GB/T 6730.10-2014 PDF English
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Iron ores -- Determination of silicon content -- Gravimetric methods
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| GB/T 6730.10-1986 | English | 199 |
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Methods for chemical analysis of iron ores--The gravimetric method for the determination of silicon content
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.10
D 31
Replacing GB/T 6730.10-1986
Iron Ores - Determination of Silicon Content -
Gravimetric Methods
(ISO 2598-1.1992 Iron Ores - Determination of Silicon Content - Part 1.
Gravimetric Methods, NEQ)
Issued on. SEPTEMBER 30, 2014
Implemented on. MAY 1, 2015
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative References... 5
3 Principle... 6
4 Reagents and Materials... 6
5 Instruments... 7
6 Test Portion... 7
7 Analytical Procedures... 8
8 Result Calculation... 12
9 Test Report... 15
Appendix A (Normative) Flow Chart of Specimen Analytical Value Acceptance
Procedure... 16
Appendix B (Informative) Formula Derivation of Repeatability and Tolerance 17
Appendix C (Informative) Precision Data Obtained in International Analytical
Tests... 18
Foreword
GB/T 6730 Iron Ores is divided into 64 parts.
This is Part 10 of GB/T 6730.
This Part was drafted in accordance with the rules provided in GB/T 1.1-2009.
This Part serves as a replacement of GB/T 6730.10-1986 Methods for Chemical
Analysis of Iron Ores - The Gravimetric Method for the Determination of Silicon Content.
In comparison with GB/T 6730.10-1986, apart from editorial modifications, the main
technical changes are as follows.
---In the previous version, the specimen is decomposed with hydrochloric acid,
and the residue is melted with a mixed solvent of sodium carbonate and boric
acid. In this Part, two methods are used for the decomposition of the test portion.
Method 1 uses sodium peroxide to melt and decompose, then, uses
hydrochloric acid and perchloric acid for treatment; Method 2 uses hydrochloric
acid, nitric acid and perchloric acid (if necessary, including boric acid) to
dissolve, and evaporates, until it emits perchloric acid fumes; then, filters the
silica precipitate together with all residues; uses sodium carbonate to melt it,
and dissolves it in hydrochloric acid and perchloric acid.
---The range of determination is modified from 1.50% ~ 25.00% to 1.00% ~ 15.00%.
---In the previous version, in terms of data processing, rounding off the result data
in accordance with the numerical rounding-off rules is only mentioned, without
making a specific statement. After the revision, specific requirements are made
for the data rounding-off rules.
---The clause of safety warning is added.
---Specific requirements for the content of the test report are added.
This Part uses the re-drafting method and takes ISO 2598-1.1992 Iron Ores -
Determination of Silicon Content - Part 1.Gravimetric Methods as a reference in the
formulation. The degree of consistency with ISO 2598-1.1992 is non-equivalent.
In comparison with ISO 2598-1.1992, the technical differences and the causes for the
differences are as follows.
---In terms of Normative References, this Part makes adjustments with technical
differences to adapt to the technical conditions of China. The adjustment is
intensively reflected in Chapter 2 “Normative References”. See the specific
adjustment below.
The reference of GB/T 6682 is added (see Chapter 4);
GB/T 6730.1, which equivalently adopts international standard, is used to
replace ISO 7764 (see 6.1);
GB/T 6730.3, which equivalently adopts international standard, is used to
replace ISO 2596 (see 6.2.1);
GB/T 10322.1, which equivalently adopts international standard, is used to
replace ISO 3082 (see 6.1);
GB/T 12806, which non-equivalently adopts international standard, is used
to replace ISO 1042 (see Chapter 5);
GB/T 12808, which equivalently adopts international standard, is used to
replace ISO 648 (see Chapter 5).
---In the final result calculation in 8.2.3, the expression of ISO 2598-1.1992 is
modified in accordance with the expression mode of the current Chinese
standard, so as to be more consistent with the customs of China and facilitate
the application.
This Part was proposed by China Iron and Steel Association.
This Part shall be under the jurisdiction of National Technical Committee 317 on Iron
Ores and Directly Reduced Iron of Standardization Administration of China (SAC/TC
317).
The drafting organizations of this Part. ANSTEEL Group Mining Corporation Limited;
Shanghai Entry-Exit Inspection and Quarantine Bureau; Magang (Group) Holding Co.,
Ltd.; China Metallurgical Information and Standardization Institute.
The main drafters of this Part. Tian Hong, Chen Zhihua, Gao Jingjun, Ren Liping,
Cheng Jianping, Sun Deming, Yao Qiang.
The issuing of the previous versions.
---GB/T 1368-1978, GB/T 6730.10-1986.
Iron Ores - Determination of Silicon Content -
Gravimetric Methods
WARNING. This Part may involve hazardous substances, operations and
equipment. The personnel adopting this Part shall have practical experience in
formal laboratory work. This Part does not point out all possible safety issues.
It is the user’s responsibility to take appropriate safety and health measures and
ensure the proper scope of application before use.
1 Scope
This Part of GB/T 6730 specifies the gravimetric determination of silicon content in iron
ores.
This Part is applicable to natural iron ores, iron concentrates and man-made ore
agglomerates, including sintered products. The range of determination (mass fraction)
is 1.00% ~ 15.00%.
