ASTM E353-93(2000)e1
(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
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:ElementConcentration Range, %Aluminum0.002 to 5.50Boron0.001to 0.20Carbon0.01to 1.50Chromium0.01 to 35.00Cobalt0.01to 15.00Columbium (Niobium)0.01to 4.00Copper0.01to 5.00Lead0.001to 0.50Manganese0.01 to 20.00Molybdenum0.01 to 7.00Nickel0.01to 48.00Nitrogen0.001 to 0.50Phosphorus0.002 to 0.35Selenium0.01 to 0.50Silicon0.01 to 4.00Sulfur0.002to 0.50Tantalum0.01 to 0.80Tin0.001to 0.05Titanium0.01 to 4.50Tungsten0.01 to 4.50Vanadium0.005 to 1.00Zirconium0.001 to 0.20
1.2 The test methods in this standard are contained in the sections indicated below: SectionsAluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to 7.00 %) 119Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003 to 0.20 %) 71Carbon, Total, by the Combustion-Thermal Conductivity Method 2aCarbon, Total, by the Combustion Gravimetric Method (0.05 to 1.50 %)98Chromium by the Atomic Absorption Method (0.006 to 1.00 %)202Chromium by the Peroxydisulfate Oxidation-Titration Method (0.10 to 35.00 %) 212Chromium by the Peroxydisulfate-Oxidation Titrimetric Method2bCobalt by the Ion-Exchange-Potentiometric Titration Method (2 to 15. %) 53Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 5.0 %)61Copper by the Neocuproine Photometric Method (0.01 to 5.00) %) 109Copper by the Sulfide Precipitation-Electrodeposition Gravimetric Method (0.01 to 5.00 %) 82Lead by the Ion-Exchange-Atomic Absorption Method (0.001 to 0.50 %) 127Manganese by the Periodate Photometric Method (0.01 to 5.00 %)8Molybdenum by the Ion Exchange-8-Hydroxyquinoline Gravimetric Method242Molybdenum by the Photometric Method (0.01 to 1.50 %)190Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to 48.0 %)172Phosphorus by the Alkalimetric Method (0.02 to 0.35 %)164Phosphorus by the Molybdenum Blue Photometric Method (0.002 to 0.35 %) 18Silicon by the Gravimetric Method (0.05 to 4.00 %)46Sulfur by the Gravimetric Method2cSulfur by the Combustion-Iodate Titration Method (0.005 to 0.5 %)37Sulfur by the Chromatographic Gravimetric Method2bTin by the Solvent Extraction-Atomic Absorption Method (0.002 to 0.10 %) 180Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.05 %)90Titanium, Total, by the Diantipyrylmethane Spectrophotometric Method (0.01 to 0.35 %)231Vanadium by the Atomic Absorption Method (0.006 to 0.15 %)221
1.3 Test 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 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 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 test methods.
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e1
Designation:E353–93 (Reapproved 2000)
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 E 353; 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 November 2000.
