GB/T 1508-2002 PDF English
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Manganese Ores - Determination of Total Iron Content - Potassium Dichromate Titrimetric Method and 1,10-Phenanthroline Spectrophotometric Method
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| GB/T 1508-1979 | English | 199 |
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Method for determination of total iron content in manganese ores
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GB/T 1508-2002: Manganese Ores - Determination of Total Iron Content - Potassium Dichromate Titrimetric Method and 1,10-Phenanthroline Spectrophotometric Method
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT1508-2002
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.20
D 32
Replacing GB/T 1508-1979
Manganese Ores – Determination of Total Iron Content
– Potassium Dichromate Titrimetric Method and 1,10-
Phenanthroline Spectrophotometric Method
Issued on. SEPTEMBER 11, 2002
Implemented on. APRIL 01, 2003
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Method I -- Potassium Dichromate Titrimetric Method... 5
4 Method II -- 1,10-Phenanthroline Spectrophotometric Method... 9
Foreword
There are several separate parts under the general title of Manganese Ores; and this
Part is one of them.
This Part includes the Method-I potassium dichromate titrimetric method, and Method-
II 1,10-phenanthroline spectrophotometric method. The Method-I, on the basis of GB/T
1508-1979, abandons the mercury method, while adopts the mercury-free method.
The Method-II modifies and adopts ISO 9292.1988 in the technical contents.
Compared with GB/T 1508-1979, Method-I has the major changes as follows.
--- Due to the contamination of mercury salts; abandon the mercury method, while
adopt the mercury-free method; and use neutral red as an indicator;
--- Change the sample decomposition method into hydrochloric acid dissolution and
slag return treatment.
Method-II modifies and adopts the international standard ISO 9292.1998; its major
changes are as follows.
--- The sampling volume is different from the volume of test solution;
--- The measurement range (mass fraction) is 0.10%~3.00%.
This Part was proposed by the original State Bureau of Metallurgical Industry.
This Part shall be under the jurisdiction of China Metallurgical Information and
Standardization Institute.
Drafting organization of this Part. Guilin Research Institute of Geology for Mineral
Resources.
Chief drafting staffs of this Part. Jin Xiaozhu, Yang Zhongping, Shi Yihua.
The historical edition replaced by this Standard is as follows.
--- GB/T 1508-1979.
Manganese Ores – Determination of Total Iron Content
– Potassium Dichromate Titrimetric Method and 1,10-
Phenanthroline Spectrophotometric Method
Warning. This Part does not point out all possible safety issues. It is the
responsibility of the user to take appropriate safety and health measures; and
ensure compliance with the conditions stipulated by relevant national
regulations.
1 Scope
This Part specifies the principle, reagents and materials, instruments, sampling and
sample preparation, analytical procedures, result calculation, etc. of using potassium
dichromate titrimetric method and 1,10-phenanthroline spectrophotometric method to
determine the total iron content.
This Part is applicable to the determination of total iron in the manganese ores and the
manganese concentrates with vanadium content (mass fraction) < 0.02%; the test
range (mass fraction). Method-I potassium dichromate titrimetric method is
2.00%~25.00%; while Method-II 1,10-phenanthroline spectrophotometric method is
0.10%~3.00%.
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB/T 2011 Method of Sampling and Sample Preparation of Manganese Ores in
Bulk
3 Method I -- Potassium Dichromate Titrimetric Method
3.1 Principle
The sample shall be decomposed by hydrochloric acid; the residue slag shall be
melted by potassium pyrosulfate. After leaching, the iron was precipitated and
separated by ammonia water; use the hydrochloric acid to dissolve the precipitate.
3.2 Reagents and materials
Unless otherwise specified, only the reagents that are determined to be analytically
pure and distilled water or water with equivalent purity shall be used in the analysis.
