ASTM E1473-94a(2003)
(Test Method)Standard Test Methods for Chemical Analysis of Nickel, Cobalt, and High-Temperature Alloys
Standard Test Methods for Chemical Analysis of Nickel, Cobalt, and High-Temperature Alloys
SCOPE
1.1 These test methods describe the chemical analysis of nickel, cobalt, and high-temperature alloys having chemical compositions within the following limits:ElementConcentration Range, %Aluminum0.005 to 7.00Beryllium0.001 to 0.05Boron0.001 to 1.00Calcium0.002 to 0.05Carbon0.001 to 1.10Chromium0.10 to 33.00Cobalt0.10 to 75.00Copper0.01 to 35.00Iron0.01 to 50.00Lead0.001 to 0.01Magnesium0.001 to 0.05Manganese0.01 to 3.0 Molybdenum0.01 to 30.0 Niobium (Columbium)0.01 to 6.0 Nickel0.10 to 98.0 Nitrogen0.001 to 0.20Phosphorus0.002 to 0.08Sulfur0.002 to 0.10Silicon0.01 to 5.00Tantalum0.005 to 1.00Tin0.002 to 0.10Titanium0.01 to 5.00Tungsten0.01 to 18.00Vanadium0.01 to 3.25Zinc0.001 to 0.01Zirconium0.01 to 2.50
1.2 The test methods in this standard are contained in the sections indicated as follows:SectionsAluminum, Total by the 8-Quinolinol Gravimetric Method (0.20 to7.00 %)62 to 69Chromium by the Atomic Absorption Method (0.018 to 1.00 %)100 to 109Chromium by the Peroxydisulfate Oxidation-Titration Method(0.10 to 33.00 %)110 to 118Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to75 %)34 to 41Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to5.0 %)42 to 51Copper by Neocuproine Photometric Method (0.010 to 10.00 %)52 to 61Iron by the Silver Reduction Titrimetric Method (1.0 to 50.0 %)127 to 134Manganese by the Metaperiodate Photometric Method (0.05 to2.00 %)8 to 17Molybdenum by the Ion Exchange-8-Hydroxyquinoline Gravi-metric Method (1.5 to 30 %)119 to 126Molybdenum by the Photometric Method (0.01 to 1.50 %)88 to 99Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to84.0 %)70 to 77Niobium by the Ion Exchange-Cupferron Gravimetric Method(0.5 to 6.0 %)135 to 142Silicon by the Gravimetric Method (0.05 to 5.00 %)27 to 33Sulfur by the Combustion-Iodate Titration Method (0.006 to0.1 %)18 to 26Tantalum by the Ion Exchange-Pyrogallol SpectrophotometricMethod (0.03 to 1.0%)143 to 151Tin by the Solvent Extraction-Atomic Absorption Method (0.002to 0.10 %)78 to 87
1.3 Methods for the determination of several elements not included in these test methods can be found in Test Methods E 30, E 76, and E 1019.
1.4 Some of the concentration ranges given in are too broad to be covered by a single method, and therefore, these test methods contain multiple 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.
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 hazard statements are given in Section 7 and in special caution and warning paragraphs throughout these test methods.
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Standards Content (Sample)
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Designation: E 1473 – 94a (Reapproved 2003)
Standard Test Methods for
Chemical Analysis of Nickel, Cobalt, and High-Temperature
Alloys
This standard is issued under the fixed designation E 1473; 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.
1. Scope
Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to
5.0 %) 42 to 51
1.1 These test methods describe the chemical analysis of
Copper by Neocuproine Photometric Method (0.010 to 10.00 %) 52 to 61
nickel, cobalt, and high-temperature alloys having chemical
Iron by the Silver Reduction Titrimetric Method (1.0 to 50.0 %) 127 to 134
Manganese by the Metaperiodate Photometric Method (0.05 to
compositions within the following limits:
2.00 %) 8to17
Element Concentration Range, %
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravi-
Aluminum 0.005 to 7.00 2
metric Method (1.5 to 30 %) 119to126
Beryllium 0.001 to 0.05
Molybdenum by the Photometric Method (0.01 to 1.50 %) 88 to 99
Boron 0.001 to 1.00
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Calcium 0.002 to 0.05 2
84.0 %) 70 to 77
Carbon 0.001 to 1.10
Niobium by the Ion Exchange—Cupferron Gravimetric Method
Chromium 0.10 to 33.00
(0.5 to 6.0 %) 135 to 142
Cobalt 0.10 to 75.00
Silicon by the Gravimetric Method (0.05 to 5.00 %) 27 to 33
Copper 0.01 to 35.00
Sulfur by the Combustion-Iodate Titration Method (0.006 to
Iron 0.01 to 50.00
0.1 %) 18 to 26
Lead 0.001 to 0.01
Tantalum by the Ion Exchange—Pyrogallol Spectrophotometric
Magnesium 0.001 to 0.05
Method (0.03 to 1.0%) 143 to 151
Manganese 0.01 to 3.0
Tin by the Solvent Extraction-Atomic Absorption Method (0.002
Molybdenum 0.01 to 30.0
to 0.10 %) 78 to 87
Niobium (Columbium) 0.01 to 6.0
Nickel 0.10 to 98.0
1.3 Methods for the determination of several elements not
Nitrogen 0.001 to 0.20
included in these test methods can be found in Test Methods
Phosphorus 0.002 to 0.08
E 30, E 76, and E 1019.