1. Scope
Sections
Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003 to 71
1.1 These test methods cover the chemical analysis of
0.20 %)
2a
stainless, heat-resisting, maraging, and other similar
Carbon, Total, by the Combustion—Thermal Conductivity Method
Carbon, Total, by the Combustion Gravimetric Method (0.05 to 98
chromium-nickel-iron alloys having chemical compositions
1.50 %)
within the following limits:
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 202
Element Concentration Range, % Chromium by the Peroxydisulfate Oxidation—Titration Method (0.10 212
to 35.00 %)
Aluminum 0.002 to 5.50
2b
Boron 0.001 to 0.20 Chromium by the Peroxydisulfate-Oxidation Titrimetric Method
Cobalt by the Ion-Exchange—Potentiometric Titration Method (2 to 53
Carbon 0.01 to 1.50
15. %)
Chromium 0.01 to 35.00
Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 5.0 %) 61
Cobalt 0.01 to 15.00
Copper by the Neocuproine Photometric Method (0.01 to 5.00) %) 109
Columbium (Niobium) 0.01 to 4.00
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric 82
Copper 0.01 to 5.00
Method (0.01 to 5.00 %)
Lead 0.001 to 0.50
Manganese 0.01 to 20.00 Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to 127
0.50 %)
Molybdenum 0.01 to 7.00
Nickel 0.01 to 48.00 Manganese by the Periodate Photometric Method (0.01 to 5.00 %) 8
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravimetric 242
Nitrogen 0.001 to 0.50
Method
Phosphorus 0.002 to 0.35
Molybdenum by the Photometric Method (0.01 to 1.50 %) 190
Selenium 0.01 to 0.50
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to 48.0 %) 172
Silicon 0.01 to 4.00
Phosphorus by the Alkalimetric Method (0.02 to 0.35 %) 164
Sulfur 0.002 to 0.50
Phosphorus by the Molybdenum Blue Photometric Method (0.002 to 18
Tantalum 0.01 to 0.80
0.35 %)
Tin 0.001 to 0.05
Silicon by the Gravimetric Method (0.05 to 4.00 %) 46
Titanium 0.01 to 4.50
2c
Sulfur by the Gravimetric Method
Tungsten 0.01 to 4.50
Sulfur by the Combustion-Iodate Titration Method (0.005 to 0.5 %) 37
Vanadium 0.005 to 1.00
2b
Sulfur by the Chromatographic Gravimetric Method
Zirconium 0.001 to 0.20
Tin by the Solvent Extraction—Atomic Absorption Method (0.002 to 180
1.2 The test methods in this standard are contained in the
0.10 %)
Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.05 %) 90
sections indicated below:
Titanium, Total, by the Diantipyrylmethane Spectrophotometric 231
Sections
Method (0.01 to 0.35 %)
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to 119
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 221
7.00 %)
1.3 Test methods for the determination of several elements
notincludedinthisstandardcanbefoundinTestMethodsE 30
and Test Methods E 1019.
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
1.4 Some of the concentration ranges given in 1.1 are too
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
broad to be covered by a single test method and therefore this
Current edition approved July 15, 1993. Published September 1993. Originally
1 standard contains multiple test methods for some elements.
published as E353 – 68 T. Last previous edition E353 – 89e .
The user must select the proper test method by matching the
These test methods represent revisions of methods covered byASTM Methods
E 30 and E 38 which appear in this publication.
information given in the Scope and Interference sections of
2a
DiscontinuedApril25,1986.ItsreplacementappearsaspartofASTMMethod
each method with the composition of the alloy to be analyzed.
E 1019, found in Annual Book of ASTM Standards, Vol 03.05.
2b
Discontinued May 30, 1980.
2c
Discontinued April 29, 1988.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E353–93 (2000)
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 E 380 Tests
are also used.
1.6 This standard does not purport to address all of the 3. Significance and Use
safety concerns, if any, associated with its use. It is the
3.1 These test methods for the chemical analysis of metals
responsibility of the user of this standard to establish appro-
and alloys are primarily intended as referee methods to test
priate safety and health practices and determine the applica-
such materials for compliance with compositional specifica-
bility of regulatory limitations prior to use. Specific hazards
tions, particularly those under the jurisdiction of ASTM Com-
statements are given in Section 5 and in special “Warning”
mittee A1 on Steel, Stainless Steel, and Related Alloys. It is
paragraphs throughout these test methods.
assumed that all who use these test methods will be trained
analysts capable of performing common laboratory procedures
2. Referenced Documents
skillfully and safely. It is expected that work will be performed
in a properly equipped laboratory under appropriate quality
2.1 ASTM Standards:
D 1193 Specification for Reagent Water control practices such as those described in Guide E 882.
