ASTM E352-93(2006)
(Test Method)Standard Test Methods for Chemical Analysis of Tool Steels and Other Similar Medium- and High-Alloy Steels
Standard Test Methods for Chemical Analysis of Tool Steels and Other Similar Medium- and High-Alloy Steels
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 tool steels and other similar medium- and high-alloy steels 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 test 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 0.10 to 5.00 %.
1.7 This test method covers the determination of phosphorus in concentrations from 0.002 to 0.05 %.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E352 − 93 (Reapproved2006)
Standard Test Methods for
Chemical Analysis of Tool Steels and Other Similar Medium-
and High-Alloy Steels
This standard is issued under the fixed designation E352; 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
Copper by the Neocuproine Photometric Method (0.01 to 2.00 %) 89
1.1 These test methods cover the chemical analysis of tool
Copper by the Sulfide Precipitation-
steels and other similar medium- and high-alloy steels having Electrodeposition Gravimetric Method (0.01 to 2.0 %) 70
Lead by the Ion-Exchange—Atomic Absorption
chemical compositions within the following limits:
Method (0.001 to 0.001 %) 99
Element Concentration Range, % Nickel by the Dimethylglyoxime Gravimetric
Aluminum 0.005 to 1.5
Method (0.1 to 4.0 %) 144
Boron 0.001 to 0.10 Manganese by the Periodate Photometric
Carbon 0.03 to 2.50 Method (0.10 to 5.00 %) 8
Chromium 0.10 to 14.0 Molybdenum by the Ion Exchange–8-Hydro-
Cobalt 0.10 to 14.0 xyquinoline Gravimetric Method 203
Copper 0.01 to 2.0 Molybdenum by the Photometric Method (0.01 to 1.50 %) 162
Lead 0.001 to 0.01 Phosphorus by the Alkalimetric Method (0.01 to 0.05 %) 136
Manganese 0.10 to 15.00 Phosphorus by the Molybdenum Blue Photo-
Molybdenum 0.01 to 10.00 metric Method (0.002 to 0.05 %) 18
Nickel 0.02 to 4.00 Silicon by the Gravimetric Method (0.10 to 2.50 %) 45
2c
Nitrogen 0.001 to 0.20 Sulfur by the Gravimetric Method
Phosphorus 0.002 to 0.05 Sulfur by the Combustion-Iodate Titration
Silicon 0.10 to 2.50 Method (0.005 to 0.4 %) 36
Sulfur 0.002 to 0.40 Sulfur by the Chromatographic Gravimetric
2b
Tungsten 0.01 to 21.00 Method
Vanadium 0.02 to 5.50 Tin by the Solvent Extraction—Atomic Absorp-
tion Method (0.002 to 0.10 %) 152
1.2 The test methods in this standard are contained in the
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 193
sections indicated below:
1.3 Test methods for the determination of several elements
Sections
not included in this standard can be found inTest Methods E30
Carbon, Total, by the Combustion—Thermal
2a and Test Methods E1019.
Conductivity Method
Carbon, Total, by the Combustion Gravimetrical
1.4 Some of the concentration ranges given in 1.1 are too
Method (0.05 to 2.50 %) 78
broad to be covered by a single test method and therefore this
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 174
Chromium by the Peroxydisulfate Oxidation—
standard contains multiple test methods for some elements.
Titration Method (0.10 to 14.00 %) 184
The user must select the proper test method by matching the
Chromium by the Peroxydisulfate-Oxidation
2 b
Titrimetric Method information given in the Scope and Interference sections of
Cobalt by the Ion-Exchange—Potentiometric
each test method with the composition of the alloy to be
Titration Method (2 to 14 %) 52
analyzed.
Cobalt by the Nitroso-R-Salt Photometric
Method (0.10 to 5.0 %) 60
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.
These test methods are under the jurisdiction of theASTM Committee E01 on
1.6 This standard does not purport to address all of the
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
safety concerns, if any, associated with its use. It is the
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
responsibility of the user of this standard to establish appro-
Current edition approved June 1, 2006. Published June 2006. Originally
ϵ1
approved in 1968. Last previous edition approved in 2000 as E352 – 93 (2000) .
priate safety and health practices and determine the applica-
DOI: 10.1520/E0352-93R06.
bility of regulatory limitations prior to use. Specific hazards
These test methods represent revisions of methods covered by ASTM E30,
statements are given in Section 5 and in special “Warning”
which appear in this publication. Typical alloy specification numbers for this
category are listed in the Appendix. paragraphs throughout these test methods.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E352 − 93 (2006)
2. Referenced Documents in a properly equipped laboratory under appropriate quality
3 control practices such as those described in Guide E882.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
4. Apparatus, Reagents, and Instrumental Practices
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications 4.1 Apparatus—Specialized apparatus requirements are
listed in the “Apparatus” Section in each method. In some
E30 Test Methods for ChemicalAnalysis of Steel, Cast Iron,
Open-Hearth Iron, and Wrought Iron (Withdrawn 1995) cases reference may be made to Practices E50.
