ASTM E247-01(2010)

Standard Test Method for Determination of Silica in Manganese Ores, Iron Ores, and Related Materials by Gravimetry

SIGNIFICANCE AND USE
This test method is intended to be used for compliance with compositional specifications for silica content. It is assumed that all who use these procedures 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 and that proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described in Guide E882.
SCOPE
1.1 This test method covers the determination of silica in iron ores, iron ore concentrates and agglomerates, and manganese ore in the concentration range from 0.5 % to 15 %.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Apr-2005
• ICS: 73.060.10 - Iron ores
• ICS: 73.060.20 - Manganese ores
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.02 - Ores, Concentrates, and Related Metallurgical Materials

Relations

• Replaces: ASTM E247-01(2005) - Standard Test Method for Determination of Silica in Manganese Ores, Iron Ores, and Related Materials by Gravimetry
• Effective Date: 01-May-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: E247 − 01 (Reapproved 2010)
StandardTest Method for
Determination of Silica in Manganese Ores, Iron Ores, and
Related Materials by Gravimetry
This standard is issued under the fixed designation E247; 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 4. Summary of Test Method
1.1 This test method covers the determination of silica in 4.1 The sample is fused with sodium peroxide in a zirco-
iron ores, iron ore concentrates and agglomerates, and manga- nium crucible. The melt is leached with water and dissolved in
nese ore in the concentration range from 0.5 % to 15 %. HCl. Silica is separated by double dehydration with HClO .
The two precipitates are combined, ignited, and weighed. The
1.2 The values stated in SI units are to be regarded as
silica is volatilized by treatment with HF and H SO and the
2 4
standard. No other units of measurement are included in this
residue weighed.
standard.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 This test method is intended to be used for compliance
responsibility of the user of this standard to establish appro-
with compositional specifications for silica content. It is
priate safety and health practices and determine the applica-
assumed that all who use these procedures will be trained
bility of regulatory limitations prior to use.
analysts capable of performing common laboratory procedures
2. Referenced Documents skillfully and safely. It is expected that work will be performed
in a properly equipped laboratory and that proper waste
2.1 ASTM Standards:
disposal procedures will be followed. Appropriate quality
D1193 Specification for Reagent Water
control practices must be followed such as those described in
E50 Practices for Apparatus, Reagents, and Safety Consid-
Guide E882.
erations for Chemical Analysis of Metals, Ores, and
Related Materials
6. Interferences
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials 6.1 This test method is written for iron and manganese ores
containing less than 0.25 % of fluorine. None of the elements
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method normallyfoundinironoresorinmanganeseoresinterferewith
this test method.
E877 Practice for Sampling and Sample Preparation of Iron
Ores and Related Materials for Determination of Chemi-
7. Apparatus
cal Composition
E882 Guide for Accountability and Quality Control in the
7.1 Zirconium Crucible (50-mL capacity).
Chemical Analysis Laboratory
7.2 Platinum Filter Cone.
3. Terminology
8. Reagents and Materials
3.1 Definitions—For definitions of terms used in this test
8.1 Purity of Reagents—Reagent grade chemicals shall be
method, refer to Terminology E135.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Reagents of the American Chemical Society where
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
such specification are available. Other grades may be used,
lurgical Materials.
Current edition approved June 15, 2010. Published August 2010. Originally
approved in 1964. Last previous edition approved in 2005 as E247 – 01 (2005).
DOI: 10.1520/E0247-01R10. Reagent Chemicals, American Chemical Society Specifications, American
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM testing of reagents not listed by the American Chemical Society, see the United
Standards volume information, refer to the standard’s Document Summary page on States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
the ASTM website. Inc. (USPC), Rockville, MD, http://www.usp.org.
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E247 − 01 (Reapproved 2010)
provided it is first ascertained that the reagent is of sufficient watchglass and heat to dense white fumes in the HClO fume
high purity to permit its use without lessening the accuracy of hood.Fumefor15 minto20 min.Coolfor1 minto2 min.Add
the determination. 50 mL of water containing 2 mL HCl (8.3) and heat the
contents to dissolve soluble salts. Filter through a fine-textured
8.2 Purity of Water—Unless otherwise indicated, refer-
paper with the aid of paper pulp and a platinum filter cone
ences to water shall be understood to mean reagent water as
usingsuction.WashfilterfivetimeswithhotHCl(1 + 49)(8.4)
defined by Type II of Specification D1193.
and then ten times with hot water, to remove all perchlorates
8.3 Hydrochloric Acid (sp gr 1.19)—Concentrated HCl.
(see Note 2). Reserve the filtrate. Transfer filter paper and
residue to a platinum crucible.
8.4 Hydrochloric Acid (1 + 49)—Mix 1 volume of concen-
trated HCl (sp gr 1.19) with 49 volumes of water.
NOTE 2—The residue must be washed free of perchlorates to prevent
possible loss of residue by deflagration during the ignition.
8.5 Hydrofluoric Acid (48 %)—Concentrated HF.
11.3 Add 10 mL of HClO to the reserved filtrate. Cover
8.6 Perchloric Acid (70 %)—HClO . 4
with a watchglass and take to dense white fumes and continue
8.7 Sodium Peroxide Powder—Na O .
2 2
fuming for 15 min to 20 min. Cool for 1 min to 2 min. Add
8.8 Sulfuric Acid (1 + 1)—Carefully pour one volume of
50 mL of water containing 2 mL of HCl (8.3). Heat the
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