ASTM E352-93(2000)e1
(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
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:Element Concentration Range, %Aluminum0.005 to 1.5Boron 0.001 to 0.10Carbon 0.03 to 2.50Chromium0.10 to 14.0Cobalt 0.10 to 14.0Copper 0.01 to 2.0Lead 0.001 to 0.01Manganese0.10 to 15.00Molybdenum0.01 to 10.00Nickel 0.02 to 4.00Nitrogen0.001 to 0.20Phosphorus0.002 to 0.05Silicon 0.10 to 2.50Sulfur 0.002 to 0.40Tungsten0.01 to 21.00Vanadium0.02 to 5.50
1.2 The test methods in this standard are contained in the sections indicated below:SectionsCarbon, Total, by the Combustion-ThermalConductivity Method2aCarbon, Total, by the Combustion GravimetricalMethod (0.05 to 2.50 %) 78Chromium by the Atomic Absorption Method(0.006 to 1.00 %)174Chromium by the Peroxydisulfate Oxidation-Titration Method(0.10 to 14.00 %)184Chromium by the Peroxydisulfate-OxidationTitrimetric Method2 bCobalt by the Ion-Exchange-PotentiometricTitration Method (2 to 14 %)52Cobalt by the Nitroso-R-Salt PhotometricMethod(0.10 to 5.0 %)60Copper by the Neocuproine Photometric Method (0.01 to 2.00 %) 89Copper by the Sulfide Precipitation-Electrodeposition Gravimetric Method (0.01 to 2.0 %)70Lead by the Ion-Exchange-Atomic AbsorptionMethod (0.001 to 0.001 %)99Nickel by the Dimethylglyoxime GravimetricMethod(0.1 to 4.0 %)144Manganese by the Periodate PhotometricMethod(0.10 to 5.00 %)8Molybdenum by the Ion Exchange-8-Hydro-xyquinoline Gravimetric Method 203Molybdenum by the Photometric Method(0.01 to 1.50 %)162Phosphorus by the Alkalimetric Method(0.01 to 0.05 %)136Phosphorus by the Molybdenum Blue Photo-metric Method (0.002 to 0.05 %)18Silicon by the Gravimetric Method(0.10 to 2.50 %)45Sulfur by the Gravimetric Method 2cSulfur by the Combustion-Iodate TitrationMethod(0.005 to 0.4 %)36Sulfur by the Chromatographic GravimetricMethod 2bTin by the Solvent Extraction-Atomic Absorp-tion Method (0.002 to 0.10 %)152Vanadium by the Atomic Absorption Method(0.006 to 0.15 %)193
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 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 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:E352–93 (Reapproved 2000)
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 E 352; 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
Cobalt by the Nitroso-R-Salt Photometric
1.1 These test methods cover the chemical analysis of tool
Method (0.10 to 5.0 %) 60
steels and other similar medium- and high-alloy steels having
Copper by the Neocuproine Photometric Method (0.01 to 2.00 %) 89
Copper by the Sulfide Precipitation-
chemical compositions within the following limits:
Electrodeposition Gravimetric Method (0.01 to 2.0 %) 70
Element Concentration Range, %
Lead by the Ion-Exchange—Atomic Absorption
Aluminum 0.005 to 1.5
Method (0.001 to 0.001 %) 99
Boron 0.001 to 0.10
Nickel by the Dimethylglyoxime Gravimetric
Carbon 0.03 to 2.50
Method (0.1 to 4.0 %) 144
Chromium 0.10 to 14.0
Manganese by the Periodate Photometric
Cobalt 0.10 to 14.0
Method (0.10 to 5.00 %) 8
Copper 0.01 to 2.0
Molybdenum by the Ion Exchange–8-Hydro-
Lead 0.001 to 0.01
xyquinoline Gravimetric Method 203
Manganese 0.10 to 15.00
Molybdenum by the Photometric Method (0.01 to 1.50 %) 162
Molybdenum 0.01 to 10.00
Phosphorus by the Alkalimetric Method (0.01 to 0.05 %) 136
Nickel 0.02 to 4.00
Phosphorus by the Molybdenum Blue Photo-
Nitrogen 0.001 to 0.20
metric Method (0.002 to 0.05 %) 18
Phosphorus 0.002 to 0.05
Silicon by the Gravimetric Method (0.10 to 2.50 %) 45
2c
Silicon 0.10 to 2.50
Sulfur by the Gravimetric Method
Sulfur 0.002 to 0.40
Sulfur by the Combustion-Iodate Titration
Tungsten 0.01 to 21.00
Method (0.005 to 0.4 %) 36
Vanadium 0.02 to 5.50
Sulfur by the Chromatographic Gravimetric
2b
Method
1.2 The test methods in this standard are contained in the
Tin by the Solvent Extraction—Atomic Absorp-
sections indicated below: tion Method (0.002 to 0.10 %) 152
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 193
Sections
Carbon, Total, by the Combustion—Thermal
1.3 Test methods for the determination of several elements
2a
Conductivity Method
notincludedinthisstandardcanbefoundinTestMethodsE 30
Carbon, Total, by the Combustion Gravimetrical
Method (0.05 to 2.50 %) 78 and Test Methods E 1019.
