ASTM E354-93(2006)
(Test Method)Standard Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron, Nickel, and Cobalt Alloys
Standard Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron, Nickel, and Cobalt 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 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 high-temperature, electrical, magnetic, and other similar iron, nickel, and cobalt alloys having chemical compositions within the following limits:
1.3 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 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 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 0.05 to 2.00 percent.
1.7 This method covers the determination of phosphorus in concentrations from 0.002 to 0.08 %.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E354 − 93(Reapproved 2006)
Standard Test Methods for
Chemical Analysis of High-Temperature, Electrical,
Magnetic, and Other Similar Iron, Nickel, and Cobalt Alloys
This standard is issued under the fixed designation E354; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
Chromium by the Peroxydisulfate Oxidation—Titration Method
(0.10 to 33.00 %)
1.1 These test methods cover the chemical analysis of 1b
Chromium by the Peroxydisulfate-Oxidation Titrimetric Method
high-temperature, electrical, magnetic, and other similar iron, Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to
75 %)
nickel, and cobalt alloys having chemical compositions within
Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to 5.0 %) 61
the following limits:
Copper by Neocuproine Photometric Method (0.01 to 10.00 %) 90
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric
Concentration
Element
Method (0.01 to 10.00 %)
Range, %
Iron by the Silver ReductionTitrimetric Method (1.0 to 50.0 %) 192
Manganese by the Periodate Photometric Method (0.05 to 2.00 %) 8
Aluminum 0.005 to 18.00
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravi-
Beryllium 0.001 to 0.05
metric Method (1.5 to 30 %)
Boron 0.001 to 1.00
Molybdenum by the Photometric Method (0.01 to 1.50 %) 153
Calcium 0.002 to 0.05
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Carbon 0.001 to 1.10
84.0 %)
Chromium 0.10 to 33.00
Phosphorus by the Molybdenum Blue Photometric Method (0.002
Cobalt 0.10 to 75.00
to 0.08 %)
Columbium (Niobium) 0.01 to 6.0
Silicon by the Gravimetric Method (0.05 to 5.00 %) 46
Copper 0.01 to 10.00
1 c
Sulfur by the Gravimetric Method
Iron 0.01 to 85.00
Magnesium 0.001 to 0.05
Sulfur by the Combustion-Iodate Titration Method (0.005 to
Manganese 0.01 to 3.0
0.1 %)
Molybdenum 0.01 to 30.0
1b
Sulfur by the Chromatographic Gravimetric Method
Nickel 0.10 to 84.0
Tin by the Solvent Extraction–Atomic Absorption Method (0.002
Nitrogen 0.001 to 0.20
to 0.10 %)
Phosphorus 0.002 to 0.08
Silicon 0.01 to 5.00
1.3 Methods for the determination of several elements not
Sulfur 0.002 to 0.10
includedinthisstandardcanbefoundinTestMethodsE30and
Tantalum 0.005 to 10.0
Titanium 0.01 to 5.00 Test Methods E1019.
Tungsten 0.01 to 18.00
Vanadium 0.01 to 3.25 1.4 Some of the concentration ranges given in 1.1 are too
Zirconium 0.01 to 2.50
broad to be covered by a single method and therefore this
1.2 The test methods in this standard are contained in the
standard contains multiple methods for some elements. The
sections indicated below:
user must select the proper method by matching the informa-
tion given in the Scope and Interference sections of each
Sections
method with the composition of the alloy to be analyzed.
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to
7.00 %)
1.5 The values stated in SI units are to be regarded as
1a
Carbon,Total, by the Combustion-Thermal Conductivity Method
standard. In some cases, exceptions allowed in Practice E380
Carbon, Total, by the Combustion Gravimetric Method (0.05 to
are also used.
1.10 %)
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 165
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 appro-
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
priate safety and health practices and determine the applica-
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
bility of regulatory limitations prior to use. Specific hazards
Current edition approved June 1, 2006. Published June 2006. Originally
ε1 statements are given in Section 5 and in special “Warning”
approved in 1968. Last previous edition approved in 2000 as E354 – 93 (2000) .
paragraphs throughout these test methods.
DOI: 10.1520/E0354-93R06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E354 − 93 (2006)
2. Referenced Documents 4. Apparatus, Reagents, and Instrumental Practice
2.1 ASTM Standards: 4.1 Apparatus—Specialized apparatus requirements are
D1193 Specification for Reagent Water listed in the “Apparatus” Section in each method. In some
E29 Practice for Using Significant Digits in Test Data to cases reference may be made to Practices E50.
Determine Conformance with Specifications
4.2 Reagents:
E30 Test Methods for ChemicalAnalysis of Steel, Cast Iron,
4.2.1 Purity of Reagents—Unless otherwise indicated, all
Open-Hearth Iron, and Wrought Iron (Withdrawn 1995)
reagents used in these test methods shall conform to the
E50 Practices for Apparatus, Reagents, and Safety Consid-
“Reagent Grade” Specifications of the American Chemical
erations for Chemical Analysis of Metals, Ores, and 5
Society. Other chemicals may be used, provided it is first
Related Materials
ascertained that they are of sufficiently high purity to permit
E60 Practice for Analysis of Metals, Ores, and Related
their use without adversely affecting the expected performance
Materials by Spectrophotometry
of the determination, as indicated in the section on “Precision
E173 Practice for Conducting Interlaboratory Studies of
and Bias.”
Methods for Chemical Analysis of Metals (Withdrawn
4.2.2 Purity of Water—Unless otherwise indicated, refer-
1998)
ences to water shall be understood to mean reagent water as
E350 Test Methods for Chemical Analysis of Carbon Steel,
defined by Type II of Specification D1193.