E 29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications 4. Apparatus, Reagents, and Instrumental Practices
E 30 Test Methods for Chemical Analysis of Steel, Cast
4.1 Apparatus—Specialized apparatus requirements are
Iron, Open-Hearth Iron, and Wrought Iron
listed in the “Apparatus” Section in each method. In some
E 50 Practices for Apparatus, Reagents, and Safety Precau-
cases reference may be made to Practices E 50.
tions for Chemical Analysis of Metals
4.2 Reagents:
E 60 Practice for Photometric and Spectrophotometric
4.2.1 Purity of Reagents—Unless otherwise indicated, all
Methods for Chemical Analysis of Metals
reagents used in these test methods shall conform to the
E 173 Practice for Conducting Interlaboratory Studies of
“Reagent Grade” Specifications of the American Chemical
Methods for Chemical Analysis of Metals
Society. Other chemicals may be used, provided it is first
E 350 Test Methods for ChemicalAnalysis of Carbon Steel,
ascertained that they are of sufficiently high purity to permit
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
their use without adversely affecting the expected performance
Wrought Iron
of the determination, as indicated in the section on “Precision
E 351 Test Methods for Chemical Analysis of Cast Iron—
and Bias.”
All Types
4.2.2 Purity of Water— Unless otherwise indicated, refer-
E 352 Test Methods for Chemical Analysis of Tool Steels
ences to water shall be understood to mean reagent water as
and Other Similar Medium- and High-Alloy Steels
defined by Type II of Specification D 1193.
E 354 Test Methods for Chemical Analysis of High-
4.3 Photometric Practice—Photometric prescribed in these
Temperature, Electrical, Magnetic and Other Similar Iron,
test methods shall conform to Practice E 60.
Nickel, and Cobalt Alloys
E 380 Practice for Use of the International System of Units
5. Hazards
(SI) (the Modernized Metric System)
5.1 For precautions to be observed in the use of certain
E 882 Guide for Accountability and Quality Control in the
reagents and equipment in these methods, refer to Practices
Chemical Analysis Laboratory
E 50.
E 1019 Test Methods for Determination of Carbon, Sulfur,
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
6. Sampling
Cobalt Alloys
6.1 For procedures for sampling the material, reference
E 1024 Guide for Chemical Analysis of Metals and Metal
shall be made to Practice E 1806.
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry
7. Interlaboratory Studies and Rounding Calculated
E 1097 Guide for Direct Current Plasma Emission Spec-
Values
trometry Analysis
E 1806 Practice for Sampling Steel and Iron for Determi-
7.1 These test methods have been evaluated using Practice
nation of Chemical Composition
E 173 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 E 29.
3 10
Annual Book of ASTM Standards, Vol 11.01. Available from American National Standards Institute, 11 West 42nd Street,
Annual Book of ASTM Standards, Vol 14.02. 13th Floor, New York, NY 10036.
5 11
Discontinued 1995; see 1994 Annual Book of ASTM Standards, Vol 03.05. “Reagent Chemicals, American Chemical Society Specifications,” Am.
Annual Book of ASTM Standards, Vol 03.05. Chemical Soc., Washington, DC. For suggestions on the testing of Reagents not
Discontinued 1998; see 1997 Annual Book of ASTM Standards, Vol 03.05. listed by the American Chemical Society, see “Reagent Chemicals and Standards,”
Discontinued 1997; see IEEE/ASTM SI 10–Standard, Vol 14.04. by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 03.06. Pharmacopeia,” United States Pharmacopeial Convention, Rockville, MD 20852.
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E353–93 (2000)
MANGANESE BY THE META PERIODATE Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
PHOTOMETRIC METHOD to a 500-mL volumetric flask, dilute to volume, and mix.
13.2 Nitric-Phosphoric Acid Mixture—Cautiously, while
8. Scope
stirring, add 100 mL of HNO and 400 mL of H PO to 400
3 3 4
8.1 This method covers the determination of manganese in mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as
concentrations from 0.01 to 5.00 %. needed.
