ASTM E350-95(2005)
(Test Method)Standard Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and Wrought Iron
Standard Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and Wrought Iron
SCOPE
1.1 These test methods cover the chemical analysis of carbon steels, low-alloy steels, silicon electrical steels, ingot iron, and wrought iron having chemical compositions within the following limits:
1.3 Test 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 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 IEEE/ASTM SI 10 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.
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Designation:E350–95(Reapproved2005)
Standard Test Methods for
Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon
Electrical Steel, Ingot Iron, and Wrought Iron
This standard is issued under the fixed designation E 350; 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.
1. Scope
Aluminum, Total or Acid-Soluble, by the Atomic Absorption
Method (0.005 to 0.20 %) 308–317
1.1 These test methods cover the chemical analysis of
Antimony by the Brilliant Green Photometric Method (0.0002 to
carbon steels, low-alloy steels, silicon electrical steels, ingot 0.030 %) 142–151
Bismuth by the Atomic Absorption Method (0.02 to 0.25 %) 298–307
iron, and wrought iron having chemical compositions within
Boron by the Distillation-Curcumin Photometric Method (0.0003
the following limits:
to 0.006 %) 208–219
Element Concentration Range, % Calcium by the Direct-Current Argon Plasma Optical Emission
Spectroscopy Method (0.0005 to 0.010 %) 289–297
Aluminum 0.001 to 1.50
Antimony 0.002 to 0.03 Carbon, Total, by the Combustion Gravimetric Method (0.05 to
1.80 %)—Discontinued 1995
Arsenic 0.0005 to 0.10
Cerium and Lanthanum by the D-C Plasma Optical Emission
Bismuth 0.005 to 0.50
Method (0.003 to 0.50 % Cerium, 0.001 to 0.30 % Lanthanum) 249–257
Boron 0.0005 to 0.02
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 220–229
Calcium 0.0005 to 0.01
Chromium by the Peroxydisulfate Oxidation-Titration Method
Cerium 0.005 to 0.50
(0.05 to 3.99 %) 230–238
Chromium 0.005 to 3.99
Cobalt by the Nitroso-R Salt Photometric Method (0.01 to
Cobalt 0.01 to 0.30
0.30 %) 53–62
Columbium (Niobium) 0.002 to 0.20
Copper by the Atomic Absorption Method (0.004 to 0.5 %) 279–288
Copper 0.005 to 1.50
Copper by the Neocuproine Photometric Method (0.005 to
Lanthanum 0.001 to 0.30
1.50 %) 114–123
Lead 0.001 to 0.50
Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to
Manganese 0.01 to 2.50
0.50 %) 132–141
Molybdenum 0.002 to 1.50
Manganese by the Atomic Absorption Method (0.005 to 2.0 %) 269–278
Nickel 0.005 to 5.00
Manganese by the Metaperiodate Photometric Method (0.01 to
Nitrogen 0.0005 to 0.04
2.5 %) 8-17
Oxygen 0.0001 to 0.03
Manganese by the Peroxydisulfate-Arsenite Titrimetric Method
Phosphorus 0.001 to 0.25
(0.10 to 2.50 %) 164–171
Selenium 0.001 to 0.50
Molybdenum by the Thiocyanate Photometric Method (0.01 to
Silicon 0.001 to 5.00
1.50 %) 152–163
Sulfur 0.001 to 0.60
Nickel by the Atomic Absorption Method (0.003 to 0.5 %) 318–327
Tin 0.002 to 0.10
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Titanium 0.002 to 0.60
5.00 %) 180–187
Tungsten 0.005 to 0.10
Nickel by the Ion-Exchange-Atomic—Absorption Method (0.005
Vanadium 0.005 to 0.50
to 1.00 %) 188–197
Zirconium 0.005 to 0.15
Phosphorus by the Alkalimetric Method (0.02 to 0.25 %) 172–179
1.2 The test methods in this standard are contained in the Phosphorus by the Molybdenum Blue Photometric Method (0.003
to 0.09 %) 18-29
sections indicated as follows:
Silicon by the Molybdenum Blue Photometric Method (0.01 to
Sections
0.06 %) 103–113
Silicon by the Gravimetric Titration Method (0.01 to 3.5 %) 46–52
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20
Sulfur by the Combustion-Iodate Titration Method (0.005 to
to 1.5 %) 124–131
0.3 %) 37–45
Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003
Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.1 %) 95–102
to 0.20 %) 76–86
Tin by the Solvent Extraction-Atomic Absorption Method (0.002
to 0.10 %) 198–207
Titanium, Total, by the Diantipyrylmethane Spectrophotometric
Method (0.025 to 0.30 %) 258–268
1 Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 239–248
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores and Related Materials and are the direct
1.3 Test methods for the determination of several elements
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
notincludedinthisstandardcanbefoundinTestMethodsE 30
Current edition approved May 1, 2005. Published May 2005. Originally
e1
approved in 1968. Last previous edition approved in 2000 as E 350 – 95 (2000) . and Test Methods E 1019.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E350–95 (2005)
1.4 Some of the concentration ranges given in 1.1 are too E 1097 Guide for Direct Current Plasma Emission Spec-
broad to be covered by a single test method and therefore this trometry Analysis
standard contains multiple test methods for some elements. E 1806 Practice for Sampling Steel and Iron for Determi-
The user must select the proper test method by matching the nation of Chemical Composition
information given in the Scope and Interference sections of
IEEE/ASTM SI 10 Standard for Use of the International
each test method with the composition of the alloy to be System of Units (SI): The Modern Metric System
analyzed.
