ASTM E1473-94a(1998)
(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: Element Concentration Range, % Aluminum 0.005 to 7.00 Beryllium 0.001 to 0.05 Boron 0.001 to 1.00 Calcium 0.002 to 0.05 Carbon 0.001 to 1.10 Chromium 0.10 to 33.00 Cobalt 0.10 to 75.00 Copper 0.01 to 35.00 Iron 0.01 to 50.00 Lead 0.001 to 0.01 Magnesium 0.001 to 0.05 Manganese 0.01 to 3.0 Molybdenum 0.01 to 30.0 Niobium (Columbium) 0.01 to 6.0 Nickel 0.10 to 98.0 Nitrogen 0.001 to 0.20 Phosphorus 0.002 to 0.08 Sulfur 0.002 to 0.10 Silicon 0.01 to 5.00 Tantalum 0.005 to 1.00 Tin 0.002 to 0.10 Titanium 0.01 to 5.00 Tungsten 0.01 to 18.00 Vanadium 0.01 to 3.25 Zinc 0.001 to 0.01 Zirconium 0.01 to 2.50
1.2 The test methods in this standard are contained in the sections indicated as follows: Sections Aluminum, Total by the 8-Quinolinol Gravimetric Method (0.20 to 7.00%) 2 62 to 69 Chromium by the Atomic Absorption Method (0.018 to 1.00%) 2 100 to 109 Chromium by the Peroxydisulfate Oxidation-Titration Method (0.10 to 33.00%) 2 110 to 118 Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to 75%) 2 34 to 41 Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to 5.0%) 2 42 to 51 Copper by Neocuproine Photometric Method (0.010 to 10.00%) 2 52 to 61 Iron by the Silver Reduction Titrimetric Method (1.0 to 50.0%) 2 127 to 134 Manganese by the Metaperiodate Photometric Method (0.05 to 2.00%) 2 8 to 17 Molybdenum by the Ion Exchange-8-Hydroxyquinoline Gravi- metric Method (1.5 to 30%) 2 119 to 126 Molybdenum by the Photometric Method (0.01 to 1.50%) 2 88 to 99 Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to 84.0%) 2 70 to 77 Niobium by the Ion Exchange-Cupferron Gravimetric Method (0.5 to 6.0%) 135 to 142 Silicon by the Gravimetric Method (0.05 to 5.00%) 2 27 to 33 Sulfur by the Combustion-Iodate Titration Method (0.006 to 0.1%) 2 18 to 26 Tin by the Solvent Extraction-Atomic Absorption Method (0.002 to 0.10%) 2 78 to 87
1.3 Methods for the determination of several elements not included in these test methods can be found in Test Methods E30, E76, and E1019.
1.4 Some of the concentration ranges given in 1.1 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 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 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 1998)
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
Manganese by the Metaperiodate Photometric Method (0.05 to
2.00 %) 8to17
1.1 These test methods describe the chemical analysis of
Molybdenum by the Ion Exchange—8-Hydroxyquinoline Gravi-
nickel, cobalt, and high-temperature alloys having chemical
metric Method (1.5 to 30 %) 119to126
Molybdenum by the Photometric Method (0.01 to 1.50 %) 88 to 99
compositions within the following limits:
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Element Concentration Range, % 2
84.0 %) 70 to 77
Aluminum 0.005 to 7.00
Niobium by the Ion Exchange—Cupferron Gravimetric Method
Beryllium 0.001 to 0.05
(0.5 to 6.0 %) 135 to 142
Boron 0.001 to 1.00
Silicon by the Gravimetric Method (0.05 to 5.00 %) 27 to 33
Calcium 0.002 to 0.05
Sulfur by the Combustion-Iodate Titration Method (0.006 to
Carbon 0.001 to 1.10
0.1 %) 18 to 26
Chromium 0.10 to 33.00
Tantalum by the Ion Exchange—Pyrogallol Spectrophotometric
Cobalt 0.10 to 75.00
Method (0.03 to 1.0%) 143 to 151
Copper 0.01 to 35.00
Tin by the Solvent Extraction-Atomic Absorption Method (0.002
Iron 0.01 to 50.00
to 0.10 %) 78 to 87
Lead 0.001 to 0.01
Magnesium 0.001 to 0.05
1.3 Methods for the determination of several elements not
Manganese 0.01 to 3.0
included in these test methods can be found in Test Methods
Molybdenum 0.01 to 30.0
E 30, E 76, and E 1019.
Niobium (Columbium) 0.01 to 6.0
Nickel 0.10 to 98.0
1.4 Some of the concentration ranges given in 1.1 are too
Nitrogen 0.001 to 0.20
broad to be covered by a single method, and therefore, these
Phosphorus 0.002 to 0.08
test methods contain multiple methods for some elements. The
Sulfur 0.002 to 0.10
Silicon 0.01 to 5.00
user must select the proper test method by matching the
Tantalum 0.005 to 1.00
information given in the scope and interference sections of
Tin 0.002 to 0.10
each test method with the composition of the alloy to be
Titanium 0.01 to 5.00
Tungsten 0.01 to 18.00
analyzed.