13.3 Potassium Metaperiodate Solution (7.5 g/L)—
9. Summary of Method
Dissolve 7.5 g of potassium metaperiodate (KIO ) in 200 mL
9.1 Manganous ions are oxidized to permanganate ions by ofhotHNO (1 + 1),add400mLofH PO ,cool,diluteto1L,
3 3 4
treatment with periodate. Tungsten when present at concentra- and mix.
tions greater than 0.5 % is kept in solution with phosphoric 13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
acid. Solutions of the samples are fumed with perchloric acid KIO solution to 1 L of water, mix, heat at not less than 90°C
so that the effect of periodate is limited to the oxidation of for 20 to 30 min, and cool. Use this water to dilute solutions to
manganese. Photometric measurement is made at approxi- volume that have been treated with KIO solution to oxidize
mately 545 nm. manganese, and thus avoid reduction of permanganate ions by
any reducing agents in the untreated water. Caution—Avoid
10. Concentration Range
the use of this water for other purposes.
10.1 The recommended concentration range is 0.15 to 0.8
14. Preparation of Calibration Curve
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
14.1 Calibration Solutions—Using pipets, transfer 5, 10,
or less. 15, 20, and 25 mL of manganese standard solution (1
mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetric
NOTE 1—This method has been written for cells having a 1-cm light
flasks, and if necessary, dilute to approximately 25 mL.
path and a “narrow-band” instrument. The concentration range depends
Proceed as directed in 14.3.
upon band width and spectral region used as well as cell optical path
length. Cells having other dimensions may be used, provided suitable 14.2 Reference Solution—Transfer approximately 25 mL of
adjustments can be made in the amounts of sample and reagents used.
water to a 50-mL borosilicate glass volumetric flask. Proceed
as directed in 14.3.
11. Stability of Color
14.3 Color Development—Add 10 mL of KIO solution,
11.1 The color is stable for at least 24 h.
and heat the solutions at not less than 90°C for 20 to 30 min
(Note 2). Cool, dilute to volume with pretreated water, and
12. Interferences
mix.
12.1 Perchloric acid treatment, which is used in the proce-
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
dure, yields solutions which can be highly colored due to the
means of heating them for the specified period to ensure complete color
presenceofCr(VI)ions.Althoughtheseionsandothercolored
development.
ions in the sample solution undergo no further change in color
14.4 Photometry:
quality upon treatment with metaperiodate ion, the following
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
precautionsmustbeobservedwhenfilterphotometersareused:
tion using the Reference Solution (14.2) in absorption cells
Select a filter with maximum transmittance between 545 and
with a 1-cm light path and using a light band centered at
565 nm. The filter must transmit not more than 5 % of its
approximately545nm.Usingthetestcell,takethephotometric
maximum at a wavelength shorter than 530 nm. The band
readings of the calibration solutions versus the Reference
width of the filter should be less than 30 nm when measured at
Solution (14.2).
50 % of its maximum transmittance. Similar restrictions apply
14.4.2 Single-Cell Photometer—Transfer a suitable portion
with respect to the wavelength region employed when other
of the Reference Solution (14.2) to an absorption cell with a
“wide-band” instruments are used.
1-cm light path and adjust the photometer to the initial setting,
12.2 The spectral transmittance curve of permanganate ions
using a light band centered at approximately 545 nm. While
exhibits two useful minima, one at approximately 526 nm, and
maintaining this adjustment, take the photometric readings of
the other at 545 nm. The latter is recommended when a
the calibration solutions.
“narrow-band” spectrophotometer is used.
14.5 Calibration Curve—Plot the net photometric readings
12.3 Tungsten, when present in amounts of more than 0.5 %
of the calibration solutions against milligrams of manganese
interferes by producing a turbidity in the final solution. A
per 50 mL of solution.
special procedure is provided for use with samples containing
more than 0.5 % tungsten which eliminates the problem by
15. Procedure
preventing the precipitation of the tungsten.
15.1 Test Solution — Select and weigh a sample in accor-
13. Reagents dance with the following:
Tolerance in
13.1 Mangane
...
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