ASTM E363-83(1997)e1

Standard Methods for Chemical Analysis of Chromium and Ferrochromium

SCOPE
1.1 These methods cover the chemical analysis of chromium and ferrochromium having chemical compositions within the following limits:
1.2 The analytical procedures appear in the following order:
1.3 This standard does not purport to address all of the safety problems, 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 precautionary statements are given in Section 5.

General Information

• Status: Historical
• Publication Date: 31-Dec-1982
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.01 - Iron, Steel, and Ferroalloys

Relations

• Replaced By: ASTM E363-83(2003)e1 - Standard Test Methods for Chemical Analysis of Chromium and 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
ε1
Designation:E363–83(Reapproved 1997)
Standard Methods for
Chemical Analysis of Chromium and Ferrochromium
This standard is issued under the fixed designation E 363; 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 (ε) indicates an editorial change since the last revision or reapproval.
ε NOTE—Keywords were added editorially in December 1997.
1. Scope 2. Referenced Documents
1.1 These methods cover the chemical analysis of chro- 2.1 ASTM Standards:
mium and ferrochromium having chemical compositions A 101 Specification for Ferrochromium
within the following limits: A 481 Specification for Chromium Metal
E 29 Practice for Using Significant Digits in Test Data to
Element Concentration, %
Determine Conformance with Specifications
Aluminum 0.25 max
E 32 PracticesforSamplingFerroalloysandSteelAdditives
Antimony 0.005 max
for Determination of Chemical Composition
Arsenic 0.005 max
Bismuth 0.005 max
E 50 Practices for Apparatus, Reagents, and Safety Precau-
Boron 0.005 max
tions for Chemical Analysis of Metals
Carbon 9.00 max
Chromium 51.0 to 99.5 E 60 Practice for Photometric and Spectrophotometric
Cobalt 0.10 max
Methods for Chemical Analysis of Metals
Columbium 0.05 max
E 173 Practice for Conducting Interlaboratory Studies of
Copper 0.05 max
Methods for Chemical Analysis of Metals
Lead 0.005 max
Manganese 0.75 max
E 360 Test Methods for Chemical Analysis of Silicon and
Molybdenum 0.05 max
Ferrosilicon
Nickel 0.50 max
Nitrogen 6.00 max E 361 Test Methods for ChemicalAnalysis of Ferromanga-
Phosphorus 0.03 max
nese and Spiegeleisen
Silicon 12.00 max
Silver 0.005 max
3. Significance and Use
Sulfur 0.07 max
Tantalum 0.05 max
3.1 These methods for the chemical analysis of metals and
Tin 0.005 max
alloys are primarily intended to test such materials for com-
Titanium 0.50 max
Vanadium 0.50 max pliance with compositional specifications. It is assumed that all
Zinc 0.005 max
who use these methods will be trained analysts capable of
Zirconium 0.05 max
performing common laboratory procedures skillfully and
1.2 The analytical procedures appear in the following order:
safely. It is expected that work will be performed in a properly
Sections equipped laboratory.
Arsenic by the Molybdenum Blue Photometric Method 9-19
4. Apparatus, Reagents, and Photometric Practice
Lead by the Dithizone Photometric Method 20-30
Chromium by the Sodium Peroxide Fusion-Titrimetric Method 31-37 4.1 Apparatus and reagents required for each determination
are listed in separate sections preceding the procedure. The
1.3 This standard does not purport to address all of the
apparatus, standard solutions, and certain other reagents used
safety concerns, if any, associated with its use. It is the
in more than one procedure are referred to by number and shall
responsibility of whoever uses this standard to consult and
conform to the requirements prescribed in Practices E 50,
establish appropriate safety and health practices and deter-
except that photometers shall conform to the requirements
mine the applicability of regulatory limitations prior to use.
prescribed in Practice E 60.
Specific precautionary statements are given in Section 5.
4.2 Photometric practice prescribed in these methods shall
conform to Practice E 60.
These methods are under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct Annual Book of ASTM Standards, Vol 01.02.
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. Annual Book of ASTM Standards, Vol 14.02.
Current edition approved Sept. 30, 1983. Published December 1983. Originally Annual Book of ASTM Standards, Vol 03.05.
published as E 363 – 70 T. Last previous edition E 363 – 75 (1979). Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E363