3.2.1 Potassium pyrosulfate.
3.2.2 Sodium fluoride.
3.2.9 Hydrochloric acid (1+4).
3.2.10 Hydrochloric acid (1+50).
3.2.11 Sulfuric acid (1+1).
3.2.12 Phosphoric acid (1+1).
3.2.13 Sulfur-phosphorus mixed acid. slowly add 150mL of sulfuric acid (ρ1.84g/mL)
into 500mL of water; after cooling off, add 150mL of phosphoric acid (3.2.5); use water
to dilute to 1000mL; mix evenly.
3.2.14 Ammonia water (1+50).
3.2.15 Hydrogen peroxide (volume fraction of 30%).
3.2.20 Neutral red indicator solution (1g/L).
3.2.21 Sodium diphenylamine sulfonate indicator solution (2g/L).
3.3 Instrument
The general laboratory instruments are used for analysis.
3.4 Sampling and sample preparation
The sampling and sample preparation shall be carried out as per the provisions of
GB/T 2011; the specimen shall pass through a 0.080mm sieve.
3.5 Analytical procedures
3.5.1 Sample mass
Take the air-dried sample according to Table 1, accurate to 0.0001g.
Meanwhile, take the air-dried sample according to the wet storage water content
measured by GB/T 14949.8-1994.
3.5.2 Blank test
Pipette 10.00mL of iron standard solution (3.2.19); perform the blank test together with
the sample.
3.5.3 Determination
3.7 Tolerance
The difference in analysis results between laboratories shall be no more than the
tolerance in Table 2.
3.8 Test report
The test report shall include the following contents.
4 Method II -- 1,10-Phenanthroline Spectrophotometric Method
4.1 Principle
The sample is decomposed by hydrochloric acid; the remaining slag is melted by
potassium pyrosulfate. Use hydroxylamine hydrochloride to reduce the ferric iron into
ferrous iron. At the acidity of pH 4~5, the ferrous iron and 1,10-phenanthroline forms a
red complex; then measure the absorbance at the wavelength of 510nm; calculate the
total iron content.
4.2 Reagents and materials
Unless otherwise specified, the reagents determined to be analytically pure and
distilled water or water with equivalent purity shall be used in the analysis.
4.3 Instrument
The general laboratory instruments are used for analysis.
4.4 Sampling and sample preparation
The sampling and sample preparation shall be carried out as per the provisions of
GB/T 2011; the specimen shall pass through a 0.080mm sieve.
4.5 Analytical procedures
4.5.1 Sample mass
Take the air-dried sample according to Table 3, accurate to 0.0001g.
Meanwhile, take the air-dried sample according to the wet storage water content
measured by GB/T 14949.8-1994.
4.5.2 Blank test
The blank test shall be performed together with sample.
4.5.3 Determination
4.5.3.1 Place the sample (4.5.1) into 300mL beaker; moisten it with water. Add 30mL
of hydrochloric acid (4.2.3); cover the stopper; heat slightly to dissolve; use warm water
to dilute to about 50mL. Filter by the medium-speed filter paper with a small amount of
pulp; use hot hydrochloric acid (4.2.4) and hot water to wash the precipitate for 4~5
times, respectively. Collect the filtrate and washings into 300mL beaker; reserve as the
main solution.
4.5.3.3 Separately-take test solution into 100mL volumetric flask according to Table 3;
add 50mL of water; add 5mL of hydroxylamine hydrochloride solution (4.2.6), mix
evenly. Stand for 5min; add 10mL of acetic acid-sodium acetate buffer solution (4.2.8),
10mL of 1,10-phenanthroline solution (4.2.7); stand for 1h at the room temperature or
in the 30°C water bath for 15min; cool off; dilute with water to the scale, mix evenly.
Measure the absorbance at the wavelength of 510nm by 1cm absorber with water as
reference on the spectrophotometer. After deducting the absorbance measured in the
blank test (4.5.2); find out the iron content form the calibration curve.
4.7 Tolerance
The difference in analysis results between laboratories shall be no more than the
tolerance in Table 4.
4.8 Test report
The test report shall include the following contents.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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