ASTM E350-95(2000)e1
(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:ElementConcentration Range, %Aluminum0.001 to 1.50Antimony0.002 to 0.03Arsenic 0.0005 to 0.10Bismuth 0.005 to 0.50Boron 0.0005 to 0.02Calcium 0.0005 to 0.01Cerium 0.005 to 0.50Chromium0.005 to 3.99Cobalt 0.01 to 0.30Columbium (Niobium)0.002 to 0.20Copper 0.005 to 1.50Lanthanum0.001 to 0.30Lead 0.001 to 0.50Manganese0.01 to 2.50Molybdenum0.002 to 1.50Nickel 0.005 to 5.00Nitrogen0.0005 to 0.04Oxygen 0.0001 to 0.03Phosphorus0.001 to 0.25Selenium0.001 to 0.50Silicon 0.001 to 5.00Sulfur 0.001 to 0.60Tin 0.002 to 0.10Titanium0.002 to 0.60Tungsten0.005 to 0.10Vanadium0.005 to 0.50Zirconium0.005 to 0.15
1.2 The test methods in this standard are contained in the sections indicated as follows: SectionsAluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20to 1.5 %)124-131Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003to 0.20 %)76-86Aluminum, Total or Acid-Soluble, by the Atomic AbsorptionMethod (0.005 to 0.20 %)308-317Antimony by the Brilliant Green Photometric Method (0.0002 to0.030 %)142-151Bismuth by the Atomic Absorption Method (0.02 to 0.25 %)298-307Boron by the Distillation-Curcumin Photometric Method (0.0003to 0.006 %)208-219Calcium by the Direct-Current Argon Plasma Optical EmissionSpectroscopy Method (0.0005 to 0.010 %) 289-297Carbon, Total, by the Combustion Gravimetric Method (0.05 to1.80 %)-Discontinued 1995Cerium and Lanthanum by the D-C Plasma Optical EmissionMethod (0.003 to 0.50 % Cerium, 0.001 to 0.30 % Lanthanum)249-257Chromium by the Atomic Absorption Method (0.006 to 1.00 %)220-229Chromium by the Peroxydisulfate Oxidation-Titration Method(0.05 to 3.99 %) 230-238Cobalt by the Nitroso-R Salt Photometric Method (0.01 to0.30 %) 53-62Copper by the Atomic Absorption Method (0.004 to 0.5 %)279-288Copper by the Neocuproine Photometric Method (0.005 to1.50 %) 114-123Lead by the Ion-Exchange-Atomic Absorption Method (0.001 to0.50 %)132-141Manganese by the Atomic Absorption Method (0.005 to 2.0 %)269-278Manganese by the Metaperiodate Photometric Method (0.01 to2.5 %)Manganese by the Peroxydisulfate-Arsenite Titrimetric Method(0.10 to 2.50 %)164-171Molybdenum by the Thiocyanate Photometric Method (0.01 to1.50 %) 152-163Nickel by the Atomic Absorption Method (0.003 to 0.5 %)318-327Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to5.00 %) 180-187Nickel by the Ion-Exchange-Atomic-Absorption Method (0.005to 1.00 %) 188-197Phosphorus by the Alkalimetric Method (0.02 to 0.25 %)172-179Phosphorus by the Molybdenum Blue Photometric Method (0.003to 0.09 %)Silicon by the Molybdenum Blue Photometric Method (0.01 to0.06 %) 103-113Silicon by the Gravimetric Titration Method (0.01 to 3.5 %) 46-52Sulfur by the Combustion-Iodate Titration Method (0.005 to0.03 %) 37-45Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.1 %) 95-102Tin by the Solvent Extraction-Atomic Absorption Method (0.002to 0.10 %)198-207Titanium, Total, by the Diantipyrylmethane SpectrophotometricMethod (0.025 to 0.30 %)258-268Vanadium by the Atomic Absorption Method (0.006 to 0.15 %)239-248
1.3 Test methods for the determination of several elements not included in this standard can be found in Test Methods E30 and Test Methods E1019.
1.4 Some of the concentration ranges given in 1.1 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 Practice E380 are also used.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its ...
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e1
Designation:E350–95 (Reapproved 2000)
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.
e NOTE—Editorial changes were made in November 2000.