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 174
1.4 Some of the concentration ranges given in 1.1 are too
Chromium by the Peroxydisulfate Oxidation—
broad to be covered by a single test method and therefore this
Titration Method (0.10 to 14.00 %) 184
Chromium by the Peroxydisulfate-Oxidation
standard contains multiple test methods for some elements.
2b
Titrimetric Method
The user must select the proper test method by matching the
Cobalt by the Ion-Exchange—Potentiometric
information given in the Scope and Interference sections of
Titration Method (2 to 14 %) 52
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
These test methods are under the jurisdiction of theASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
standard. In some cases, exceptions allowed in Practice E 380
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
are also used.
Current edition approved July 15, 1993. Published September 1993. Originally
e1
1.6 This standard does not purport to address all of the
published as E 352 – 68 T. Last previous edition E 352 – 89 .
These test methods represent revisions of methods covered by ASTM E 30, safety concerns, if any, associated with its use. It is the
which appear in this publication. Typical alloy specification numbers for this
responsibility of the user of this standard to establish appro-
category are listed in the Appendix.
priate safety and health practices and determine the applica-
2a
Discontinued April 25, 1986. Its replacement appears as part of ASTM
bility of regulatory limitations prior to use. Specific hazards
Methods 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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E352–93 (2000)
statements are given in Section 5 and in special “Warning” such materials for compliance with compositional specifica-
paragraphs throughout these test methods. tions particularly those under the jurisdiction of ASTM Com-
mittee A1 on Steel, Stainless Steel, and Related Alloys. It is
2. Referenced Documents
assumed that all who use these test methods will be trained
analysts capable of performing common laboratory procedures
2.1 ASTM Standards:
skillfully and safely. It is expected that work will be performed
D 1193 Specification for Reagent Water
in a properly equipped laboratory under appropriate quality
E 29 Practice for Using Significant Digits in Test Data to
control practices such as those described in Guide E 882.
Determine Conformance with Specifications
E 30 Test Methods for Chemical Analysis of Steel, Cast
4. Apparatus, Reagents, and Instrumental Practices
Iron, Open-Hearth Iron, and Wrought Iron
4.1 Apparatus—Specialized apparatus requirements are
E 50 Practices for Apparatus, Reagents, and Safety Precau-
listed in the “Apparatus” Section in each method. In some
tions for Chemical Analysis of Metals
cases reference may be made to Practices E 50.
E 60 Practice for Photometric and Spectrophotometric
6 4.2 Reagents:
Methods for Chemical Analysis of Metals
4.2.1 Purity of Reagents—Unless otherwise indicated, all
E 173 Practice for Conducting Interlaboratory Studies of
7 reagents used in these test methods shall conform to the
Methods for Chemical Analysis of Metals
“Reagent Grade” Specifications of the American Chemical
E 350 Test Methods for ChemicalAnalysis of Carbon Steel,
Society. Other chemicals may be used, provided it is first
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
6 ascertained that they are of sufficiently high purity to permit
Wrought Iron
their use without adversely affecting the expected performance
E 351 Test Methods for Chemical Analysis of Cast Iron—
6 of the determination, as indicated in the section on “Precision
All Types
and Bias.”
