GB/T 5686.2-2022 PDF English
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| GB/T 5686.2-2022 | English | 230 |
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Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal - Determination of silicon content - Molybdenum blue spectrophotometric method, silicon potassium fluoride titrimetric method and perchloric acid dehydration gravimetric method
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| GB/T 5686.2-2008 | English | 145 |
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Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal -- Determination of silicon content -- Molybdenum blue photometric method, silicon potassium fluoride titrimetric method and perchloric acid dehydration gravimetri
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| GB/T 5686.2-1985 | English | 199 |
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Methods for chemical analysis of silicomanganese alloy--The gravimetric method for the determination of silicon content
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GB/T 5686.2-2022: Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal - Determination of silicon content - Molybdenum blue spectrophotometric method, silicon potassium fluoride titrimetric method and perchloric acid dehydration gravimetric 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/GBT5686.2-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
CCS H 11
Replacing GB/T 5686.2-2008
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of Silicon
Content - Molybdenum Blue Spectrophotometric Method, Silicon
Potassium Fluoride Titrimetric Method and Perchloric Acid
Dehydration Gravimetric Method
Issued on. OCTOBER 12, 2022
Implemented on. FEBRUARY 1, 2023
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 5
1 Scope... 7
2 Normative References... 7
3 Terms and Definitions... 8
4 Method 1.Molybdenum Blue Spectrophotometric Method... 8
5 Method 2.Silicon Potassium Fluoride Titrimetric Method... 12
6 Method 3.Perchloric Acid Dehydration Gravimetric Method... 16
7 Test Report... 20
Appendix A (normative) Flow Chart of Specimen Analysis Result Acceptance
Procedure... 21
Foreword
This document was drafted in accordance with the rules provided in GB/T 1.1-2020 Directives
for Standardization - Part 1.Rules for the Structure and Drafting of Standardizing Documents.
This is Part 2 of GB/T 5686.GB/T 5686 has issued the following parts.
---Part 1.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Manganese Content - Potentiometric Method,
Titrimetric Method after Ammonium Nitrate Oxidation and Titrimetric Method after
Perchloric Acid Oxidation;
---Part 2.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Silicon Content - Molybdenum Blue
Spectrophotometric Method, Silicon Potassium Fluoride Titrimetric Method and
Perchloric Acid Dehydration Gravimetric Method;
---Part 4.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Phosphorus Content - Molybdenum Blue
Photometric Method and Alkali Content Titrimetric Method;
---Part 5.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Carbon Content - The Infrared Absorption
Method, the Gasometric Method, the Gravimetric and the Coulometric Method;
---Part 7.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Sulfur Content - Infrared Absorption Method
and Combustion-neutralization Method.
This document serves as a replacement for GB/T 5686.2-2008 Ferromanganese,
Ferromanganese-silicon, Nitrogen-bearing Ferromanganese and Manganese Metal -
Determination of Silicon Content - Molybdenum Blue Photometric Method, Silicon Potassium
Fluoride Titrimetric Method and Perchloric Acid Dehydration Gravimetric Method. In
comparison with GB/T 5686.2-2008, apart from structural adjustments and editorial
modifications, the main technical changes are as follows.
a) The scope of application and determination range are modified (see Chapter 1;
Chapter 1 of Version 2008);
b) The test portion decomposition method of molybdenum blue spectrophotometric
method is modified (see 4.5.4.1; 3.5.3.1 of Version 2008);
c) The settling time of the silicon potassium fluoride titrimetric method is modified (see
5.5.4.2; 4.5.3.2 of Version 2008);
d) The test portion amount for the perchloric acid dehydration gravimetric method is
modified (see 6.5.2; 5.5.1 of Version 2008).
Please be noted that certain content of this document may involve patents. The institution
issuing this document does not undertake the responsibility of identifying these patents.
This document was proposed by China Iron and Steel Association.
This document shall be under the jurisdiction of National Technical Committee 318 on Pig Irons
and Ferroalloys of Standardization Administration of China (SAC/TC 318).
The drafting organizations of this document. Sichuan CHUANTOU EMEI Ferroalloy (Group)
Co., Ltd.; China Metallurgical Information and Standardization Institute.
The main drafters of this document. Fang Yan, Pu Haiyan, Gu Yan, Tang Huaying, Lu
Chunsheng, Zhang Chen.
The issuing of the previous versions.