1. Scope
Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003
to 0.20 %) 76–86
1.1 These test methods cover the chemical analysis of
Aluminum, Total or Acid-Soluble, by the Atomic Absorption
carbon steels, low-alloy steels, silicon electrical steels, ingot Method (0.005 to 0.20 %) 308–317
Antimony by the Brilliant Green Photometric Method (0.0002 to
iron, and wrought iron having chemical compositions within
0.030 %) 142–151
the following limits:
Bismuth by the Atomic Absorption Method (0.02 to 0.25 %) 298–307
Element Concentration Range, % Boron by the Distillation-Curcumin Photometric Method (0.0003
to 0.006 %) 208–219
Aluminum 0.001 to 1.50
Antimony 0.002 to 0.03 Calcium by the Direct-Current Argon Plasma Optical Emission
Spectroscopy Method (0.0005 to 0.010 %) 289–297
Arsenic 0.0005 to 0.10
Bismuth 0.005 to 0.50 Carbon, Total, by the Combustion Gravimetric Method (0.05 to
1.80 %)—Discontinued 1995
Boron 0.0005 to 0.02
Cerium and Lanthanum by the D-C Plasma Optical Emission
Calcium 0.0005 to 0.01
Method (0.003 to 0.50 % Cerium, 0.001 to 0.30 % Lanthanum) 249–257
Cerium 0.005 to 0.50
Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 220–229
Chromium 0.005 to 3.99
Chromium by the Peroxydisulfate Oxidation-Titration Method
Cobalt 0.01 to 0.30
(0.05 to 3.99 %) 230–238
Columbium (Niobium) 0.002 to 0.20
Cobalt by the Nitroso-R Salt Photometric Method (0.01 to
Copper 0.005 to 1.50
0.30 %) 53–62
Lanthanum 0.001 to 0.30
Copper by the Atomic Absorption Method (0.004 to 0.5 %) 279–288
Lead 0.001 to 0.50
Copper by the Neocuproine Photometric Method (0.005 to
Manganese 0.01 to 2.50
1.50 %) 114–123
Molybdenum 0.002 to 1.50
Lead by the Ion-Exchange—Atomic Absorption Method (0.001 to
Nickel 0.005 to 5.00
0.50 %) 132–141
Nitrogen 0.0005 to 0.04
Manganese by the Atomic Absorption Method (0.005 to 2.0 %) 269–278
Oxygen 0.0001 to 0.03
Manganese by the Metaperiodate Photometric Method (0.01 to
Phosphorus 0.001 to 0.25
2.5 %) 8-17
Selenium 0.001 to 0.50
Manganese by the Peroxydisulfate-Arsenite Titrimetric Method
Silicon 0.001 to 5.00
(0.10 to 2.50 %) 164–171
Sulfur 0.001 to 0.60
Molybdenum by the Thiocyanate Photometric Method (0.01 to
Tin 0.002 to 0.10
1.50 %) 152–163
Titanium 0.002 to 0.60
Nickel by the Atomic Absorption Method (0.003 to 0.5 %) 318–327
Tungsten 0.005 to 0.10
Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to
Vanadium 0.005 to 0.50
5.00 %) 180–187
Zirconium 0.005 to 0.15
Nickel by the Ion-Exchange-Atomic—Absorption Method (0.005
1.2 The test methods in this standard are contained in the to 1.00 %) 188–197
Phosphorus by the Alkalimetric Method (0.02 to 0.25 %) 172–179
sections indicated as follows:
Phosphorus by the Molybdenum Blue Photometric Method (0.003
Sections
to 0.09 %) 18-29
Silicon by the Molybdenum Blue Photometric Method (0.01 to
Aluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20
0.06 %) 103–113
to 1.5 %) 124–131
Silicon by the Gravimetric Titration Method (0.01 to 3.5 %) 46–52
Sulfur by the Combustion-Iodate Titration Method (0.005 to
0.3 %) 37–45
Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.1 %) 95–102
These test methods are under the jurisdiction of ASTM Committee E01 on
Tin by the Solvent Extraction-Atomic Absorption Method (0.002
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
to 0.10 %) 198–207
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. Titanium, Total, by the Diantipyrylmethane Spectrophotometric
Current edition approved Jan. 15, 1995. Published March 1995. Originally Method (0.025 to 0.30 %) 258–268
published as E 350 – 68. Last previous edition E 350 – 94.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E350
E 1019 Test Methods for Determination of Carbon, Sulfur,
Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 239–248
Nitrogen, Oxygen, and Hydrogen in Steel and in Iron,
1.3 Test methods for the determination of several elements
Nickel, and Cobalt Alloys
notincludedinthisstandardcanbefoundinTestMethodsE 30
E 1024 Guide for Chemical Analysis of Metals and Metal-
and Test Methods E 1019.
