydisulfate-Arsenite Titrimetric Method (0.10 to 3.5 %) 152Molybdenum by the Ion Exchange-8-Hydroxyquinoline Gravimetric Method 257Molybdenum by the Photometric Method (0.01 to 1.5 %) 196Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to 36.00 %) 168Nickel by the Ion Exchange-Atomic Absorption Method (0.005 to 1.00 %) 176Phosphorus by the Alkalimetric Method (0.02 to 0.90 %) 160Phosphorus by the Molybdenum Blue Photometric Method (0.02 to 0.90 %) 18Silicon by the Gravimetric Method (0.1 to 6.0 %) 46Sulfur by the Gravimetric Method 30Sulfur by the Combustion-Iodate Titration Method (0.005 to 0.25 %) 37Sulfur by the Chromatographic Gravimetric Method 4bTin by the Solvent Extraction-Atomic Absorption Method (0.002 to 0.10 %) 186Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.35 %) 89Titanium, Total, by the Diantipyrylmethane Spectrophotometric Method (0.006 to 0.35 %) 246Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 227
1.3 Methods for the determination of several elements not included in this standard can be found in Test Methods E30 and Test Methods E1019.
1.4 Some of the concentration ranges given in 1.1 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 E380 are also used.
1.6 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 5 and in special "Warning" paragraphs throughout these Methods.
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e1
Designation:E351–93 (Reapproved 2000)
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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—Editorial changes were made in November 2000.
1. Scope
Sections
1.1 These test methods cover the chemical analysis of pig
Carbon, Graphitic, by the Direct Combustion Gravimetric Method (1
iron, gray cast iron (including alloy and austenitic), white cast
to 3 %) 108
Carbon, Total by the Combustion Gravimetric Method (1.25 to
iron, malleable cast iron, and ductile (nodular ) iron having
4.50 %) 97
chemical compositions within the following limits:
Cerium and Lanthanum by the D-C Plasma Optical Emission
Element Concentration Range, % 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
Aluminum 0.003 to 0.50 Chromium by the Peroxydisulfate Oxidation—Titration Method
(0.006 to 1.00 %) 218
Antimony 0.005 to 0.03
Chromium by the Peroxydisulfate-Oxidation Titrimetric Method (0.05
Arsenic 0.02 to 0.10
4 4a
to 30.0 %)
Bismuth 0.001 to 0.03
Cobalt by the Ion-Exchange—Potentiometric Titration Method (2.0 to
Boron 0.001 to 0.10
4.5 %) 53
Cadmium 0.001 to 0.005
Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 4.50 %) 61
Carbon 1.25 to 4.50
Copper by the Neocuproine Photometric Method (0.03 to 7.5 %) 116
Cerium 0.005 to 0.05
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric
Chromium 0.01 to 30.00
Method (0.03 to 7.5 %) 81
Cobalt 0.01 to 4.50
Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to
Copper 0.03 to 7.50
0.15 %) 126
Lead 0.001 to 0.15
Magnesium by the Atomic Absorption Method (0.002 to 0.10 %) 71
Magnesium 0.002 to 0.10
Manganese by the Periodate Photometric Method (0.10 to 2.00 %) 8
Manganese 0.06 to 2.50
Manganese by the Peroxydisulfate-Arsenite Titrimetric Method (0.10
Molybdenum 0.01 to 5.00
to 3.5 %) 152
Nickel 0.01 to 36.00
Molybdenum by the Ion Exchange–8-Hydroxyquinoline Gravimetric
Phosphorus 0.01 to 0.90
Method 257
Selenium 0.001 to 0.06
Molybdenum by the Photometric Method (0.01 to 1.5 %) 196
Silicon 0.10 to 6.0
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Sulfur 0.005 to 0.25
36.00 %) 168
Tellurium 0.001 to 0.35
Nickel by the Ion Exchange-Atomic Absorption Method (0.005 to
Tin 0.001 to 0.35
1.00 %) 176
Titanium 0.001 to 0.20
Phosphorus by the Alkalimetric Method (0.02 to 0.90 %) 160
Tungsten 0.001 to 0.20
Phosphorus by the Molybdenum Blue Photometric Method (0.02 to
Vanadium 0.005 to 0.50
0.90 %) 18
Zinc 0.005 to 0.20
Silicon by the Gravimetric Method (0.1 to 6.0 %) 46
1.2 The test methods in this standard are contained in the Sulfur by the Gravimetric Method 30
Sulfur by the Combustion-Iodate Titration Method (0.005 to 0.25 %) 37
sections indicated below :
4b
Sulfur by the Chromatographic Gravimetric Method
Tin by the Solvent Extraction-Atomic Absorption Method (0.002 to
0.10 %) 186
These test methods are under the jurisdiction of ASTM Committee E01 on Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.35 %) 89
Titanium, Total, by the Diantipyrylmethane Spectrophotometric
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
Method (0.006 to 0.35 %) 246
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 227
Current edition approved July 15, 1993. Published September 1993. Originally
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published as E351–68T. Last previous edition E351–89 .