2.2 ISO Standard:
1.5 The values stated in SI units are to be regarded as
ISO 5725 Precision of Test Methods—Determination of
standard. In some cases, exceptions allowed in IEEE/ASTM SI
Repeatability and Reproducibility for Inter-Laboratory
10 are also used.
Tests
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Significance and Use
responsibility of the user of this standard to establish appro-
3.1 These test methods for the chemical analysis of metals
priate safety and health practices and determine the applica-
and alloys are primarily intended as referee methods to test
bility of regulatory limitations prior to use. Specific hazards
such materials for compliance with compositional specifica-
statements are given in Section 5 and in special “Warning”
tions, particularly those under the jurisdiction of ASTM Com-
paragraphs throughout these test methods.
mittees A01 on Steel, Stainless Steel, and Related Alloys and
A04 on Iron Castings. It is assumed that all who use these test
2. Referenced Documents
methods will be trained analysts capable of performing com-
2.1 ASTM Standards:
mon laboratory procedures skillfully and safely. It is expected
D 1193 Specification for Reagent Water
that work will be performed in a properly equipped laboratory
E29 Practice for Using Significant Digits in Test Data to
under appropriate quality control practices such as those
Determine Conformance with Specifications
described in Guide E 882.
E30 Test Methods for Chemical Analysis of Steel, Cast
Iron, Open-Hearth Iron, and Wrought Iron
4. Apparatus, Reagents, and Instrumental Practices
E50 Practices forApparatus, Reagents, and Safety Consid-
4.1 Apparatus—Specialized apparatus requirements are
erationsforChemicalAnalysisofMetals,OresandRelated
listed in the “Apparatus” Section in each test method. In some
Materials
cases reference may be made to Practices E 50.
E 60 Practice for Analysis of Metals, Ores, and Related
4.2 Reagents:
Materials by Molecular Absorption Spectrometry
4.2.1 Purity of Reagents—Unless otherwise indicated, all
E 173 Practice for Conducting Interlaboratory Studies of
3 reagentsusedinthesetestmethodsshallconformtothereagent
Methods for Chemical Analysis of Metals
grade specifications of theAmerican Chemical Society. Other
E 319 Practice for the Evaluation of Single-Pan Mechanical
chemicals may be used, provided it is first ascertained that they
Balances
are of sufficiently high purity to permit their use without
E 351 Test Methods for Chemical Analysis of Cast Iron—
adversely affecting the expected performance of the determi-
All Types
nation, as indicated in the Precision and Bias section.
E 352 Test Methods for Chemical Analysis of Tool Steels
4.2.2 Purity of Water—Unless otherwise indicated, refer-
and Other Similar Medium- and High-Alloy Steels
ences to water shall be understood to mean reagent water as
E 353 Test Methods for Chemical Analysis of Stainless,
defined by Type II of Specification D 1193.
Heat-Resisting, Maraging, and Other Similar Chromium-
Nickel-Iron Alloys
5. Hazards
E 354 Test Methods for Chemical Analysis of High-
Temperature, Electrical, Magnetic, and Other Similar Iron,
5.1 For precautions to be observed in the use of certain
Nickel, and Cobalt Alloys
reagentsandequipmentinthesetestmethods,refertoPractices
E 882 Guide for Accountability and Quality Control in the
E 50.
Chemical Analysis Laboratory
E 1019 Test Methods for Determination of Carbon, Sulfur,
6. Sampling
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
6.1 For procedures for sampling the material, reference
Cobalt Alloys
shall be made to Practice E 1806.
E 1024 Guide for Chemical Analysis of Metals and Metal-
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry
Available from American National Standards Institute, 11 West 42nd St., 13th
Floor, New York, NY 10036.
Reagent Chemicals, American Chemical Society Specifications , American
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by the American Chemical Society, see Analar Standards for Laboratory
Standards volume information, refer to the standard’s Document Summary page on Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
the ASTM website. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Withdrawn. MD.