Vanadium 0.01 to 3.25
1.5 The values stated in SI units are to be regarded as
Zinc 0.001 to 0.01
standard. In some cases, exceptions allowed in Practice E 380
Zirconium 0.01 to 2.50
are also used.
1.2 The test methods in this standard are contained in the
1.6 This standard does not purport to address all of the
sections indicated as follows:
safety concerns, if any, associated with its use. It is the
Sections
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
Aluminum, Total by the 8-Quinolinol Gravimetric Method (0.20 to
7.00 %) 62 to 69
bility of regulatory limitations prior to use. Specific hazard
Chromium by the Atomic Absorption Method (0.018 to 1.00 %) 100 to 109
statements are given in Section 7 and in special caution and
Chromium by the Peroxydisulfate Oxidation—Titration Method
warning paragraphs throughout these test methods.
(0.10 to 33.00 %) 110to118
Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to
75 %) 34 to 41
2. Referenced Documents
Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to
2.1 ASTM Standards:
5.0 %) 42 to 51
Copper by Neocuproine Photometric Method (0.010 to 10.00 %) 52 to 61
D 1193 Specification for Reagent Water
Iron by the Silver Reduction Titrimetric Method (1.0 to 50.0 %) 127 to 134
E 29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
E 30 Test Methods for Chemical Analysis of Steel, Cast
These test methods are under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Material and are the direct 2
These test methods were extracted from Test Methods E 354 and the references
responsibility of Subcommittee E01.08 on Ni and Co and High-Temperature Alloys.
to Test Methods E 350, E 351, E 352, and E 353 contained therein.
Current edition approved July 15, 1994. Published September 1994. Originally 3
Annual Book of ASTM Standards, Vol 11.01.
published as E 1473 – 92. Last previous edition E 1473 – 94.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, 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
Iron, Open-Hearth Iron, and Wrought Iron listed in the Apparatus section in each test 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 59 Practice for Sampling Steel and Iron for Determination 4.2.1 Purity of Reagents—Unless otherwise indicated, all
of Chemical Composition reagents used in these test methods shall conform to the
E 60 Practice for Photometric and Spectrophotometric specifications of the Committee on Analytical Reagents of the
Methods for Chemical Analysis of Metals American Chemical Society where such specifications areav-
E 76 Test Methods for Chemical Analysis of Nickel-Copper ailable. Other chemicals may be used, provided it is first
Alloys ascertained that they are of sufficiently high purity to permit
E 173 Practice for Conducting Interlaboratory Studies of their use without adversely affecting the expected performance
Methods for Chemical Analysis of Metals of the determination, as indicated in the Precision and Bias
E 350 Test Methods for Chemical Analysis of Carbon Steel, section.
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
E 351 Test Methods for Chemical Analysis of Cast Iron— defined by Type II of Specification D 1193.
All Types 4.3 Photometric Practice—Photometric practice prescribed
E 352 Test Methods for Chemical Analysis of Tool Steels in these test methods shall conform to Practice E 60.
and Other Similar Medium- and High-Alloy Steels
5. Sampling
E 353 Test Methods for Chemical Analysis of Stainless,
5.1 For procedures for sampling the material, reference
Heat-Resisting, Maraging, and Other Similar Chromium-
shall be made to Method E 59.
Nickel-Iron Alloys
E 354 Test Methods for Chemical Analysis of High-
6. Interlaboratory Studies and Rounding Calculated
Temperature, Electrical, Magnetic, and Other Similar Iron,
Values
Nickel, and Cobalt Alloys
6.1 These test methods have been evaluated using Practice
E 380 Practice for Use of the International System of Units
E 173 or ISO 5725.
(SI) (the Modernized Metric System)
6.2 Round calculated values to the desired number of places
E 882 Guide for Accountability and Quality Control in the
as directed in 3.4 to 3.6 of Practice E 29.
Chemical Analysis Laboratory
E 1019 Test Methods for Determination of Carbon, Sulfur,
7. Hazards
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
7.1 For precautions to be observed in the use of certain
Cobalt Alloys
reagents and equipment in these test methods, refer to Practices
E 1024 Guide for Chemical Analysis of Metals and Metal
E 50.
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry
MANGANESE BY THE METAPERIODATE
E 1097 Guide for Direct Current Plasma Emission Spec- PHOTOMETRIC METHOD
trometry Analysis
8. Scope
2.2 Other Document:
8.1 This test method covers the determination of manganese
ISO 5725 Precision of Test Methods—Determination of
in concentrations from 0.05 to 2.00 %.