5. Safety Precautions 19. Precision and Bias
5.1 For precautions to be observed in the use of certain 19.1 Ninelaboratoriescooperatedintestingthismethodand
reagents in these methods, refer to Practices E 50. obtained the data summarized inTable 1. Samples with arsenic
concentrations near the upper limit of the scope were not
6. Sampling available for testing. The user is cautioned to verify, by the use
of reference materials, if available, that the precision and bias
6.1 For procedures for sampling the material, and for
of this method is adequate for the contemplated use.
particle size of the sample for chemical analysis, refer to
Practices E 32.
LEAD BY THE DITHIZONE PHOTOMETRIC
METHOD
7. Rounding Calculated Values
7.1 Calculated values shall be rounded to the desired num-
20. Scope
ber of places as directed in 3.4 to 3.6 of Practice E 29.
20.1 This method covers the determination of lead in
chromium and ferrochromium in concentrations from 0.001 to
8. Interlaboratory Studies
0.05 %.
8.1 These methods have been evaluated in accordance with
PracticeE 173,unlessotherwisenotedintheprecisionandbias
21. Summary of Method
section.
21.1 See Section 21 of Test Methods E 361.
ARSENIC BY THE MOLYBDENUM
22. Concentration Range
BLUEPHOTOMETRIC METHOD
22.1 See Section 22 of Test Methods E 361.
9. Scope
23. Stability of Color
9.1 This method covers the determination of arsenic in
23.1 See Section 23 of Test Methods E 361.
chromium and ferrochromium in concentrations from 0.001 to
0.005 %.
24. Interferences
24.1 See Section 24 of Test Methods E 361.
10. Summary of Method
10.1 See Section 10 of Test Methods E 360.
25. Apparatus
25.1 See Section 25 of Test Methods E 361.
11. Concentration Range
11.1 See Section 11 of Test Methods E 360.
26. Reagents
26.1 Proceed as directed in Section 26 of Test Methods
12. Stability of Color
E 361.
12.1 See Section 12 of Test Methods E 360.
27. Preparation of Calibration Curve
13. Interferences
27.1 Proceed as directed in 27.1 through 27.5 of Test
13.1 See Section 13 of Test Methods E 360.
Methods E 361.
14. Apparatus 28. Procedure
14.1 See Section 14 of Test Methods E 360. 28.1 Test Solution:
28.1.1 Transferasample,selectedinaccordancewith28.1.1
15. Reagents
of Test Methods E 361 and weighed to the nearest 0.1 mg, to
a 250-mL beaker. Add 30 mL of HCl (1 + 1) and heat until
15.1 Proceed as directed in 15.1 through 15.9 of Test
dissolution is nearly complete. In the case of high-carbon
Methods E 360.
ferrochromium (4.00 to 9.00 % C), add 30 mL of HCl
(concentrated) and several drops of HF, and heat until the
16. Preparation of Calibration Curve
reaction has subsided.
16.1 Proceed as directed in 16.1 through 16.5 of Test
28.1.2 Add several drops of HF (omit if added in preceding
Methods E 360.
paragraph) plus 10 mL of HNO and 10 mL of HClO .
3 4
Evaporate to heavy fumes of HClO and fume until the volume
17. Procedure
is reduced to approximately 5 mL. Add H O solution (1 + 9)
2 2
17.1 Proceed as directed in 17.1 through 17.4 of Test
Methods E 360.
TABLE 1 Statistical Information—Arsenic
18. Calculation Repeatability (R , Reproduci-
Ferroalloy Type Arsenic Found, %
E 173) bility (R , E 173)
18.1 Proceed as directed in Section 18 of Test Methods
1. 70Cr-1Si-5C 0.0015 0.0001 0.0005
E 360.
E363
dropwise until any precipitated manganese dioxide is dis- tion, and using a 50-mL buret, titrate with 0.1 N KMnO
solved. Boil to remove excess H O and cool. solutiontothecolorchangefromredtogreen.Recordtheburet
2 2
28.1.3 Proceed as directed in 28.1.4 through 28.4 of Test reading to the nearest 0.05 mL. Calculate the volume of 0.1 N
Methods E 361. K Cr O solution equivalent to1gof ferrous ammonium
2 2 7
sulfate as follows:
29. Calculation
A 5 ~200 1 B!/8 (1)
29.1 Proceed as directed in Section 29 of Test Methods
where:
E 361.
A = millilitres of 0.1 N K Cr O solution equivalent to 1 g
2 2 7
30. Precision and Bias
of ferrous ammonium sulfate, and
B = millilitres of 0.1 N KMnO solution used.
30.1 Four laboratories cooperated in testing this method and
The salt has proved to be stable for at least 1 week.
obtained the results shown in Table 2. Samples with lead
34.3 Ferrous Ammonium Sulfate, Standard Solution (0.25
concentrations near the upper limit of the scope were not
N) (Note 1)—Dissolve 89.6 g of Fe (NH ) (SO ) ·6H Oin
available for testing. The user is cautioned to verify, by the use 4 2 4 2 2
500 mL of cold H SO (5 + 95) and dilute to 1 litre with
2 4
of reference materials, if available, that the precision
...