ASTM E247-01(2015)e1

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

SIGNIFICANCE AND USE
5.1 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 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: 14-Nov-2015
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
´1
Designation: E247 − 01 (Reapproved 2015)
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 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.
ε NOTE—Editorially corrected 1.1 and Table 1 in November 2015.
1. Scope 3. Terminology
3.1 Definitions—For definitions of terms used in this test
1.1 This test method covers the determination of silica in
method, refer to Terminology E135.
iron ores, iron ore concentrates and agglomerates, and manga-
nese ore in the range from 0.5 % to 15 %.
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as
4.1 The sample is fused with sodium peroxide in a zirco-
standard. No other units of measurement are included in this
nium crucible. The melt is leached with water and dissolved in
standard.
HCl. Silica is separated by double dehydration with HClO .
1.3 This standard does not purport to address all of the
The two precipitates are combined, ignited, and weighed. The
safety concerns, if any, associated with its use. It is the
silica is volatilized by treatment with HF and H SO and the
2 4
responsibility of the user of this standard to establish appro-
residue weighed.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
5.1 This test method is intended to be used for compliance
2. Referenced Documents
with compositional specifications for silica content. It is
2.1 ASTM Standards:
assumed that all who use these procedures will be trained
D1193 Specification for Reagent Water
analysts capable of performing common laboratory procedures
E50 Practices for Apparatus, Reagents, and Safety Consid-
skillfully and safely. It is expected that work will be performed
erations for Chemical Analysis of Metals, Ores, and
in a properly equipped laboratory and that proper waste
Related Materials
disposal procedures will be followed. Appropriate quality
E135 Terminology Relating to Analytical Chemistry for
control practices must be followed such as those described in
Metals, Ores, and Related Materials
Guide E882.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
6. Interferences
E877 Practice for Sampling and Sample Preparation of Iron
6.1 This test method is written for iron and manganese ores
Ores and Related Materials for Determination of Chemi-
containing less than 0.25 % of fluorine. None of the elements
cal Composition and Physical Properties
normallyfoundinironoresorinmanganeseoresinterferewith
E882 Guide for Accountability and Quality Control in the
this test method.
Chemical Analysis Laboratory
7. Apparatus
This test method is under the jurisdiction of ASTM Committee E01 on 7.1 Zirconium Crucible (50-mL capacity).
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
7.2 Platinum Filter Cone.
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Current edition approved Nov. 15, 2015. Published December 2015. Originally
8. Reagents and Materials
approved in 1964. Last previous edition approved in 2010 as E247 – 01 (2010).
DOI: 10.1520/E0247-01R15E01.
8.1 Purity of Reagents—Reagent grade chemicals shall be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
all reagents conform to the specifications of the Committee on
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Analytical Reagents of the American Chemical Society where
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
E247 − 01 (Reapproved 2015)
such specification are available. Other grades may be used, 10 mL to 15 mL of water into the crucible. When the reaction
provided it is first ascertained that the reagent is of sufficient ceases, empty the crucible contents and crucible rinsings into
high purity to permit its use without lessening the accuracy of the beaker. Add 25 mL HCl by means of the crucible. Finally,
the determination. rinse and police crucible with water and add rinsings to the
beaker. Heat to a boil to obtain a complete and clear solution.
8.2 Purity of Water—Unless otherwise indicated, refer-
Cool for 1 min to 2 min. Add 25 mL of HClO . Cover with a
ences to water shall be understood to mean reagent water as
watchglass and heat to dense white fumes in the HClO fume
defined by Type II of Specification D1193.
hood.Fumefor15 minto20 min.Coolfor1 minto2 min.Add
8.3 Hydrochloric Acid (sp gr 1.19)—Concentrated HCl.
50 mL of water containing 2 mL HCl (8.3) and heat the
8.4 Hydrochloric Acid (1 + 49)—Mix 1 volume of concen- contents to dissolve soluble salts. Filter through a fine-textured
paper with the aid of paper pulp and a platinum filter cone
trated HCl (sp gr 1.19) with 49 volumes of water.
usingsuction.WashfilterfivetimeswithhotHCl(1 + 49)(8.4)
8.5 Hydrofluoric Acid (48 %)—Concentrated HF.
and then ten times with hot water, to remove all perchlorates
8.6 Perchloric Acid (70 %)—HClO .
(see Note 2). Reserve the filtrate. Transfer filter paper and
residue to a platinum crucible.