Bearing Ores by Flame Atomic Absorption Spectropho-
1.4 Some of the concentration ranges given in 1.1 are too
tometry
broad to be covered by a single test method and therefore this
E 1097 Guide for Direct Current Plasma Emission Spec-
standard contains multiple test methods for some elements.
trometry Analysis
The user must select the proper test method by matching the
E 1806 Practice for Sampling Steel and Iron for Determi-
information given in the Scope and Interference sections of
nation of Chemical Composition
each test method with the composition of the alloy to be
2.2 ISO Standard:
analyzed.
ISO 5725 Precision of Test Methods—Determination of
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”
mittees A-1 on Steel, Stainless Steel, and Related Alloys and
paragraphs throughout these test methods.
A-4 on Iron Castings. It is assumed that all who use these test
methods will be trained analysts capable of performing com-
2. Referenced Documents
mon laboratory procedures skillfully and safely. It is expected
2.1 ASTM Standards:
2 that work will be performed in a properly equipped laboratory
D 1193 Specification for Reagent Water
under appropriate quality control practices such as those
E 29 Practice for Using Significant Digits in Test Data to
3 described in Guide E 882.
Determine Conformance with Specifications
E 30 Test Methods for Chemical Analysis of Steel, Cast
4 4. Apparatus, Reagents, and Instrumental Practices
Iron, Open Hearth Iron, and Wrought Iron
E 50 Practices for Apparatus, Reagents, and Safety Precau- 4.1 Apparatus—Specialized apparatus requirements are
listed in the “Apparatus” Section in each test method. In some
tions for Chemical Analysis of Metals
E 60 Practice for Photometric and Spectrophotometric cases reference may be made to Practices E 50.
4.2 Reagents:
Methods for Chemical Analysis of Metals
E 173 Practice for Conducting Interlaboratory Studies of 4.2.1 Purity of Reagents—Unless otherwise indicated, all
Methods for Chemical Analysis of Metals reagentsusedinthesetestmethodsshallconformtothereagent
E 319 Practice for the Evaluation of Single-Pan Mechanical gradespecificationsoftheAmericanChemicalSociety. Other
Balances chemicals may be used, provided it is first ascertained that they
E 351 Test Methods for Chemical Analysis of Cast Iron— are of sufficiently high purity to permit their use without
All Types adversely affecting the expected performance of the determi-
nation, as indicated in the Precision and Bias section.
E 352 Test Methods for Chemical Analysis of Tool Steels
and Other Similiar Medium- and High-Alloy Steels 4.2.2 Purity of Water—Unless otherwise indicated, refer-
ences to water shall be understood to mean reagent water as
E 353 Test Methods for Chemical Analysis of Stainless,
Heat-Resisting, Maraging, and Other Similar Chromium- defined by Type II of Specification D 1193.
Nickel-Iron Alloys
E 354 Test Methods for Chemical Analysis of High- 5. Hazards
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 380 Practice for Use of the International System of Units
E 50.
(SI) (the Modernized Metric System)
E 882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
Annual Book of ASTM Standards, Vol 03.06.
Available from American National Standards Institute, 11 West 42nd St., 13th
Floor, New York, NY 10036.
2 10
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
Discontinued 1995; see 1994 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 03.05. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Discontinued 1998; see 1997 Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Discontinued 1997; see IEEEE/ASTM SI 10–Standard , Vol 14.04. MD.
E350
6. Sampling 13. Reagents
6.1 For procedures for sampling the material, reference 13.1 Manganese, Standard Solution (1 mL = 0.032 mg
shall be made to Practice E 1806. Mn)—Transfer the equivalent of 0.4000 g of assayed, high-
purity manganese (purity: 99.99 % minimum), to a 500-mL
7. Interlaboratory Studies and Rounding Calculated
volumetric flask and dissolve in 20 mL of HNO by heating.
Values
Cool, dilute to volume, and mix. Using a pipet, transfer 20 mL
to a 500-mL volumetric flask, dilute to volume, and mix.