1.3 Methods for the determination of several elements not
These test methods represent revisions of methods covered by Test Methods
included in this standard can be found in Test Methods E30
E30, which appear in this publication. Typical alloy specification numbers for this
category are listed in the Appendix.
and Test Methods E1019.
As typified by compositions listed in Cast Metals Handbook, 1957, pp.
1.4 Some of the concentration ranges given in 1.1 are too
196–197.
broad to be covered by a single method and therefore this
a Discontinued.
4b Discontinued as of April 29, 1988. 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.
e1
E351–93 (2000)
user must select the proper method by matching the informa- nation of Chemical Composition
tion given in the Scope and Interference sections of each 2.2 Other Document:
method with the composition of the alloy to be analyzed. ISO 5725 Precision of Test Methods—Determination of
1.5 The values stated in SI units are to be regarded as Repeatability and Reproducibility for Inter-Laboratory
standard. In some cases, exceptions allowed in Practice E380 Tests
are also used.
3. Significance and Use
1.6 This standard does not purport to address all of the
3.1 These test methods for the chemical analysis of metals
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- and alloys are primarily intended as referee methods to test
such materials for compliance with compositional specifica-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards tions, particularly those under the jurisdiction ofASTM Com-
mittee on Iron Castings. It is assumed that all who use these
statements are given in Section 5 and in special “Warning”
paragraphs throughout these Methods. test methods will be trained analysts capable of performing
common laboratory procedures skillfully and safely. It is
2. Referenced Documents expected that work will be performed in a properly equipped
laboratory under appropriate quality control practices such as
2.1 ASTM Standards:
those described in Guide E882.
D1193 Specifications for Reagent Water
E29 Practice for Using Significant Digits in Test Data to
4. Apparatus, Reagents, and Instrumental Practices
Determine Conformance with Specifications
4.1 Apparatus—Specialized apparatus requirements are
E30 Test Methods for Chemical Analysis of Steel, Cast
7 listed in the “Apparatus” Section in each method. In some
Iron, Open-Hearth Iron, and Wrought Iron
cases reference may be made to Practices E50.
E50 Practices forApparatus, Reagents, and Safety Precau-
8 4.2 Reagents:
tions for Chemical Analysis of Metals
4.2.1 Purity of Reagents—Unless otherwise indicated, all
E 60 Practice for Photometric and Spectrophotometric
8 reagents used in these test methods shall conform to the
Methods for Chemical Analysis of Metals
“Reagent Grade” Specifications of the American Chemical
E173 Practice for Conducting Interlaboratory Studies of
9 Society. Other chemicals may be used, provided it is first
Methods for Chemical Analysis of Metals
ascertained that they are of sufficiently high purity to permit
E350 TestMethodsforChemicalAnalysisofCarbonSteel,
their use without adversely affecting the expected performance
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
of the determination, as indicated in the section on “Precision
Wrought Iron
and Bias.”