Sulfur 0.002 to 0.10
Silicon 0.01 to 5.00 1.4 Some of the concentration ranges given in 1.1 are too
Tantalum 0.005 to 1.00
broad to be covered by a single method, and therefore, these
Tin 0.002 to 0.10
test methods contain multiple methods for some elements. The
Titanium 0.01 to 5.00
Tungsten 0.01 to 18.00
user must select the proper test method by matching the
Vanadium 0.01 to 3.25
information given in the scope and interference sections of
Zinc 0.001 to 0.01
each test method with the composition of the alloy to be
Zirconium 0.01 to 2.50
analyzed.
1.2 The test methods in this standard are contained in the
1.5 The values stated in SI units are to be regarded as
sections indicated as follows:
standard. In some cases, exceptions allowed in Practice E 380
Sections
are also used.
1.6 This standard does not purport to address all of the
Aluminum, Total by the 8-Quinolinol Gravimetric Method (0.20 to
7.00 %) 62 to 69
safety concerns, if any, associated with its use. It is the
Chromium by the Atomic Absorption Method (0.018 to 1.00 %) 100 to 109
responsibility of the user of this standard to establish appro-
Chromium by the Peroxydisulfate Oxidation—Titration Method
priate safety and health practices and determine the applica-
(0.10 to 33.00 %) 110to118
Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to
bility of regulatory limitations prior to use. Specific hazard
75 %) 34 to 41
statements are given in Section 7 and in special caution and
warning paragraphs throughout these test methods.
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Material and are the direct
responsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys
.
Current edition approved October 1, 2003. Published October 2003. Originally These test methods were extracted from Test Methods E 354 and the references
approved in 1992. Last previous edition approved in 1998 as E 1473 – 94 (1998). to Test Methods E 350, E 351, E 352, and E 353 contained therein.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1473 – 94a (2003)
2. Referenced Documents mittee B-2 on Nonferrous Metals and Alloys. It is assumed that
all who use these test methods will be trained analysts capable
2.1 ASTM Standards:
3 of performing common laboratory procedures skillfully and
D 1193 Specification for Reagent Water
safely. It is expected that work will be performed in a properly
E 29 Practice for Using Significant Digits in Test Data to
4 equipped laboratory under appropriate quality control practices
Determine Conformance with Specifications
such as those described in Guide E 882.
E 30 Test Methods for Chemical Analysis of Steel, Cast
Iron, Open-Hearth Iron, and Wrought Iron
4. Apparatus, Reagents, and Instrumental Practice
E 50 Practices for Apparatus, Reagents, and Safety Precau-
4.1 Apparatus—Specialized apparatus requirements are
tions for Chemical Analysis of Metals
listed in the Apparatus section in each test method. In some
E 59 Practice for Sampling Steel and Iron for Determination
cases, reference may be made to Practices E 50.
of Chemical Composition
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 76 Test Methods for Chemical Analysis of Nickel-Copper
specifications of the Committee on Analytical Reagents of the
Alloys
American Chemical Society where such specifications areav-
E 173 Practice for Conducting Interlaboratory Studies of
ailable. Other chemicals may be used, provided it is first
Methods for Chemical Analysis of Metals
ascertained that they are of sufficiently high purity to permit
E 350 Test Methods for Chemical Analysis of Carbon Steel,
their use without adversely affecting the expected performance
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
of the determination, as indicated in the Precision and Bias
Wrought Iron
section.