7.1 These test methods have been evaluated using Practice
13.2 Nitric-Phosphoric Acid Mixture— Cautiously, while
E 173 or ISO 5725.
stirring, add 100 mL of HNO and 400 mL of H PO to 400
7.2 Calculated values shall be rounded to the desired num- 3 3 4
mL of water. Cool, dilute to 1 L, and mix. Prepare fresh as
ber of places in accordance with 3.4 to 3.6 of Practice E 29.
needed.
MANGANESE BY THE METAPERIODATE 13.3 Potassium Metaperiodate Solution (7.5 g/L)—
Dissolve 7.5 g of potassium metaperiodate (KIO ) in 200 mL
PHOTOMETRIC METHOD
of hot HNO (1+1), add 400 mL of H PO , cool, dilute to 1 L,
3 3 4
8. Scope and mix.
13.4 Water, Pretreated with Metaperiodate—Add 20 mL of
8.1 This test method covers the determination of manganese
KIO solution to 1 L of water, mix, heat at not less than 90°C
in concentrations from 0.01 to 2.5 %.
for 20 to 30 min, and cool. Use this water to dilute solutions to
volume that have been treated with KIO solution to oxidize
9. Summary of Test Method 4
manganese, and thus avoid reduction of permanganate ions by
9.1 Manganous ions are oxidized to permanganate ions by
any reducing agents in the untreated water. Caution—Avoid
reaction with metaperiodate ions. Solutions of the samples are
the use of this water for other purposes.
fumed with perchloric acid so that the effect of metaperiodate
ion is limited to the oxidation of manganese. Photometric
14. Preparation of Calibration Curve
measurement is made at approximately 545 nm.
14.1 Calibration Solutions—Using pipets, transfer 5, 10,
15, 20, and 25 mL of manganese standard solution (1
10. Concentration Range
mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetric
10.1 The recommended concentration range is from 0.15 to
flasks, and, if necessary, dilute to approximately 25 mL.
0.8 mg of manganese per 50 mL of solution, using a 1-cm cell
Proceed as directed in 14.3.
(Note 1) and a spectrophotometer with a band width of 10 nm
14.2 Reference Solution—Transfer approximately 25 mL of
or less.
water to a 50-mL borosilicate glass volumetric flask. Proceed
NOTE 1—This test method has been written for cells having a 1-cm
as directed in 14.3.
light path and a “narrow-band” instrument. The concentration range
14.3 Color Development—Add 10 mL of KIO solution,
depends upon band width and spectral region used as well as cell optical
and heat the solutions at not less than 90°C for 20 to 30 min
path length. Cells having other dimensions may be used, provided suitable
(Note 2). Cool, dilute to volume with pretreated water, and
adjustments can be made in the amounts of sample and reagents used.
mix.
11. Stability of Color
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
11.1 The color is stable for at least 24 h.
development.
12. Interferences
14.4 Photometry:
14.4.1 Multiple-Cell Photometer—Measure the cell correc-
12.1 The elements ordinarily present do not interfere. Per-
chloric acid treatment, which is used in the procedure, yields tion using the Reference Solution (14.2) in absorption cells
with a 1-cm light path and using a light band centered at
solutionswhichcanbehighlycoloredduetothepresenceofCr
(VI) ions. Although these ions and other colored ions in the approximately545nm.Usingthetestcell,takethephotometric
readings of the calibration solutions versus the reference
sample solution undergo no further change in color quality
upon treatment with metaperiodate ion, the following precau- solution (14.2).
14.4.2 Single-Cell Photometer—Transfer a suitable portion
tionsmustbeobservedwhenfilterphotometersareused:Select
a filter with maximum transmittance between 545 and 565 nm. of the reference solution (14.2) to an absorption cell with a
1-cm light path and adjust the photometer to the initial setting,
The filter must transmit not more than5%ofits maximum at
a wavelength shorter than 530 nm. The band width of the filter using a light band centered at approximately 545 nm. While
maintaining this adjustment, take the photometric readings of
should be less than 30 nm when measured at 50 % of its
maximum transmittance. Similar restrictions apply with re- the calibration solutions.
14.5 Calibration Curve—Plot the net photometric readings
spect to the wavelength region employed when other “wide-
band” instruments are used. of
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