Repeatability and Reproducibility for Inter-Laboratory
Tests
9. Summary of Test Method
3. Significance and Use
9.1 Manganous ions are oxidized to permanganate ions by
3.1 These test methods for the chemical analysis of metals treatment with periodate. Tungsten when present at concentra-
and alloys are primarily intended as referee methods to test tions greater than 0.5 % is kept in solution with phosphoric
such materials for compliance with compositional specifica- acid. Solutions of the samples are fumed with perchloric acid
tions, particularly those under the jurisdiction of ASTM Com- so that the effect of periodate is limited to the oxidation of
mittee B-2 on Nonferrous Metals and Alloys. It is assumed that manganese. Photometric measurements are made at 545 nm.
all who use these test methods will be trained analysts capable
10. Concentration Range
of performing common laboratory procedures skillfully and
10.1 The recommended concentration range is from 0.15 to
safely. It is expected that work will be performed in a properly
0.8 mg of manganese per 50 mL of solution, using a 1-cm cell
equipped laboratory under appropriate quality control practices
(Note 1) and a spectrophotometer with a band width of 10 nm
such as those described in Guide E 882.
or less.
4. Apparatus, Reagents, and Instrumental Practice
4.1 Apparatus—Specialized apparatus requirements are
Reagent Chemicals, American Chemical Society Specifications, American
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
NOTE 1—This test method has been written for cells having a 1-cm
Proceed as directed in 14.3.
light path and a “narrow-band” instrument. The concentration range
14.2 Reference Solution—Transfer approximately 25 mL of
depends upon band width and spectral region used as well as cell optical
water to a 50-mL borosilicate glass volumetric flask. Proceed
path length. Cells having other dimensions may be used, provided suitable
as directed in 14.3
adjustments can be made in the amounts of sample and reagents used.
14.3 Color Development—Add 10 mL of KIO solution,
11. Stability of Color 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
11.1 The color is stable for at least 24 h.
mix.
12. Interferences
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
12.1 Perchloric acid treatment, which is used in the proce-
means of heating them for the specified period to ensure complete color
dure, yields solutions which can be highly colored due to the development.
presence of Cr (VI) ions. Although these ions and other colored
14.4 Photometry:
ions in the sample solution undergo no further change in color
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
quality upon treatment with metaperiodate ion, the following
tion using the Reference Solution (14.2) in absorption cells
precautions must be observed when filter photometers are used:
with a 1-cm light path and using a light band centered at
Select a filter with maximum transmittance between 545 and
approximately 545 nm. Using the test cell, take the photometric
565 nm. The filter must transmit not more than 5 % of its
readings of the calibration solutions versus the reference
maximum at a wavelength shorter than 530 nm. The band
solution (14.2)
width of the filter should be less than 30 nm when measured at
14.4.2 Single-Cell Photometer—Transfer a suitable portion
50 % of its maximum transmittance. Similar restrictions apply
of the reference solution (14.2) to an absorption cell with a
with respect to the wavelength region employed when other“
1-cm light path and adjust the photometer to the initial setting,
wide-band” instruments are used.
using a light band centered at approximately 545 nm. While
12.2 The spectral transmittance curve of permanganate ions
maintaining this adjustment, take the photometric readings of
exhibits two useful minima, one at approximately 526 nm, and
the calibration solutions.
the other at 545 nm. The latter is recommended when a
14.5 Calibration Curve—Plot the net photometric readings
“narrow-band” spectrophotometer is used.
of the calibration solutions against milligrams of manganese
12.3 Tungsten, when present in amounts of more than 0.5 %
per 50 mL of solution.
interferes by producing a turbidity in the final solution. A
special procedure is provided for use with samples containing
15. Procedure
more than 0.5 % tungsten which eliminates the problem by
15.1 Test Solutions—Select and weigh a sample in accor-
preventing the precipitation of the tungsten.
dance with the following:
13. Reagents Tolerance in
Manganese, Sample Sample Dilution,
13.1 Manganese, Standard Solution (1 mL 5 0.032 mg
% Weight, g Weight, mg mL
0.01 to 0.5 0.80 0.5 100
Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
0.45 to 1.0 0.35 0.3 100
purity manganese (purity: 99.99 % minimum), to a 500-mL
0.85 to 2.0 0.80 0.5 500
volumetric flask and dissolve in 20 mL of HNO by heating.
15.1.1 For Samples Containing Not More Than 0.5 %
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
Tungsten:
to a 500-mL volumetric flask, dilute to volume, and mix.
15.1.1.1 To dissolve samples that do not require HF, add 8
13.2 Nitric-Phosphoric Acid Mixture—Cautiously, while
to 10 mL of HCl (1 + 1), and heat. Add HNO as needed to
stirring, add 100 mL of HNO and 400 mL of H PO to 400 mL 3
3 3 4
hasten dissolution, and then add 3 to 4 mL in excess. When
of water. Cool, dilute to 1 L, and mix. Prepare fresh as needed.
dissolution is complete, cool, then add 10 mL of HClO ;
13.3 Potassium Metaperiodate Solution (7.5 g/L)— 4
evaporate to fumes to oxidize chromium, if present, and to
Dissolve 7.5 g of potassium metaperiodate (KIO ) in 200 mL
expel HCl. Continue fuming until salts begin to separate. Cool,
of hot HNO (1 + 1), add 400 mL of H PO , cool, dilute to 1 L,
3 3 4
add 50 mL of water, and digest if necessary to dissolve the
and mix.
salts. Cool and transfer the solution to a 100-mL volumetric
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
flask. Proceed to 15.1.3.
KIO solution to 1 L of water, mix, heat at not
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