E 351 Test Methods for Chemical Analysis of Cast Iron—
4.2.2 Purity of Water—Unless otherwise indicated, refer-
All Types
ences to water shall be understood to mean reagent water as
E 352 Test Methods for Chemical Analysis of Tool Steels
defined by Type II of Specification D 1193.
and Other Similar Medium- and High-Alloy Steels
4.3 Photometric Practice—Photometric practice prescribed
E 353 Test Methods for Chemical Analysis of Stainless,
in these test methods shall conform to Practice E 60.
Heat-Resisting, Maraging, and Other Similar Chromium-
Nickel-Iron Alloys
5. Sampling
E 354 Test Methods for Chemical Analysis of High-
5.1 For procedures for sampling the material, reference
Temperature, Electrical, Magnetic, and Other Similar Iron,
shall be made to Method E 59.
Nickel, and Cobalt Alloys
6. Interlaboratory Studies and Rounding Calculated
E 380 Practice for Use of the International System of Units
(SI) (the Modernized Metric System) Values
E 882 Guide for Accountability and Quality Control in the
6.1 These test methods have been evaluated using Practice
Chemical Analysis Laboratory
E 173 or ISO 5725.
E 1019 Test Methods for Determination of Carbon, Sulfur,
6.2 Round calculated values to the desired number of places
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
as directed in 3.4 to 3.6 of Practice E 29.
Cobalt Alloys
7. Hazards
E 1024 Guide for Chemical Analysis of Metals and Metal
Bearing Ores by Flame Atomic Absorption Spectropho-
7.1 For precautions to be observed in the use of certain
tometry reagents and equipment in these test methods, refer to Practices
E 1097 Guide for Direct Current Plasma Emission Spec-
E 50.
trometry Analysis
MANGANESE BY THE METAPERIODATE
2.2 Other Document:
PHOTOMETRIC METHOD
ISO 5725 Precision of Test Methods—Determination of
Repeatability and Reproducibility for Inter-Laboratory
8. Scope
Tests
8.1 This test method covers the determination of manganese
in concentrations from 0.05 to 2.00 %.
3. Significance and Use
3.1 These test methods for the chemical analysis of metals 9. Summary of Test Method
and alloys are primarily intended as referee methods to test
9.1 Manganous ions are oxidized to permanganate ions by
such materials for compliance with compositional specifica-
treatment with periodate. Tungsten when present at concentra-
tions, particularly those under the jurisdiction of ASTM Com-
tions greater than 0.5 % is kept in solution with phosphoric
3 8
Annual Book of ASTM Standards, Vol 11.01. Reagent Chemicals, American Chemical Society Specifications, American
Annual Book of ASTM Standards, Vol 14.02. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 03.05. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 03.06. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Available from American National Standards Institute, 11 West 42nd St., 13th and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Floor, New York, NY 10036. MD.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1473 – 94a (2003)
acid. Solutions of the samples are fumed with perchloric acid for 20 to 30 min, and cool. Use this water to dilute solutions to
so that the effect of periodate is limited to the oxidation of volume that have been treated with KIO solution to oxidize
manganese. Photometric measurements are made at 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 from 0.15 to
14. Preparation of Calibration Curve
0.8 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
14.1 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 test method has been written for cells having a 1-cm
flasks, and, if necessary, dilute to approximately 25 mL.
light path and a “narrow-band” instrument. The concentration range
Proceed as directed in 14.3.
depends 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
presence of Cr (VI) ions. Although these ions and other colored
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-
precautions must be observed when filter photometers are used:
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
approximately 545 nm. Using the test cell, take the photometric
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 Solutions—Select and weigh a sample in accor-
13. Reagents
dance with the following:
Tolerance in
13.1 Manganese, Standard Solution (1 mL = 0.032 mg
Manganese, Sample Sample Dilution,
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
% Weight, g Weight, mg mL
purity manganese (purity: 99.99 % minimum), to a 500-mL
0.01 to 0.5 0.80 0.5 100
0.45 to 1.0 0.35 0.3 100
volumetric flask and dissolve in 20 mL of HNO by heating.
0.85 to 2.0 0.80 0.5 500
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
to a 500-mL volumetric flask, dilute to volume, and mix. 15.1.1 For Samples Containing Not More Than 0.5 %
13.2 Nitric-Phosphoric Acid Mixture—Cautiously, while Tungsten:
stirring, add 100 mL of HNO and 400 mL of H PO to 400 15.1.1.1 To dissolve samples that do not require HF, add 8
3 3 4
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as to 10 mL of HCl (1 + 1), and heat. Add HNO as needed to
needed. hasten dissolution, and then add 3 to 4 mL in excess. W
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