E352 Test Methods for Chemical Analysis of Tool Steels
4.2.2 Purity of Water—Unless otherwise indicated, refer-
and Other Similar Medium- and High-Alloy Steels
ences to water shall be understood to mean reagent water as
E353 Test Methods for Chemical Analysis of Stainless,
defined by Type II of Specification D1193.
Heat-Resisting, Maraging, and Other Similar Chromium-
8 4.3 Photometric Practice—Photometric practice prescribed
Nickel-Iron Alloys
in these test methods shall conform to Practice E60.
E354 Test Methods for Chemical Analysis of High Tem-
perature, Electrical, Magnetic, and Other Similar Iron,
5. Hazards
Nickel, and Cobalt Alloys
5.1 For precautions to be observed in the use of certain
E380 Practice for Use of the International System of Units
10 reagents and equipment in these methods, refer to Practices
(SI) (the Modernized Metric System)
E50.
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
6. Sampling
E1019 Test Methods for Determination of Carbon, Sulfur,
6.1 For procedures for sampling the material, reference
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
shall be made to Practice E1806.
Cobalt Alloys
E1024 Guide for Chemical Analysis of Metals and Metal
7. Interlaboratory Studies and Rounding Calculated
Bearing Ores by Flame Atomic Absorption Spectropho-
Values
tometry
7.1 These test methods have been evaluated using Practice
E1097 Guide for Direct Current Plasma Emission Spec-
E173 or ISO 5725.
trometry Analysis
E1806 Practice for Sampling Steel and Iron for Determi-
Annual Book of ASTM Standards, Vol 03.06.
Available from American National Standards Institute, 11 West 42nd Street,
13th Floor, New York, NY 10036.
5 13
Annual Book of ASTM Standards, Vol 11.01. Reagent Chemicals, American Chemical Society Specifications, American
Annual Book of ASTM Standards, Vol 14.02. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Discontinued 1995; see 1994 Annual Book of ASTM Standards, Vol 03.05. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 03.05. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Discontinued 1998; see 1997 Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Discontinued 1997; see IEEE/ASTM SI 10–Standard, Vol 14.04. MD.
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E351–93 (2000)
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
MANGANESE BY THE METAPERIODATE
stirring, add 100 mL of HNO and 400 mL of H PO to 400
3 3 4
PHOTOMETRIC METHOD
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as
needed.
8. Scope
13.3 Potassium Metaperiodate Solution (7.5 g/L)—
8.1 This method covers the determination of manganese in
Dissolve 7.5 g of potassium metaperiodate (KIO ) in 200 mL
concentrations from 0.10 to 2.00 %.
ofhotHNO (1+1),add400mLofH PO ,cool,diluteto1L,
3 3 4
and mix.
9. Summary of Method
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
9.1 Manganous ions are oxidized to permanganate ions by
KIO solution to 1 L of water, mix, heat at not less than 90°C
reaction with metaperiodate ions. Solutions of the samples are
for 20 to 30 min, and cool. Use this water to dilute solutions to
fumed with perchloric acid so that the effect of metaperiodate
volume that have been treated with KIO solution to oxidize
ion is limited to the oxidation of manganese. Photometric
manganese, and thus avoid reduction of permanganate ions by
measurement is made at approximately 545 nm.
any reducing agents in the untreated water. Caution—Avoid
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—Using pipets, transfer 5, 10,
mg of manganese per 50 mL of solution, using a 1-cm cell
15, 20, and 25 mL of manganese standard solution (1
(Note 1) and a spectrophotometer with a band width of 10 nm
mL=0.032 mg Mn) to 50-mL borosilicate glass volumetric
or less.
flasks, and, if necessary, dilute to approximately 25 mL.
NOTE 1—This method has been written for cells having a 1-cm light
Proceed as directed in 14.3.
path and a “narrow-band” instrument. The concentration range depends
14.2 Reference Solution—Transfer approximately 25 mLof
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
a filter with maximum transmittance between 545 and 565 nm.
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
12.2 The spectral transmittance curve of permanganate ions
the calibration solutions.
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
...
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