ASTM E247-96

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

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  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 oi 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: 09-Nov-2001
• 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

• Replaced By: ASTM E247-01 - Standard Test Method for Determination of Silica in Manganese Ores, Iron Ores, and Related Materials by Gravimetry
• Effective Date: 10-Nov-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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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 247 – 96
Standard Test Method for
Determination of Silica in Manganese Ores, Iron Ores, and
Related Materials by Gravimetry
This standard is issued under the fixed designation E 247; 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 in a properly equipped laboratory and that proper waste
disposal procedures will be followed. Appropriate quality
1.1 This test method covers the determination of silica in
control practices must be followed such as those described in
iron ores, iron ore concentrates and agglomerates, and manga-
Guide E 882.
nese ore in the concentration range from 0.5 to 15 %.
1.2 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
5.1 This test method is written for iron and manganese ores
responsibility of the user oi this standard to establish appro-
containing less than 0.25 % of fluorine. None of the elements
priate safety and health practices and determine the applica-
normally found in iron ores or in manganese ores interfere with
bility of regulatory limitations prior to use.
this test method.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
2 6.1 Zirconium Crucible (50-mL capacity).
D 1193 Specification for Reagent Water
6.2 Platinum Filter Cone.
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
7. Reagents
E 877 Practice for Sampling and Sample Preparation of Iron
7.1 Purity of Reagents—Reagent grade chemicals shall be
Ores
used in all tests. Unless otherwise indicated, it is intended that
E 882 Guide for Accountability and Quality Control in the
4 all reagents conform to the specifications of the Committee on
Chemical Analysis Laboratory
Analytical Reagents of the American Chemical Society where
such specification are available. Other grades may be used,
3. Summary of Test Method
provided it is first ascertained that the reagent is of sufficient
3.1 The sample is fused with sodium peroxide in a zirco-
high purity to permit its use without lessening the accuracy of
nium crucible. The melt is leached with water and dissolved in
the determination.
hydrochloric acid. Silica is separated by double dehydration
7.2 Purity of Water—Unless otherwise indicated, refer-
with perchloric acid. The two precipitates are combined,
ences to water shall be understood to mean reagent water as
ignited, and weighed. The silica is volatilized by treatment with
defined by Type I of Specification D 1193.
hydrofluoric and sulfuric acids and the residue weighed.
7.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
4. Significance and Use chloric acid (HCl).
7.4 Hydrochloric Acid (1 + 49)—Mix 1 volume of concen-
4.1 This test method is intended to be used for compliance
trated HCl (sp gr 1.19) with 49 volumes of water.
with compositional specifications for silica content. It is
7.5 Hydrofluoric Acid (48%)—Concentrated hydrofluoric
assumed that all who use these procedures will be trained
acid (HF).
analysts capable of performing common laboratory procedures
7.6 Perchloric Acid (70%) (HClO ).
skillfully and safely. It is expected that work will be performed 4
7.7 Sodium Peroxide Powder (Na O ).
2 2
7.8 Sulfuric Acid (1 + 1)—Carefully pour 1 volume of
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved April 10, 1996. Published June 1996. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as E 247 – 64 T. Last previous edition E 247 – 95. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 14.02. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 03.06. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 247
concentrated sulfuric acid (H SO , sp gr 1.84) into 1 volume of reserved filter paper and residue in the platinum crucible.
2 4
water. 9.4 Ignite crucible and contents at 500°C for 1 h and then at
1000°C for 30 min. Cool in a desiccator. After 20 min, weigh.
8. Sampling and Sample Preparation
9.5 Add 6 drops of H SO (1 + 1) (7.8) to moisten the
2 4
8.1 Sampling—The gross sample shall be collected and
contents of the crucible. Add 5 mL of HF. Cautiously and
prepared in acordance with Practice E 877.
slowly heat to the absence of SO fumes. Ignite the residue in
8.2 Sample Preparation—The laboratory sample shall be
a muffle furnace at 1000°C for 10 min. Cool in a desiccator.
pulverized to pass a No. 100 (150-μm) sieve.
After 20 min, weigh. The difference in weight is the weight of
the silica.
NOTE 1—To facilitate decomposition, some ores, such as specular
hematite, require grinding to pass a No. 200 (75-μm) sieve.
A
TABLE 1 Statistical Summary
8.3 Sample Weight—Weigh approximately (within 625 mg)
an amou
...