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
4.3 Photometric Practice—Photometric practice prescribed
Wrought Iron
in these test methods shall conform to Practice E60.
E351 Test Methods for ChemicalAnalysis of Cast Iron—All
Types
5. Hazards
E352 TestMethodsforChemicalAnalysisofToolSteelsand
Other Similar Medium- and High-Alloy Steels 5.1 For precautions to be observed in the use of certain
E353 Test Methods for Chemical Analysis of Stainless, reagents and equipment in these methods, refer to Practices
Heat-Resisting, Maraging, and Other Similar Chromium- E50.
Nickel-Iron Alloys
6. Sampling
E380 Practice for Use of the International System of Units
(SI) (the Modernized Metric System) (Withdrawn 1997)
6.1 For procedures for sampling the material, reference
E882 Guide for Accountability and Quality Control in the
shall be made to Practice E1806.
Chemical Analysis Laboratory
E1019 Test Methods for Determination of Carbon, Sulfur,
7. Interlaboratory Studies and Rounding Calculated
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
Values
Alloys by Various Combustion and Fusion Techniques
7.1 These test methods have been evaluated using Practice
E1806 Practice for Sampling Steel and Iron for Determina-
E173 or ISO 5725.
tion of Chemical Composition
2.2 Other Document: 7.2 Calculated values shall be rounded to the desired num-
ber of places as directed in 3.4 to 3.6 of Practice E29.
ISO 5725 Precision of Test Methods—Determination of
Repeatability and Reproducibility for Inter-Laboratory
4 MANGANESE BY THE METAPERIODATE
Tests
PHOTOMETRIC METHOD
3. Significance and Use
8. Scope
3.1 These test methods for the chemical analysis of metals
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 0.05 to 2.00 percent.
specifications, particularly those under the jurisdiction of
ASTM Committee D1193 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-
proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
tions greater than 0.5 % is kept in solution with phosphoric
performed in a properly equipped laboratory under appropriate
acid. Solutions of the samples are fumed with perchloric acid
quality control practices such as those described in Guide
so that the effect of periodate is limited to the oxidation of
E882.
manganese. Photometric measurements are made at approxi-
mately 545 nm.
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, American
The last approved version of this historical standard is referenced on Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
www.astm.org. testing of reagents not listed by the American Chemical Society, see the United
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
4th Floor, New York, NY 10036, http://www.ansi.org. Inc. (USPC), Rockville, MD, http://www.usp.org.
E354 − 93 (2006)
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
in 14.3.
adjustments can be made in the amounts of sample and reagents used.
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—Add10mLofKIO solution,and
12. Interferences
heat the solutions at not less than 90°C for 20 to 30 min (Note
12.1 Perchloric acid treatment, which is used in the 2). Cool, dilute to volume with pretreated water, and mix.
procedure, yields solutions which can be highly colored due to
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
the presence of Cr (VI) ions. Although these ions and other
means of heating them for the specified period to ensure complete color
colored ions in the sample solution undergo no further change
development.
in color quality upon treatment with metaperiodate ion, the
14.4 Photometry:
following precautions must be observed when filter photom-
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
eters are used: Select a filter with maximum transmittance
tion using the Reference Solution (14.2) in absorption cells
between 545 and 565 nm. The filter must transmit not more
with a 1-cm light path and using a light band centered at
than 5 % of its maximum at a wavelength shorter than 530 nm.
approximately545nm.Usingthetestcell,takethephotometric
The band width of the filter should be less than 30 nm when
readings of the calibration solutions versus the Reference
measured at 50 % of its maximum transmittance. Similar
Solution (14.2)
restrictions apply with respect to the wavelength region em-
14.4.2 Single-Cell Photometer—Transfer a suitable portion
ployed when other“ wide-band” instruments are used.
of the Reference Solution (14.2) to an absorption cell with a
12.2 The spectral transmittance curve of permanganate ions 1-cm light path and adjust the photometer to the initial setting,
exhibits two useful minima, one at approximately 526 nm, and using a light band centered at approximately 545 nm. While
the other at 545 nm. The latter is recommended when a 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
15. Procedure
preventing the precipitation of the tungsten.
15.1 Test Solutions—Select and weigh a sample in accor-
13. Reagents dance with the following:
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
purity manganese (purity: 99.99 % minimum), to a 500-mL
volumetric flask and dissolve in 20 mL of HNO by heating.
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
to a 500-mL volumetric flask, dilute to volume, and mix.
13.2 Nitric-Phosphoric Acid Mixture— Cautiously, while
stirring,add100mLofHNO and400mLofH PO to400mL
3 3 4
of water. Cool, dilute to 1 L, and mix. Prepare fresh as needed.
13.3 Potassium Metaperiodate Solution(7.5g/L)—Dissolve
7.5 g of potassium metaperiodate (KIO ) in 200 mL of hot
HNO (1 + 1), add 400 mL of H PO , cool, dilute to 1 L, and
3 4
mix.
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
KIO solution to 1 L of water, mix, heat at not less than 90°C
for 20 to 30 min, and cool. Use this water to dilute solutions to
volume that have been treated with KIO solution to oxidize
E354 − 93 (2006)
15.4.1 Background Color Solution—To one of the sample
Tolerance in
Manganese, Sample Sample Dilution,
aliquots in a 50-mL volumetric flask, add 10 mL of nitric-
% Weight, g Weight, mg mL
phosphoric acid mixture, and heat the solution at not less than
0.01 to 0.5 0.80 0.5 100 90°C for 20 to 30 min (Note 2). Cool, dilute to volume (with
0.45 to 1.0 0.35 0.3 100
untreated water), and mix.
0.85 to 2.0 0.80 0.5 500
15.4.2 Reagent Blank Reference Solution— Transfer the
15.1.1 For Samples Containing Not More Th
...
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