8.7 Sodium Peroxide Powder—Na O .
2 2
8.8 Sulfuric Acid (1 + 1)—Carefully pour one volume of NOTE 2—The residue must be washed free of perchlorates to prevent
possible loss of residue by deflagration during the ignition.
concentrated H SO , sp gr 1.84, into one volume of water.
2 4
11.3 Add 10 mL of HClO to the reserved filtrate. Cover
9. Hazards
with a watchglass and take to dense white fumes and continue
9.1 For
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: E247 − 01 (Reapproved 2010) E247 − 01 (Reapproved 2015)
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 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.
ε NOTE—Editorially corrected 1.1 and Table 1 in November 2015.
1. 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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E877 Practice for Sampling and Sample Preparation of Iron Ores and Related Materials for Determination of Chemical
Composition and Physical Properties
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The sample is fused with sodium peroxide in a zirconium crucible. The melt is leached with water and dissolved in HCl.
Silica is separated by double dehydration with HClO . The two precipitates are combined, ignited, and weighed. The silica is
volatilized by treatment with HF and H SO and the residue weighed.
2 4
5. Significance and Use
5.1 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.
6. Interferences
6.1 This test method is written for iron and manganese ores containing less than 0.25 % of fluorine. None of the elements
normally found in iron ores or in manganese ores interfere with this test method.
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.
Current edition approved June 15, 2010Nov. 15, 2015. Published August 2010December 2015. Originally approved in 1964. Last previous edition approved in 20052010
as E247 – 01 (2005).(2010). DOI: 10.1520/E0247-01R10.10.1520/E0247-01R15E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
E247 − 01 (Reapproved 2015)
7. Apparatus
7.1 Zirconium Crucible (50-mL capacity).
7.2 Platinum Filter Cone.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specification are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient high purity
to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II of Specification D1193.
8.3 Hydrochloric Acid (sp gr 1.19)—Concentrated HCl.
8.4 Hydrochloric Acid (1 + 49)—Mix 1 volume of concentrated HCl (sp gr 1.19) with 49 volumes of water.
8.5 Hydrofluoric Acid (48 %)—Concentrated HF.
8.6 Perchloric Acid (70 %)—HClO .
8.7 Sodium Peroxide Powder—Na O .
2 2
8.8 Sulfuric Acid (1 + 1)—Carefully pour one volume of concentrated H SO , sp gr 1.84, into one volume of water.
2 4
9. Hazards
9.1 For precautions to be observed in this method, refer to Practices E50.
10. Sampling and Sample Preparation
10.1 Sampling—The gross sample shall be collected and prepared in accordance with Practice E877.
10.2 Sample Preparation—The laboratory sample shall be pulverized to pass a No. 100 (150-μm) sieve.
NOTE 1—To facilitate decomposition, some ores, such as specular hematite, require grinding to pass a No. 200 (75-μm) sieve.
10.3 Sample Weight—Weigh approximately (within 6 25 mg) an amount of test sample specified as following:
Content of Silica, % Weight of Test Sample, g
Less than 2 1.0
2 and over 0.5
11. Procedure
11.1 Transfer the test sample to a small, dry weighing bottle and place in a drying oven. Dry iron ore samples at 110 °C and
manganese ore samples at 120 °C for 1 h. Cap the bottle and cool to room temperature in a desiccator. Momentarily release the
cap to equalize pressure and weigh the capped bottle to the nearest 0.1 mg. Repeat the drying and weighing until there is no further
weight loss. Transfer the test sample to a zirconium crucible and reweigh the capped bottle to the n
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