E350–95 (2005)
7. Interlaboratory Studies and Rounding Calculated purity manganese (purity: 99.99 % minimum), to a 500-mL
Values volumetric flask and dissolve in 20 mL of HNO by heating.
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
7.1 These test methods have been evaluated using Practice
to a 500-mL volumetric flask, dilute to volume, and mix.
E 173 or ISO 5725.
13.2 Nitric-Phosphoric Acid Mixture— Cautiously, while
7.2 Calculated values shall be rounded to the desired num-
stirring, add 100 mL of HNO and 400 mL of H PO to 400
3 3 4
ber of places in accordance with the Rounding Method of
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as
Practice E 29.
needed.
MANGANESE BY THE METAPERIODATE
13.3 Potassium Metaperiodate Solution (7.5 g/L)—
PHOTOMETRIC METHOD
Dissolve 7.5 g of potassium metaperiodate (KIO ) in 200 mL
of hot HNO (1+1), add 400 mLof H PO , cool, dilute to 1 L,
3 3 4
8. Scope
and mix.
8.1 This test method covers the determination of manganese
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
in concentrations from 0.01 to 2.5 %.
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
9. Summary of Test Method
volume that have been treated with KIO solution to oxidize
9.1 Manganous ions are oxidized to permanganate ions by
manganese, and thus avoid reduction of permanganate ions by
reaction with metaperiodate ions. Solutions of the samples are
any reducing agents in the untreated water. Caution—Avoid
fumed with perchloric acid so that the effect of metaperiodate
the use of this water for other purposes.
ion is limited to the oxidation of manganese. Photometric
measurement is made at approximately 545 nm.
14. Preparation of Calibration Curve
14.1 Calibration Solutions—Using pipets, transfer 5, 10,
10. Concentration Range
15, 20, and 25 mL of manganese standard solution (1
10.1 The recommended concentration range is from 0.15 to
mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetric
0.8 mg of manganese per 50 mL of solution, using a 1-cm cell
flasks, and, if necessary, dilute to approximately 25 mL.
(Note 1) and a spectrophotometer with a band width of 10 nm
Proceed as directed in 14.3.
or less.
14.2 Reference Solution—Transfer approximately 25 mL of
NOTE 1—This test method has been written for cells having a 1-cm
water to a 50-mL borosilicate glass volumetric flask. Proceed
light path and a “narrow-band” instrument. The concentration range
as directed in 14.3.
depends upon band width and spectral region used as well as cell optical
14.3 Color Development—Add 10 mL of KIO solution,
pathlength.Cellshavingotherdimensionsmaybeused,providedsuitable
and heat the solutions at not less than 90°C for 20 to 30 min
adjustments can be made in the amounts of sample and reagents used.
(Note 2). Cool, dilute to volume with pretreated water, and
11. Stability of Color mix.
11.1 The color is stable for at least 24 h.
NOTE 2—Immersing the flasks in a boiling water bath is a preferred
means of heating them for the specified period to ensure complete color
12. Interferences
development.
12.1 The elements ordinarily present do not interfere. Per-
14.4 Photometry:
chloric acid treatment, which is used in the procedure, yields
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
solutionswhichcanbehighlycoloredduetothepresenceofCr
tion using the Reference Solution (14.2) in absorption cells
(VI) ions. Although these ions and other colored ions in the
with a 1-cm light path and using a light band centered at
sample solution undergo no further change in color quality
approximately545nm.Usingthetestcell,takethephotometric
upon treatment with metaperiodate ion, the following precau-
readings of the calibration solutions versus the reference
tionsmustbeobservedwhenfilterphotometersareused:Select
solution (14.2).
a filter with maximum transmittance between 545 and 565 nm.
14.4.2 Single-Cell Photometer—Transfer a suitable portion
The filter must transmit not more than5%ofits maximum at
of the reference solution (14.2) to an absorption cell with a
a wavelength shorter than 530 nm. The band width of the filter
1-cm light path and adjust the photometer to the initial setting,
should be less than 30 nm when measured at 50 % of its
using a light band centered at approximately 545 nm. While
maximum transmittance. Similar restrictions apply with re-
maintaining this adjustment, take the photometric readings of
spect to the wavelength region employed when other “wide-
the calibration solutions.
band” instruments are used.
14.5 Calibration Curve—Plot the net photometric readings
12.2 The spectral transmittance curve of permanganate ions
of the calibration solutions against milligrams of manganese
exhibits two useful minima, one at approximately 526 nm, and
per 50 mL of solution.
the other at 545 nm. The latter is recommended when a
“narrow-band” s
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