ASTM E353-93(2006)
(Test Method)Standard Test Methods for Chemical Analysis of Stainless, Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron Alloys
Standard Test Methods for Chemical Analysis of Stainless, Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron Alloys
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 A1 on Steel, Stainless Steel, and Related Alloys. 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 stainless, heat-resisting, maraging, and other similar chromium-nickel-iron alloys having chemical compositions within the following limits:
1.3 Test methods for the determination of several elements not included in this standard 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 test method and therefore this standard contains multiple test methods for some elements. The user must select the proper test 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 test methods.
1.6 This method covers the determination of manganese in concentrations from 0.01 to 5.00 %.
1.7 This method covers the determination of phosphorus in concentrations from 0.002 to 0.35 %.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E353 − 93(Reapproved 2006)
Standard Test Methods for
Chemical Analysis of Stainless, Heat-Resisting, Maraging,
and Other Similar Chromium-Nickel-Iron Alloys
This standard is issued under the fixed designation E353; 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
Sections
2b
Chromium by the Peroxydisulfate-Oxidation Titrimetric Method
1.1 These test methods cover the chemical analysis of
Cobalt by the Ion-Exchange—Potentiometric Titration Method (2 to 53
stainless, heat-resisting, maraging, and other similar 15. %)
Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 5.0 %) 61
chromium-nickel-iron alloys having chemical compositions
Copper by the Neocuproine Photometric Method (0.01 to 5.00) %) 109
within the following limits:
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric 82
Method (0.01 to 5.00 %)
Element Concentration Range, %
Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to 127
Aluminum 0.002 to 5.50
0.50 %)
Boron 0.001 to 0.20
Manganese by the Periodate Photometric Method (0.01 to 5.00 %) 8
Carbon 0.01 to 1.50
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravimetric 242
Chromium 0.01 to 35.00
Method
Cobalt 0.01 to 15.00
Molybdenum by the Photometric Method (0.01 to 1.50 %) 190
Columbium (Niobium) 0.01 to 4.00
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to 48.0 %) 172
Copper 0.01 to 5.00
Phosphorus by the Alkalimetric Method (0.02 to 0.35 %) 164
Lead 0.001 to 0.50
Phosphorus by the Molybdenum Blue Photometric Method (0.002 to 18
Manganese 0.01 to 20.00
0.35 %)
Molybdenum 0.01 to 7.00
Silicon by the Gravimetric Method (0.05 to 4.00 %) 46
Nickel 0.01 to 48.00
2c
Sulfur by the Gravimetric Method
Nitrogen 0.001 to 0.50
Sulfur by the Combustion-Iodate Titration Method (0.005 to 0.5 %) 37
Phosphorus 0.002 to 0.35
2b
Sulfur by the Chromatographic Gravimetric Method
Selenium 0.01 to 0.50
Tin by the Solvent Extraction—Atomic Absorption Method (0.002 to 180
Silicon 0.01 to 4.00
0.10 %)
Sulfur 0.002 to 0.50
Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.05 %) 90
Tantalum 0.01 to 0.80
Titanium, Total, by the Diantipyrylmethane Spectrophotometric 231
Tin 0.001 to 0.05
Method (0.01 to 0.35 %)
Titanium 0.01 to 4.50
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 221
Tungsten 0.01 to 4.50
Vanadium 0.005 to 1.00
1.3 Test methods for the determination of several elements
Zirconium 0.001 to 0.20
not included in this standard can be found inTest Methods E30
1.2 The test methods in this standard are contained in the
and Test Methods E1019.
sections indicated below:
1.4 Some of the concentration ranges given in 1.1 are too
Sections
broad to be covered by a single test method and therefore this
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to 119
7.00 %)
standard contains multiple test methods for some elements.
Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003 to 71
The user must select the proper test method by matching the
0.20 %)
2a
information given in the Scope and Interference sections of
Carbon, Total, by the Combustion—Thermal Conductivity Method
Carbon, Total, by the Combustion Gravimetric Method (0.05 to 98 each method with the composition of the alloy to be analyzed.
1.50 %)
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 202 1.5 The values stated in SI units are to be regarded as
Chromium by the Peroxydisulfate Oxidation—Titration Method (0.10 212
standard. In some cases, exceptions allowed in Practice E380
to 35.00 %)
are also used.
1.6 This standard does not purport to address all of the
These test methods are under the jurisdiction of ASTM Committee E01 on
safety concerns, if any, associated with its use. It is the
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of the user of this standard to establish appro-
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved June 1, 2006. Published June 2006. Originally
priate safety and health practices and determine the applica-
ϵ1
approved in 1968. Last previous edition approved in 2000 as E353 – 93 (2000) .
bility of regulatory limitations prior to use. Specific hazards
DOI: 10.1520/E0353-93R06.
