ASTM E363-83(2003)e1

Standard Test Methods for Chemical Analysis of Chromium and Ferrochromium

SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 These test methods cover the chemical analysis of chromium and ferrochromium having chemical compositions within the following limits:ElementConcentration, %Aluminum0.25 maxAntimony0.005 maxArsenic0.005 maxBismuth0.005 maxBoron0.005 maxCarbon9.00 maxChromium51.0 to 99.5Cobalt0.10 maxColumbium0.05 maxCopper0.05 maxLead0.005 maxManganese0.75 maxMolybdenum0.05 maxNickel0.50 maxNitrogen6.00 maxPhosphorus0.03 maxSilicon12.00 maxSilver0.005 maxSulfur0.07 maxTantalum0.05 maxTin0.005 maxTitanium0.50 maxVanadium0.50 maxZinc0.005 maxZirconium0.05 max
1.2 The analytical procedures appear in the following order: SectionsArsenic by the Molybdenum Blue Photometric Method9-19Lead by the Dithizone Photometric Method20-30Chromium by the Sodium Peroxide Fusion-Titrimetric Method31-37
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 5.

General Information

• Status: Historical
• Publication Date: 09-Jun-2003
• ICS: 77.040.30 - Chemical analysis of metals
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.01 - Iron, Steel, and Ferroalloys

