ASTM E372-01(2006)
(Test Method)Standard Test Method for Determination of Calcium and Magnesium in Magnesium Ferrosilicon
Standard Test Method for Determination of Calcium and Magnesium in Magnesium Ferrosilicon
SIGNIFICANCE AND USE
This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use this test method 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 This test method covers the chemical analysis of magnesium ferrosilicon having chemical compositions within the following limits:
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. For general precautions to be observed in this test method, refer to Practices E 50.
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Designation: E372 − 01 (Reapproved2006)
Standard Test Method for
Determination of Calcium and Magnesium in Magnesium
Ferrosilicon
This standard is issued under the fixed designation E372; 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.
1. Scope E173 Practice for Conducting Interlaboratory Studies of
Methods for Chemical Analysis of Metals (Withdrawn
1.1 This test method covers the chemical analysis of mag-
1998)
nesium ferrosilicon having chemical compositions within the
following limits:
3. Significance and Use
Element Concentration Range, %
3.1 This test method for the chemical analysis of metals and
Aluminum 2.0 max
alloys is primarily intended to test such materials for compli-
Calcium 0.25 to 3.00
Carbon 0.50 max ance with compositional specifications. It is assumed that all
Cerium 1.0 max
who use this test method will be trained analysts capable of
Chromium 0.50 max
performing common laboratory procedures skillfully and
Magnesium 2.00 to 12.00
Manganese 1.0 max safely. It is expected that work will be performed in a properly
Silicon 40.00 to 55.00
equipped laboratory.
Sulfur 0.025 max
Titanium 0.2 max
4. Apparatus, Reagents, and Photometric Practice
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 Apparatus and reagents required for each determination
responsibility of the user of this standard to establish appro-
are listed in separate sections preceding the procedure. The
priate safety and health practices and determine the applica-
apparatus, standard solutions, and certain other reagents used
bility of regulatory limitations prior to use. For general
in more than one procedure are referred to by number and shall
precautions to be observed in this test method, refer to
conform to the requirements prescribed in Practices E50,
Practices E50.
except that photometers shall conform to the requirements
prescribed in Practice E60.
2. Referenced Documents
4.2 Photometric practice prescribed in this test method shall
2.1 ASTM Standards:
conform to Practice E60.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
5. Sampling
E32 Practices for Sampling Ferroalloys and Steel Additives
5.1 For procedures for sampling the material, refer to
for Determination of Chemical Composition
Methods E32.
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
6. Rounding Calculated Values
Related Materials
E60 Practice for Analysis of Metals, Ores, and Related
6.1 Calculated values shall be rounded to the desired num-
Materials by Spectrophotometry
ber of places as directed in 3.4 to 3.6 of Practice E29.
7. Interlaboratory Studies
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
7.1 This test method has been evaluated in accordance with
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Practice E173, unless otherwise noted in the precision and bias
Current edition approved Nov. 1, 2006. Published November 2006. Originally
section.
approved in 1976. Redesignated E372 in 1980. Last previous edition approved in
2001 as E372 – 01. DOI: 10.1520/E0372-01R06.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
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E372 − 01 (2006)
CALCIUM AND MAGNESIUM BY THE
B = EDTA solution required to titrate the calcium solution,
(ETHYLENEDINITRILO)TETRAACETIC ACID
mL.
(EDTA) TITRIMETRIC METHOD
12.3.3 Calculate the magnesium equivalent of the solution
as follows:
8. Scope
Magnesium equivalent, mg/mL 5 C 30.6068 (2)
8.1 This test method covers the determination of magne-
sium in concentrations from 2 to 12 % and calcium in
where C = calcium equivalent (12.3.2).
concentrations from 0.25 to 3.0 %.
12.4 Eriochrome Black-T Indicator Solution (6 g/L of
9. Summary of Test Method methanol)—Dissolve 0.3 g of Eriochrome Black-T and1gof
sodium borate decahydrate (Na B O ·10H O) in 50 mL of
2 4 7 2
9.1 Afterdissolutionofthesampleinnitricandhydrofluoric
methanol. Do not use a solution that has stood for more than 8
acids, an ammonium hydroxide precipitation is made to sepa-
h.
rate other elements from calcium and magnesium. Calcium,
and magnesium plus calcium are titrated in separate aliquot
12.5 Hydroxy Naphthol Blue Mixture—Add 1.0 g of indica-
portions after adding triethanolamine and potassium cyanide to tor to 100 g NaCl and mix thoroughly.
mask residual traces of iron, copper, nickel, manganese, and
12.6 Magnesium Chloride (2.5 g/L) —Dissolve 0.25 g of
aluminum that may be present. Calcium is titrated with
magnesium chloride hexahydrate (MgCl ·6H O) in 50 mL of
2 2
disodium (ethylenedinitrilo)tetraacetate (EDTA) at pH 12.
water, and dilute to 100 mL.
Magnesium plus calcium is titrated with EDTAat pH 10.0 and
themagnesiumconcentrationiscalculatedbycorrectingforthe 12.7 Potassium Cyanide Solution (50 g/L)—Dissolve2gof
potassium hydroxide (KOH) in water, add5gof potassium
volume of EDTA required to titrate the calcium.
cyanide (KCN) (Warning; see 12.7.1 ), dilute to 100 mL, and
10. Interferences
transfer to a plastic bottle.
12.7.1 Warning: The preparation, storage, and use of KCN
10.1 Provision is made for the removal or masking of
require care and attention. Avoid inhalation of fumes and
interfering elements ordinarily present in magnesium ferrosili-
exposure of the skin to the chemical and its solutions. Work in
con.
a well-ventilated hood. Refer to Section 7 of Practices E50.
11. Apparatus
12.8 Potassium Hydroxide Buffer Solution (pH 12.5)—
11.1 Beakers, TFE-fluorocarbon 500-mL.
Dissolve 531 g of KOH in water, add 50 g of KCN (Warning;
see 12.7.1 ), and dilute to 1 L. Store the solution in a plastic
11.2 pH Meter—Apparatus No. 3A.
container.
12. Reagents
12.9 Triethanolamine Solution (200
...
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