2 statements are given in Section 5 and in special “Warning”
These test methods represent revisions of methods covered byASTM Methods
E30 and E38 which appear in this publication. paragraphs throughout these test methods.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E353 − 93 (2006)
2. Referenced Documents proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
3 performed in a properly equipped laboratory under appropriate
2.1 ASTM Standards:
quality control practices such as those described in Guide
D1193 Specification for Reagent Water
E882.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
4. Apparatus, Reagents, and Instrumental Practices
E30 Test Methods for ChemicalAnalysis of Steel, Cast Iron,
4.1 Apparatus—Specialized apparatus requirements are
Open-Hearth Iron, and Wrought Iron (Withdrawn 1995)
listed in the “Apparatus” Section in each method. In some
E50 Practices for Apparatus, Reagents, and Safety Consid-
cases reference may be made to Practices E50.
erations for Chemical Analysis of Metals, Ores, and
Related Materials 4.2 Reagents:
E60 Practice for Analysis of Metals, Ores, and Related
4.2.1 Purity of Reagents—Unless otherwise indicated, all
Materials by Spectrophotometry reagents used in these test methods shall conform to the
E173 Practice for Conducting Interlaboratory Studies of
“Reagent Grade” Specifications of the American Chemical
Methods for Chemical Analysis of Metals (Withdrawn Society. Other chemicals may be used, provided it is first
1998)
ascertained that they are of sufficiently high purity to permit
E350 Test Methods for Chemical Analysis of Carbon Steel,
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.”
E351 Test Methods for ChemicalAnalysis of Cast Iron—All
4.2.2 Purity of Water— Unless otherwise indicated, refer-
Types
ences to water shall be understood to mean reagent water as
E352 TestMethodsforChemicalAnalysisofToolSteelsand
defined by Type II of Specification D1193.
Other Similar Medium- and High-Alloy Steels
4.3 Photometric Practice—Photometric prescribed in these
E354 Test Methods for Chemical Analysis of High-
test methods shall conform to Practice E60.
Temperature,Electrical,Magnetic,andOtherSimilarIron,
Nickel, and Cobalt Alloys
5. Hazards
E380 Practice for Use of the International System of Units
5.1 For precautions to be observed in the use of certain
(SI) (the Modernized Metric System) (Withdrawn 1997)
reagents and equipment in these methods, refer to Practices
E882 Guide for Accountability and Quality Control in the
E50.
Chemical Analysis Laboratory
E1019 Test Methods for Determination of Carbon, Sulfur,
6. Sampling
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
6.1 For procedures for sampling the material, reference
Alloys by Various Combustion and Fusion Techniques
shall be made to Practice E1806.
E1024 Guide for Chemical Analysis of Metals and Metal
Bearing Ores by Flame Atomic Absorption Spectropho-
7. Interlaboratory Studies and Rounding Calculated
tometry (Withdrawn 2004)
Values
E1806 Practice for Sampling Steel and Iron for Determina-
7.1 These test methods have been evaluated using Practice
tion of Chemical Composition
E173 or ISO 5725.
2.2 Other Document:
7.2 Calculated values shall be rounded to the desired num-
ISO 5725 Precision of Test Methods—Determination of
ber of places as directed in 3.4 to 3.6 of Practice E29.
Repeatability and Reproducibility for Inter-Laboratory
Tests
MANGANESE BY THE META PERIODATE
PHOTOMETRIC METHOD
3. Significance and Use
3.1 These test methods for the chemical analysis of metals
8. Scope
and alloys are primarily intended as referee methods to test
8.1 This method covers the determination of manganese in
such materials for compliance with compositional
concentrations from 0.01 to 5.00 %.
specifications, particularly those under the jurisdiction of
ASTM Committee A1 on Steel, Stainless Steel, and Related
9. Summary of Method
Alloys. It is assumed that all who use these test methods will
9.1 Manganous ions are oxidized to permanganate ions by
be trained analysts capable of performing common laboratory
treatment with periodate. Tungsten when present at concentra-
tions greater than 0.5 % is kept in solution with phosphoric
acid. Solutions of the samples are fumed with perchloric acid
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. “Reagent Chemicals,American Chemical Society Specifications,”Am. Chemi-
The last approved version of this historical standard is referenced on cal Soc., Washington, DC. For suggestions on the testing of Reagents not listed by
www.astm.org. theAmerican Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
4th Floor, New York, NY 10036, http://www.ansi.org. Pharmacopeia,” United States Pharmacopeial Convention, Rockville, MD 20852.