E 353 Test Methods for Chemical Analysis of Stainless,
4.2.2 Purity of Water—Unless otherwise indicated, refer-
Heat-Resisting, Maraging, and Other Similar Chromium-
6 ences to water shall be understood to mean reagent water as
Nickel-Iron Alloys
defined by Type II of Specification D 1193.
E 354 Test Methods for Chemical Analysis of High-
4.3 Photometric Practice—Photometric practice prescribed
Temperature, Electrical, Magnetic and Other Similar Iron,
in these 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-
7. Interlaboratory Studies and Rounding Calculated
tometry
Values
E 1097 Guide for Direct Current Plasma Emission Spec-
trometry Analysis
7.1 These test methods have been evaluated using Practice
E 1806 Practice for Sampling Steel and Iron for Determi- E 173 or ISO 5725.
nation of Chemical Compostion
7.2 Calculated values shall be rounded to the desired num-
2.2 Other Document:
ber of places as directed in 3.4 to 3.6 of Practice E 29.
ISO 5725 Precision of Test Methods—Determination of
MANGANESE BY THE METAPERIODATE
Repeatability and Reproducibility for Inter-Laboratory
PHOTOMETRIC METHOD
Tests
8. Scope
3. Significance and Use
8.1 This method covers the determination of manganese in
3.1 These test methods for the chemical analysis of metals
concentrations from 0.10 to 5.00 %.
and alloys are primarily intended as referee methods to test
9. Summary of Method
9.1 Manganous ions are oxidized to permanganate ions by
treatment with periodate. Tungsten when present at concentra-
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.02. tions greater than 0.5 % is kept in solution with phosphoric
Discontinued 1995; see 1994 Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.05.
7 11
Discontinued 1998; see 1997 Annual Book of ASTM Standards, Vol 03.05. “Reagent Chemicals,American Chemical Society Specifications,”Am. Chem-
Discontinued 1997; see IEEE/ASTM SI 10–Standard, Vol 14.04. ical Soc., Washington, DC. For suggestions on the testing of Reagents not listed by
Annual Book of ASTM Standards, Vol 03.06. theAmerican Chemical Society, see“ Reagent Chemicals and Standards,” by Joseph
Available from American National Standards Institute, 11 West 42nd Street, Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
13th Floor, New York, NY 10036. Pharmacopeia.” United States Pharmacopeial Convention, Rockville, MD 20852.
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E352–93 (2000)
acid. Solutions of the samples are fumed with perchloric acid 13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
so that the effect of periodate is limited to the oxidation of KIO solution to 1 L of water, mix, heat at not less than 90°C
manganese. Photometric measurement is made at approxi- for 20 to 30 min, and cool. Use this water to dilute solutions to
mately 545 nm. 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
the use of this water for other purposes.
10.1 The recommended concentration range is 0.15 to 0.8
mg of manganese per 50 mL of solution, using a 1-cm cell
14. Preparation of Calibration Curve
(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
NOTE 1—This method has been written for cells having a 1-cm light
mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetric
path and a “narrow-band” instrument. The concentration range depends
flasks, and, if necessary, dilute to approximately 25 mL.
upon band width and spectral region used as well as cell optical path
Proceed as directed in 14.3.
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,whenpresentinamountsofmorethan0.5 %
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 Solutions—Select and weigh a sample in accor-
dance with the following:
13. Reagents
Tolerance in Dilu- Aliquot
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
Sample Sample tion, Volume,
Manganese, % Weight, g Weight, mg mL mL
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
purity manganese (purity: 99.99 % minimum), to a 500-mL
0.10 to 0.5 0.80 0.5 100 20
volumetric flask and dissolve in 20 mL of HNO by heating.
0.45 to 1.0 0.35 0.3 100 20
0.85 to 2.0 0.80 0.5 500 20
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
0.95 to 5.0 0.80 0.5 500 10
to a 500-mL volumetric flask, dilute to volume, and mix.
13.2 Nitric-Phosphoric Acid Mixture— Cautiously, while Transfer it to a 300-mL Erlenmeyer flask.
stirring, add 100 mL of HNO and 400 mL of H PO to 400 15.1.1 For Samples Containing Not More Than 0.5 %
3 3 4
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as Tungsten:
needed. 15.1.1.1 To dissolve samples that do not require HF, add 8
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