Method 1.this method is not applicable to iron ores with a reducing agent content
greater than 2% (mass fraction), for example, pyrite, or iron ores with fluorine content
greater than 0.1% (mass fraction). This method is recommended for low-grade ores
with a relatively high amphoteric element content.
Method 2.this method may be used for iron ores with fluorine content greater than 0.1%
(mass fraction). This method is recommended for high-grade ores with low gangue
content.
NOTE. for samples whose silicon content is less than 5% (mass fraction), the silico-
molybdic acid reduction spectrophotometry is more suitable.
2 Normative References
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods (GB/T
6682-2008, ISO 3696.1987, MOD)
GB/T 6730.1 Methods for Chemical Analysis of Iron Ores - Preparation of Pre-dried
Test Samples for Chemical Analysis (GB/T 6730.1-1986, idt ISO 7764.1985)
GB/T 6730.3 Methods for Chemical Analysis of Iron Ores - The Gravimetric Method for
the Determination of Hygroscopic Moisture Content in Analytical Samples (GB/T
6730.3-1986, idt ISO 2596.1984)
GB/T 10322.1 Iron Ores - Sampling and Sample Preparation Procedures (GB/T
10322.1-2000, ISO 3082.1998, IDT)
3 Principle
Use Method 1 or Method 2 to decompose the specimen to be tested.
Method 1.use sodium peroxide to melt and decompose, then, use hydrochloric acid
and perchloric acid for treatment.
4 Reagents and Materials
Unless it is otherwise stated in the analysis, only approved analytically pure reagents
and Grade-2 water that complies with the stipulations of GB/T 6682 are used in the
analysis.
4.1 Sodium peroxide, solid.
4.2 Boric acid, solid.
4.8 Sulfuric acid, 1 + 1.
4.9 Sulfuric acid, 1 + 9.
4.12 Silver nitrate solution, 10 g/L.
5 Instruments
Commonly used laboratory instruments, including one-mark volumetric flasks and one-
mark pipettes that comply with the stipulations of GB/T 12806 and GB/T 12808.
5.1 Nickel crucible, corundum crucible or graphite crucible. with a volume of about 40
mL.
5.2 Platinum crucible. with a volume of about 40 mL.
5.3 Nickel spoon.
6 Test Portion
6.1 Laboratory Specimens
In accordance with the stipulations of GB/T 10322.1, conduct sampling and specimen
preparation. Generally speaking, the particle size of the specimen shall be less than
100 m. When the content of ore combined water or easily oxidized compounds is
relative high, the particle size shall be less than 160 m.
6.2 Preparation of Specimens
In accordance with the type of ores, prepare the specimens in accordance with 6.2.1
or 6.2.2.
6.2.1 The content of combined water or easily oxidized compounds is relatively high,
and the silicon content is higher than 10% (mass fraction).
Under the circumstance where the silicon content is higher than 10% (mass fraction),
for the following types of ores, prepare an air balance specimen (see GB/T 6730.3).
7 Analytical Procedures
WARNING. during the operation of the decomposition of the test portion (see
7.4.1.1 and 7.4.1.2), safety goggles shall be worn.
7.1 Number of Determinations
In accordance with Appendix A, perform at least two independent analyses on a pre-
dried specimen.
7.2 Amount of Test Portion
In accordance with Table 1, weigh-take an approximate amount of the pre-dried
specimen, accurate to 0.0002 g.
7.3 Blank Test and Verification Test
For each operation, under the same conditions, a standard sample of the same type
of ore shall be analyzed in parallel with the ore specimen and a blank test shall be
performed. The pre-drying of the standard sample shall be performed in accordance
with the stipulations of 6.2.The standard sample and the analytical sample shall be of
the same type, and the properties shall be sufficiently similar, so as to ensure that there
are no changes in the analytical procedures of the standard sample and the analytical
sample.
7.4 Determination
7.4.1 Decomposition of test portion
7.4.1.1 Alkali fusion method (Method 1)
Place the specimen (see 7.2) in a nickel crucible, corundum crucible or graphite
crucible (see 5.1); add 3 g of sodium peroxide (see 4.1); use nickel spoon (see 5.3) to
mix and fill it.
7.4.1.2 Acid-soluble method (Method 2)
Place the test portion (see 7.2) in a 400 mL beaker in low form; use 5 mL of water to
moisten it. For ores with fluorine content greater than 0.1% (mass fraction) or unknown
fluorine content, before adding 5 mL of water, firstly, add 0.8 g of boric acid (see 4.2)
to the beaker containing the test portion.
8 Result Calculation
8.1 Calculation of Silicon Content
The silicon content, counted in mass fraction wSi, expressed in (%), is calculated to
four decimal places in accordance with Formula (1).
8.2 General Treatment of Analytical Results
8.2.1 Repeatability and tolerance
The precision of this analytical method is represented by the following regression
equations (see Appendix B and Appendix C).
8.2.2 Acceptance of analytical values
There shall be no statistically significant difference between the analytical value of the
standard sample and its standard value. For a standard sample that has been analyzed
by at least 10 laboratories with a method similar to this method in both accuracy and
precision, the difference may be determined through Formula (6);
8.3 Calculation of Silica Content
The silica content, counted in mass fraction, expressed in (%), is calculated in
accordance with Formula (8).
9 Test Report
The test report shall at least include the following information.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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