E50 Practices for Apparatus, Reagents, and Safety Consid-
4.2 Reagents:
erations for Chemical Analysis of Metals, Ores, and
4.2.1 Purity of Reagents—Unless otherwise indicated, all
Related Materials
reagents used in these test methods shall conform to the
E60 Practice for Analysis of Metals, Ores, and Related
“Reagent Grade” Specifications of the American Chemical
Materials by Spectrophotometry
Society. Other chemicals may be used, provided it is first
E173 Practice for Conducting Interlaboratory Studies of
ascertained that they are of sufficiently high purity to permit
Methods for Chemical Analysis of Metals (Withdrawn
their use without adversely affecting the expected performance
1998)
of the determination, as indicated in the section on “Precision
E350 Test Methods for Chemical Analysis of Carbon Steel,
and 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
E351 Test Methods for ChemicalAnalysis of Cast Iron—All
defined by Type II of Specification D1193.
Types
4.3 Photometric Practice—Photometric practice prescribed
E353 Test Methods for Chemical Analysis of Stainless,
in these test methods shall conform to Practice E60.
Heat-Resisting, Maraging, and Other Similar Chromium-
Nickel-Iron 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)
E882 Guide for Accountability and Quality Control in the reagents and equipment in these methods, refer to Practices
E50.
Chemical Analysis Laboratory
E1019 Test Methods for Determination of Carbon, Sulfur,
6. Sampling
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
Alloys by Various Combustion and Fusion Techniques
6.1 For procedures for sampling the material, reference
E1024 Guide 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
E1806 Practice for Sampling Steel and Iron for Determina-
Values
tion of Chemical Composition
7.1 These test methods have been evaluated using Practice
2.2 Other Document:
E173 or ISO 5725.
ISO 5725 Precision of Test Methods—Determination of
7.2 Calculated values shall be rounded to the desired num-
Repeatability and Reproducibility for Inter-Laboratory
ber of places as directed in 3.4 to 3.6 of Practice E29.
Tests
MANGANESE BY THE METAPERIODATE
3. Significance and Use
PHOTOMETRIC METHOD
3.1 These test methods for the chemical analysis of metals
8. Scope
and alloys are primarily intended as referee methods to test
such materials for compliance with compositional specifica-
8.1 This method covers the determination of manganese in
tions particularly those under the jurisdiction of ASTM Com-
concentrations from 0.10 to 5.00 %.
mittee A1 on Steel, Stainless Steel, and Related Alloys. It is
assumed that all who use these test methods will be trained
9. Summary of Method
analysts capable of performing common laboratory procedures
9.1 Manganous ions are oxidized to permanganate ions by
skillfully and safely. It is expected that work will be performed
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.
E352 − 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
10. Concentration Range
manganese, and thus avoid reduction of permanganate ions by
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 mL of solution, using a 1-cm cell
(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
exhibits two useful minima, one at approximately 526 nm, and
1-cm light path and adjust the photometer to the initial setting,
the other at 545 nm. The latter is recommended when a
using a light band centered at approximately 545 nm. While
“narrow-band” spectrophotometer is used.
maintaining this adjustment, take the photometric readings of
12.3 Tungsten,whenpresentinamountsofmorethan0.5 %
the calibration solutions.
interferes by producing a turbidity in the final solution. A
14.5 Calibration Curve—Plot the net photometric readings
special procedure is provided for use with samples containing
of the calibration solutions against milligrams of manganese
more than 0.5 % tungsten which eliminates the problem by
per 50 mL of solution.
preventing the precipitation of the tungsten.
15. Procedure
13. Reagents
15.1 Test Solutions—Select and weigh a sample in accor-
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
dance with the following:
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
Tolerance in Dilu- Aliquot
purity manganese (purity: 99.99 % minimum), to a 500-mL
Sample Sample tion, Volume,
Manganese, % Weight, g Weight, mg mL mL
volumetric flask and dissolve in 20 mL of HNO by heating.
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
0.10 to 0.5 0.80 0.5 100 20
to a 500-mL volumetric flask, dilute to volume, and mix.
0.45 to 1.0 0.35 0.3 100 20
0.85 to 2.0 0.80 0.5 500 20
13.2 Nitric-Phosphoric Acid Mixture— Cautiously, while
0.95 to 5.0 0.80 0.5 500 10
stirring, add 100 mL of HNO and 400 mL of H PO to 400
3 3 4
Transfer it to a 300-mL Erlenmeyer flask.
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as
15.1.1 For Samples Containing Not More Than 0.5 %
needed.
Tungsten:
13.3 Potassium Metaperiodate Solution(7.5g/L)—Dissolve 15.1.1.1 To dissolve samples that do not require HF, add 8
7.5 g of potassium metaperiodate (KIO ) in 200 mL of hot to 10 mL of HCl (1+1), and heat. Add HNO as needed to
4 3
HNO (1 + 1), add 400 mL of H PO , cool, dilute to 1 L, and hasten dissolution, and then add 3 to 4 mL in excess. When
3 3 4
mix. dissolution is complete, cool, then add 10 mL of HClO
...
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