ASTM E354-93(2000)e1

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e1
Designation:E354–93 (Reapproved 2000)
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 E 354; 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.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—Editorial changes were made in November 2000.
1. Scope
Sections
1.1 These test methods cover the chemical analysis of
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to
high-temperature, electrical, magnetic, and other similar iron, 7.00 %)
1a
Carbon,Total, by the Combustion-Thermal Conductivity Method
nickel, and cobalt alloys having chemical compositions within
Carbon, Total, by the Combustion Gravimetric Method (0.05 to
the following limits:
1.10 %)
Concentration Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 165
Element
Chromium by the Peroxydisulfate Oxidation—Titration Method
Range, %
(0.10 to 33.00 %)
1b
Chromium by the Peroxydisulfate-Oxidation Titrimetric Method
Aluminum 0.005 to 18.00
Beryllium 0.001 to 0.05 Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to
75 %)
Boron 0.001 to 1.00
Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to 5.0 %) 61
Calcium 0.002 to 0.05
Copper by Neocuproine Photometric Method (0.01 to 10.00 %) 90
Carbon 0.001 to 1.10
Copper by the Sulfide Precipitation-Electrodeposition Gravimetric
Chromium 0.10 to 33.00
Method (0.01 to 10.00 %)
Cobalt 0.10 to 75.00
Iron by the Silver ReductionTitrimetric Method (1.0 to 50.0 %) 192
Columbium (Niobium) 0.01 to 6.0
Copper 0.01 to 10.00 Manganese by the Periodate Photometric Method (0.05 to 2.00 %) 8
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravi-
Iron 0.01 to 85.00
Magnesium 0.001 to 0.05 metric Method (1.5 to 30 %)
Molybdenum by the Photometric Method (0.01 to 1.50 %) 153
Manganese 0.01 to 3.0
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Molybdenum 0.01 to 30.0
84.0 %)
Nickel 0.10 to 84.0
Phosphorus by the Molybdenum Blue Photometric Method (0.002
Nitrogen 0.001 to 0.20
to 0.08 %)
Phosphorus 0.002 to 0.08
Silicon by the Gravimetric Method (0.05 to 5.00 %) 46
Silicon 0.01 to 5.00
1 c
Sulfur by the Gravimetric Method
Sulfur 0.002 to 0.10
Tantalum 0.005 to 10.0
Sulfur by the Combustion-Iodate Titration Method (0.005 to
Titanium 0.01 to 5.00
0.1 %)
Tungsten 0.01 to 18.00
1b
Sulfur by the Chromatographic Gravimetric Method
Vanadium 0.01 to 3.25
Tin by the Solvent Extraction–Atomic Absorption Method (0.002
Zirconium 0.01 to 2.50
to 0.10 %)
1.2 The test methods in this standard are contained in the
1.3 Methods for the determination of several elements not
sections indicated below:
included in this standard can be found in Test Methods E 30
and Test Methods E 1019.
These test methods are under the jurisdiction of ASTM Committee E01 on 1.4 Some of the concentration ranges given in 1.1 are too
Analytical Chemistry for Metals, Ores, and Related Material and are the direct
broad to be covered by a single method and therefore this
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
standard contains multiple methods for some elements. The
Current edition approved July 15, 1993. Published September 1993. Originally
e1
user must select the proper method by matching the informa-
published as E 354 – 68 T. Last previous edition E 354 – 89 .
1a
Discontinued April 25, 1986. Its replacement appears as part of ASTM Test
tion given in the Scope and Interference sections of each
Methods E 1019, found in Annual Book of ASTM Standards, Vol 03.06.
method with the composition of the alloy to be analyzed.
1b
Discontinued May 30, 1980.
1c
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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E354–93 (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 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 Practice
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 353 Test Methods for Chemical Analysis of Stainless,
4.3 Photometric Practice—Photometric practice prescribed
Heat-Resisting, Maraging, and Other Similar Chromium-
in these test methods shall conform to Practice E 60.
Nickel-Iron 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 Compostion
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.
2 9
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.
4 10
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., NewYork, 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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E354–93 (2000)
MANGANESE BY THE METAPERIODATE 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 0.05 to 2.00 percent.
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 measurements are made at approxi-
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
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—Using pipets, transfer 5, 10,
NOTE 1—This method has been written for cells having a 1-cm light
15, 20, and 25 mL of manganese standard solution (1
path and a “narrow-band” instrument. The concentration range depends
mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetric
upon band width and spectral region used as well as cell optical path
flasks, and, if necessary, dilute to approximately 25 mL.
length. Cells having other dimensions may be used, provided suitable
Proceed as directed 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—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 proce-
(Note 2). Cool, dilute to volume with pretreated water, and
dure, yields solutions which can be highly colored due to the
mix.
presenceofCr(VI)ions.Althoughtheseionsandothercolored
ions in the sample solution undergo no further change in color
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
quality upon treatment with metaperiodate ion, the following
means of heating them for the specified period to ensure complete color
development.
precautionsmustbeobservedwhenfilterphotometersareused:
Select a filter with maximum transmittance between 545 and
14.4 Photometry:
565 nm. The filter must transmit not more than 5 % of its
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
maximum at a wavelength shorter than 530 nm. The band
tion using the Reference Solution (14.2) in absorption cells
width of the filter should be less than 30 nm when measured at
with a 1-cm light path and using a light band centered at
50 % of its maximum transmittance. Similar restrictions apply
approximately545nm.Usingthetestcell,takethephotometric
with respect to the wavelength region employed when other“
readings of the calibration solutions versus the Reference
wide-band” instruments are used.
Solution (14.2)
12.2 The spectral transmittance curve of permanganate ions
exhibits two useful minima, one at approximately 526 nm, and 14.4.2 Single-Cell Photometer—Transfer a suitable portion
the other at 545 nm. The latter is recommended when a
of the Reference Solution (14.2) to an absorption cell with a
“narrow-band” spectrophotometer is used.
1-cm light path and adjust the photometer to the initial setting,
12.3 Tungsten,whenpresentinamountsofmorethan0.5 %
using a light band centered at approximately 545 nm. While
interferes by producing a turbidity in the final solution. A
maintaining this adjustment, take the photometric readings of
special procedure is provided for use with samples containing
the calibration solutions.
more than 0.5 % tungsten which eliminates the problem by
14.5 Calibration Curve—Plot the net photometric readings
preventing the precipitation of the tungsten.
of the calibration solutions against milligrams of manganese
per 50 mL of solution.
13. Reagents
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
15. Procedure
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
15.1 Test Solutions—Select and weigh a sample in accor-
purity manganese (purity: 99.99 % minimum), to a 500-mL
volumetric flask and dissolve in 20 mL of HNO by heating. dance with the following:
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E354–93 (2000)
15.4.1 Background Color Solution—To one of the sample
Tolerance in
Manganese, Sam
...