ASTM E372-84(1996)

Standard Test Method Determination of Calcium and Magnesium Ferrosilicon

SCOPE
1.1 This test method covers the chemical analysis of magnesium ferrosilicon having chemical compositions within the following limits:ElementConcentration Range, %Aluminum2.0 maxCalcium 0.25 to 3.00Carbon 0.50 maxCerium 1.0 maxChromium0.50 maxMagnesium2.00 to 12.00Manganese1.0 maxSilicon 40.00 to 55.00Sulfur 0.025 maxTitanium0.2 max
1.2 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 E50.

General Information

• Status: Historical
• Publication Date: 09-May-2001
• 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

• Replaced By: ASTM E372-01 - Standard Test Method Determination of Calcium and Magnesium Ferrosilicon
• Effective Date: 10-May-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 372 – 84 (Reapproved 1996)
Standard Test Method for
Chemical Analysis of Magnesium Ferrosilicon
This standard is issued under the fixed designation E 372; 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.
1. Scope ance with compositional specifications. It is assumed that all
who use this test method will be trained analysts capable of
1.1 This test method covers the chemical analysis of mag-
performing common laboratory procedures skillfully and
nesium ferrosilicon having chemical compositions within the
safely. It is expected that work will be performed in a properly
following limits:
equipped laboratory.
Element Concentration Range, %
4. Apparatus, Reagents, and Photometric Practice
Aluminum 2.0 max
Calcium 0.25 to 3.00
4.1 Apparatus and reagents required for each determination
Carbon 0.50 max
are listed in separate sections preceding the procedure. The
Cerium 1.0 max
Chromium 0.50 max
apparatus, standard solutions, and certain other reagents used
Magnesium 2.00 to 12.00
in more than one procedure are referred to by number and shall
Manganese 1.0 max
conform to the requirements prescribed in Practices E 50,
Silicon 40.00 to 55.00
Sulfur 0.025 max
except that photometers shall conform to the requirements
Titanium 0.2 max
prescribed in Practice E 60.
1.2 This standard does not purport to address all of the
4.2 Photometric practice prescribed in this test method shall
safety concerns, if any, associated with its use. It is the conform to Practice E 60.
responsibility of the user of this standard to establish appro-
5. Sampling
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For general 5.1 For procedures for sampling the material, refer to
precautions to be observed in this test method, refer to Methods E 32.
Practices E 50.
6. Rounding Calculated Values
2. Referenced Documents
6.1 Calculated values shall be rounded to the desired num-
2.1 ASTM Standards: ber of places as directed in 3.4 to 3.6 of Practice E 29.
E 29 Practice for Using Significant Digits in Test Data to
7. Interlaboratory Studies
Determine Conformance with Specifications
7.1 This test method has been evaluated in accordance with
E 32 Practices for Sampling Ferroalloys and Steel Additives
for Determination of Chemical Composition Practice E 173, unless otherwise noted in the precision and bias
section.
E 50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals
CALCIUM AND MAGNESIUM BY THE
E 60 Practice for Photometric and Spectrophotometric
3 (ETHYLENEDINITRILO)TETRAACETIC ACID
Methods for Chemical Analysis of Metals
(EDTA) TITRIMETRIC METHOD
E 173 Practice for Conducting Interlaboratory Studies of
Methods for Chemical Analysis of Metals
8. Scope
8.1 This test method covers the determination of magne-
3. Significance and Use
sium in concentrations from 2 to 12 % and calcium in
3.1 This test method for the chemical analysis of metals and
concentrations from 0.25 to 3.0 %.
alloys is primarily intended to test such materials for compli-
9. Summary of Test Method
This test method is under the jurisdiction of ASTM Committee E-1 on
9.1 After dissolution of the sample in nitric and hydrofluoric
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
acids, an ammonium hydroxide precipitation is made to sepa-
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
rate other elements from calcium and magnesium. Calcium,
Current edition approved Oct. 26, 1984. Published January 1985. Originally
published as E 568 – 76 T. Redesignated E 372 in 1980. Last previous edition
and magnesium plus calcium are titrated in separate aliquot
E 372 – 80.
portions after adding triethanolamine and potassium cyanide to
Annual Book of ASTM Standards, Vol 14.02.
3 mask residual traces of iron, copper, nickel, manganese, and
Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 372
aluminum that may be present. Calcium is titrated with cyanide (KCN) (Caution, Note 2), dilute to 100 mL, and
disodium (ethylenedinitrilo)tetraacetate (EDTA) at pH 12. transfer to a plastic bottle.
Magnesium plus calcium is titrated with EDTA at pH 10.0 and
NOTE 2—Caution: The preparation, storage, and use of KCN require
the magnesium concentration is calculated by correcting for the
care and attention. Avoid inhalation of fumes and exposure of the skin to
volume of EDTA required to titrate the calcium.
the chemical and its solutions. Work in a well-ventilated hood. Refer to
Section 7 of Practices E 50.
10. Interferences
12.8 Potassium Hydroxide Buffer Solution (pH 12.5)—
10.1 Provision is made for the removal or masking of
Dissolve 531 g of KOH in water, add 50 g of KCN (Caution,
interfering elements ordinarily present in magnesium ferrosili-
Note 2), and dilute to 1 L. Store the solution in a plastic
con.
container.
12.9 Triethanolamine Solution (200 mL/L)—Dilute 20 mL
11. Apparatus
of triethanolamine to 100 mL with water.
11.1 Beakers, TFE-fluorocarbon 500-mL.
13. Procedure
11.2 pH Meter—Apparatus No. 3A.
13.1 Transfer a 1.0-g sample, weighed to the nearest 0.1 mg,
12. Reagents
to a dry 500-mL TFE-fluorocarbon beaker. Add 10 mL of
HNO . Cautiously add 10 mL of HF, and heat gently until the
12.1 Ammonium Chloride Buffer Solution (pH 10.0)— 3
sample is dissolved. Wash the sides of the beaker with a fine
Dissolve 60 g of ammonium chloride (NH Cl) in 200 mL of
stream of water. Add 20 mL of HClO , place on a hot plate with
water, add 570 mL of NH OH, and dilute to 1 L. 4
a surface temperature not exceeding 300°C, and evaporate to
12.2 Calcium, Standard Solution (1 mL = 0.2002 mg Ca)—
dense fumes of HClO . Cool, add 10 mL of HCl (1+1), and
Dissolve 0.5000 g of calcium carbonate (CaCO ) (purity: 4
heat to dissolve salts. Transfer to a 600-mL glass beaker and
99.9 % min) in 100 mL of HCl (5+95). Boil 1 min, cool,
evaporate to moderate dryness on a hot plate. Place on a burner
transfer to a 1-L volumetric flask, dilute to volume, an
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