E353 − 93 (2006)
so that the effect of periodate is limited to the oxidation of 13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
manganese. Photometric measurement is made at approxi- KIO solution to 1 L of water, mix, heat at not less than 90°C
mately 545 nm. for 20 to 30 min, and cool. Use this water to dilute solutions to
volume that have been treated with KIO solution to oxidize
manganese, and thus avoid reduction of permanganate ions by
10. Concentration Range
any reducing agents in the untreated water. Caution—Avoid
10.1 The recommended concentration range is 0.15 to 0.8
the use of this water for other purposes.
mg of manganese per 50 mLof solution, using a 1-cm cell (see
Note 1) and a spectrophotometer with a band width of 10 nm
14. Preparation of Calibration Curve
or less.
14.1 Calibration Solutions—Usingpipets,transfer5,10,15,
NOTE 1—This method has been written for cells having a 1-cm light
20, and 25 mL of manganese standard solution (1 mL = 0.032
path and a “narrow-band” instrument. The concentration range depends
mg Mn) to 50-mL borosilicate glass volumetric flasks, and if
upon band width and spectral region used as well as cell optical path
necessary, dilute to approximately 25 mL. Proceed as directed
length. Cells having other dimensions may be used, provided suitable
adjustments can be made in the amounts of sample and reagents used. in 14.3.
14.2 Reference Solution—Transfer approximately 25 mL of
11. Stability of Color
water to a 50-mL borosilicate glass volumetric flask. Proceed
11.1 The color is stable for at least 24 h. as directed in 14.3.
14.3 Color Development—Add 10 mL of KIO solution,
12. Interferences
and heat the solutions at not less than 90°C for 20 to 30 min
12.1 Perchloric acid treatment, which is used in the (Note 2). Cool, dilute to volume with pretreated water, and
procedure, yields solutions which can be highly colored due to mix.
the presence of Cr (VI) ions. Although these ions and other
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
colored ions in the sample solution undergo no further change
means of heating them for the specified period to ensure complete color
in color quality upon treatment with metaperiodate ion, the
development.
following precautions must be observed when filter photom-
14.4 Photometry:
eters are used: Select a filter with maximum transmittance
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
between 545 and 565 nm. The filter must transmit not more
tion using the Reference Solution (14.2) in absorption cells
than 5 % of its maximum at a wavelength shorter than 530 nm.
with a 1-cm light path and using a light band centered at
The band width of the filter should be less than 30 nm when
approximately545nm.Usingthetestcell,takethephotometric
measured at 50 % of its maximum transmittance. Similar
readings of the calibration solutions versus the Reference
restrictions apply with respect to the wavelength region em-
Solution (14.2).
ployed when other “wide-band” instruments are used.
14.4.2 Single-Cell Photometer—Transfer a suitable portion
12.2 The spectral transmittance curve of permanganate ions of the Reference Solution (14.2) to an absorption cell with a
1-cm light path and adjust the photometer to the initial setting,
exhibits two useful minima, one at approximately 526 nm, and
the other at 545 nm. The latter is recommended when a using a light band centered at approximately 545 nm. While
maintaining this adjustment, take the photometric readings of
“narrow-band” spectrophotometer is used.
the calibration solutions.
12.3 Tungsten,whenpresentinamountsofmorethan0.5 %
14.5 Calibration Curve—Plot the net photometric readings
interferes by producing a turbidity in the final solution. A
of the calibration solutions against milligrams of manganese
special procedure is provided for use with samples containing
per 50 mL of solution.
more than 0.5 % tungsten which eliminates the problem by
preventing the precipitation of the tungsten.
15. Procedure
13. Reagents
15.1 Test Solution— Select and weigh a sample in accor-
dance with the following:
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
Tolerance in
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
Sample Sample Dilution, Aliquot
purity manganese (purity: 99.99 % minimum), to a 500-mL
Manganese, % Weight, g Weight, mg mL Volume, mL
volumetric flask and dissolve in 20 mL of HNO by heating.
0.01 to 0.5 0.80 0.5 100 20
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
0.45 to 1.0 0.35 0.3 100 20
to a 500-mL volumetric flask, dilute to volume, and mix.
0.85 to 2.0 0.80 0.5 500 20
1.95 to 5.0 0.80 0.5 500 10
13.2 Nitric-Phosphoric Acid Mixture—Cautiously, while
stirring,add100mLofHNO and400mLofH PO to400mL
Transfer it to a 300-mL Erlenmeyer flask.
3 3 4
of water. Cool, dilute to 1 L, and mix. Prepare fres
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