Relations

• Replaces: ASTM E363-83(1997)e1 - Standard Methods for Chemical Analysis of Chromium and Ferrochromium
• Effective Date: 10-Jun-2003
• Replaced By: ASTM E363-09 - Standard Test Methods for Chemical Analysis of Chromium and Ferrochromium
• Effective Date: 01-Oct-2009
• Referred By: ASTM A481-05(2020) - Standard Specification for Chromium Metal
• Effective Date: 10-Jun-2003
• Referred By: ASTM A101-04(2019) - Standard Specification for Ferrochromium
• Effective Date: 10-Jun-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation:E363–83(Reapproved 2003)
Standard Test Methods for
Chemical Analysis of Chromium and Ferrochromium
This standard is issued under the fixed designation E363; 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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Warnings were moved from notes to section text editorially December 2002.
1. Scope mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Section 5.
1.1 These test methods cover the chemical analysis of
chromium and ferrochromium having chemical compositions
2. Referenced Documents
within the following limits:
2.1 ASTM Standards:
Element Concentration, %
A101 Specification for Ferrochromium
Aluminum 0.25 max
A481 Specification for Chromium Metal
Antimony 0.005 max
E29 Practice for Using Significant Digits in Test Data to
Arsenic 0.005 max
Determine Conformance with Specifications
Bismuth 0.005 max
Boron 0.005 max
E32 Practices for Sampling Ferroalloys and SteelAdditives
Carbon 9.00 max
for Determination of Chemical Composition
Chromium 51.0 to 99.5
E50 Practices for Apparatus, Reagents, and Safety Consid-
Cobalt 0.10 max
Columbium 0.05 max
erations for Chemical Analysis of Metals, Ores, and
Copper 0.05 max
Related Materials
Lead 0.005 max
E60 Practice for Analysis of Metals, Ores, and Related
Manganese 0.75 max
Molybdenum 0.05 max
Materials by Molecular Absorption Spectrometry
Nickel 0.50 max
E173 Practice for Conducting Interlaboratory Studies of
Nitrogen 6.00 max
Phosphorus 0.03 max Test Methods for Chemical Analysis of Metals
Silicon 12.00 max
E360 Test Methods for Chemical Analysis of Silicon and
Silver 0.005 max
Ferrosilicon
Sulfur 0.07 max
E361 Test Methods for the Determination of Arsenic and
Tantalum 0.05 max
Tin 0.005 max
Lead in Ferromanganese
Titanium 0.50 max
Vanadium 0.50 max
3. Significance and Use
Zinc 0.005 max
Zirconium 0.05 max
3.1 These test methods for the chemical analysis of metals
and alloys are primarily intended to test such materials for
1.2 The analytical procedures appear in the following order:
compliance with compositional specifications. It is assumed
Sections
that all who use these test methods will be trained analysts
Arsenic by the Molybdenum Blue Photometric Method 9-19
capable of performing common laboratory procedures skill-
Lead by the Dithizone Photometric Method 20-30
fully and safely. It is expected that work will be performed in
Chromium by the Sodium Peroxide Fusion-Titrimetric Method 31-37
a properly equipped laboratory.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Apparatus, Reagents, and Photometric Practice
responsibility of whoever uses this standard to consult and
4.1 Apparatus and reagents required for each determination
establish appropriate safety and health practices and deter-
are listed in separate sections preceding the procedure. The
1 2
These test methods are under the jurisdiction of ASTM Committee E01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 10, 2003. Published July 2003. Originally the ASTM website.
approved in 1970. Last previous edition approved in 2002 as E363 – 83 (2002). Withdrawn. The last approved version of this historical standard is referenced
DOI: 10.1520/E0363-83R03E01. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E363–83 (2003)
TABLE 1 Statistical Information—Arsenic
apparatus, standard solutions, and certain other reagents used
in more than one procedure are referred to by number and shall Repeatability (R , Reproduci-
Ferroalloy Type Arsenic Found, %
E173) bility (R , E173)
conform to the requirements prescribed in Practices E50,
1. 70Cr-1Si-5C 0.0015 0.0001 0.0005
except that photometers shall conform to the requirements
prescribed in Practice E60.
4.2 Photometric practices prescribed in these test methods
17. Procedure
shall conform to Practice E60.
17.1 Proceed as directed in 17.1 through 17.4 of Test
5. Safety Hazards Methods E360.
5.1 For precautions to be observed in the use of certain
18. Calculation
reagents in these test methods, refer to Practices E50.
18.1 Proceed as directed in Section 18 of Test Methods
E360.
6. Sampling
6.1 For procedures for sampling the material, and for
19. Precision and Bias
particle size of the sample for chemical analysis, refer to
19.1 Ninelaboratoriescooperatedintestingthismethodand
Practices E32.
obtained the data summarized inTable 1. Samples with arsenic
concentrations near the upper limit of the scope were not
7. Rounding Calculated Values
available for testing. The user is cautioned to verify, by the use
7.1 Calculated values shall be rounded to the desired num-
of reference materials, if available, that the precision and bias
ber of places as directed in 6.4 to 6.6, Rounding Procedure, of
of this method is adequate for the contemplated use.
Practice E29.
LEAD BY THE DITHIZONE PHOTOMETRIC
8. Interlaboratory Studies
METHOD
8.1 These test methods have been evaluated in accordance
20. Scope
withPracticeE173,unlessotherwisenotedintheprecisionand
bias section.
20.1 This method covers the determination of lead in
chromium and ferrochromium in concentrations from 0.001 to
ARSENIC BY THE MOLYBDENUM BLUE
0.05 %.
PHOTOMETRIC METHOD
21. Summary of Method
9. Scope
21.1 See Section 21 of Test Methods E361.
9.1 This method covers the determination of arsenic in
22. Concentration Range
chromium and ferrochromium in concentrations from 0.001 to
0.005 %. 22.1 See Section 22 of Test Methods E361.
23. Stability of Color
10. Summary of Method
23.1 See Section 23 of Test Methods E361.
10.1 See Section 10 of Test Methods E360.
24. Interferences
11. Concentration Range
24.1 See Section 24 of Test Methods E361.
11.1 See Section 11 of Test Methods E360.
25. Apparatus
12. Stability of Color
25.1 See Section 25 of Test Methods E361.
12.1 See Section 12 of Test Methods E360.
26. Reagents
13. Interferences
26.1 Proceed as directed in Section 26 of Test Methods
13.1 See Section 13 of Test Methods E360.
E361.
14. Apparatus
27. Preparation of Calibration Curve
14.1 See Section 14 of Test Methods E360.
27.1 Proceed as directed in 27.1 through 27.5 of Test
Methods E361.
15. Reagents
28. Procedure
15.1 Proceed as directed in 15.1 through 15.9 of Test
Methods E360.
28.1 Test Solution:
28.1.1 Transferasample,selectedinaccordancewith28.1.1
16. Preparation of Calibration Curve
of Test Methods E361 and weighed to the nearest 0.1 mg, to a
16.1 Proceed as directed in 16.1 through 16.5 of Test 250-mL beaker. Add 30 mL of HCl (1 + 1) and heat until
Methods E360. dissolution is nearly complete. In the case of high-carbon
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E363–83 (2003)
TABLE 2 Statistical Information—Lead
34.2 Ferrous Ammonium Sulfate Salt—Fine, well mixed,
Ferroalloy Type Lead Found, % free flowing crystals of Fe (NH ) (SO ) ·6H O will be re-
4 2 4 2 2
quired. Standardize as follows: Transfer 0.9806 g of NBS
1. Electrolytic Cr Metal Lab A: 0.0020, 0.0020
0.0019, 0.0020
K Cr O (equivalent to 200 mLof 0.1 N solution) to a 600-mL
2 2 7
Lab B: 0.0025, 0.0023
beaker.Add300mLofwater,30mLofH SO (1 + 1),and8.00
2 4
0.0020, 0.0011
g of the ferrous ammonium sulfate. Stir until completely
Lab C: 0.0020, 0.0021
0.0020, 0.0020
dissolved. Add 6 drops of 1,10-phenanthroline indicator solu-
Lab D: 0.0011, 0.0009
tion, and using a 50-mL buret, titrate with 0.1 N KMnO
Average: 0.0019
solutiontothecolorchangefromredtogreen.Recordtheburet
reading to the nearest 0.05 mL. Calculate the volume of 0.1 N
K Cr O solution equivalent to1gof ferrous ammonium
2 2 7
ferrochromium (4.00 to 9.00 % C), add 30 mL of HCl
sulfate as follows:
(concentrated) and several drops of HF, and heat until the
A 5 ~200 1 B!/8 (1)
reaction has subsided.
28.1.2 Add several drops of HF (omit if added in preceding where:
paragraph) plus 10 mL of HNO and 10 mL of HClO . A = millilitres of 0.1 N K Cr O solution equivalent to 1 g
2 2 7
3 4
Evaporate to heavy fumes of HClO and fume until the volume of ferrous ammonium sulfate, and
B = millilitres of 0.1 N KMnO solution used.
is reduced to approximately 5 mL. Add H O solution (1 + 9)
2 2
dropwise unti
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