---Firstly issued in 1985 as GB 5686.2-1985;
---During the first revision in 2008, the contents of GB/T 7730.2-2002 Ferromanganese
and Blast Furnace Ferromanganese - Determination of Silicon Content - Gravimetric
Method after Perchloric Acid Dehydration, GB 8654.3-1988 Methods for Chemical
Analysis of Manganese Metal - The Molybdenum Blue Photometric Method for the
Determination of Silicon Content, GB 8654.4-1988 Methods for Chemical Analysis of
Manganese Metal - The Perchloric Acid Dehydration Gravimetric Method for the
Determination of Silicon Content were incorporated (the issuing of the previous version
of GB/T 7730.2-2002 is as follows. GB 7730.2-1987 Methods for Chemical Analysis
of Ferromanganese and Blast Furnace Ferromanganese - The Perchloric Acid
Dehydration - Gravimetric Method for the Determination of Silicon Content);
---This is the second revision.
1 Scope
This document specifies the determination of silicon content in ferromanganese,
ferromanganese-silicon, micro-low carbon ferromanganese-silicon, nitrogen-bearing
ferromanganese and manganese metal, using molybdenum blue spectrophotometric method,
silicon potassium fluoride titrimetric method and perchloric acid dehydration gravimetric
method.
This document is applicable to the determination of silicon content in ferromanganese,
ferromanganese-silicon, micro-low carbon ferromanganese-silicon, nitrogen-bearing
ferromanganese and manganese metal. The determination range (mass fraction) is 0.10% ~
40.00%. Method 1.molybdenum blue spectrophotometric method, which is applicable to the
determination of silicon content in manganese metal, with a determination range (mass fraction)
of 0.10% ~ 2.00%; Method 2.silicon potassium fluoride titrimetric method, which is applicable
to the determination of silicon content in ferromanganese-silicon and micro-low carbon
ferromanganese-silicon, with a determination range (mass fraction) of 12.00% ~ 40.00%;
Method 3.perchloric acid dehydration gravimetric method, which is applicable to the
determination of silicon content in ferromanganese, ferromanganese-silicon, micro-low carbon
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal, with a
determination range (mass fraction) of 0.50% ~ 40.00%.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 4010 Ferroalloys Sampling and Preparation of Samples for Chemical Analysis
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 12805 Laboratory Glassware - Burettes
GB/T 12806 Laboratory Glassware - One-mark Volumetric Flasks
GB/T 12807 Laboratory Glassware - Graduated Pipettes
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Method 1.Molybdenum Blue Spectrophotometric Method
4.1 Principle
The test portion is dissolved with sodium peroxide-sodium carbonate and acidified with sulfuric
acid.
4.2 Reagents and Materials
Unless otherwise specified, only reagents that are confirmed to be analytically pure are used in
the analysis.
4.2.1 Water, GB/T 6682, Grade-3.
4.2.6 Sodium sulfite solution, 100 g/L. Weigh-take 100 g of anhydrous sodium sulfite, dissolve
it in water (see 4.2.1), then, use water (see 4.2.1) to dilute it to 1,000 mL.
4.2.7 Ammonium molybdate solution, 40 g/L. Weigh-take 40 g of ammonium molybdate
[(NH4)6Mo7O24 4H2O], place it in a 400 mL beaker, add 200 mL of water (see 4.2.1), warm
to dissolve it, filter it, then add 800 mL of water (see 4.2.1), and mix it well.
4.2.11 Iron solution, 4 mg/mL. Weigh-take 3.5 g of iron sulfate into a 500 mL beaker, add 200
mL of water (see 4.2.1) and heat to dissolve it. After the sample is completely dissolved, transfer
it to a 250 mL volumetric flask, use water (see 4.2.1) to dilute to the scale, and mix it well. 1
mL of this solution contains approximately 4 mg of iron.
4.3 Instruments
In the analysis, only common laboratory instruments are used. The one-mark volumetric flasks,
graduated pipettes and one-mark pipettes used shall respectively comply with the requirements
of GB/T 12806, GB/T 12807 and GB/T 12808.
4.4 Sampling and Sample Preparation
In accordance with the provisions of GB/T 4010, conduct sampling and sample preparation.
The specimens shall all pass the 0.125 mm sieve mesh.
4.5 Analytical Steps
4.5.4 Determination
4.5.4.1 Decomposition of test portion
Place the test portion (see 4.5.2) in a nickel crucible containing 3 g of sodium peroxide (see
4.2.3) and 1 g of anhydrous sodium carbonate (see 4.2.4), evenly stir it and place it in a high-
temperature furnace at 700 C to melt for 7 minutes ~ 8 minutes. Take it out and let it slightly
cool. Use hot water (see 4.2.1) to leach it into a 200 mL plastic beaker containing 80 mL of hot
water (see 4.2.1), clean the crucible and take it out. While using a plastic rod to stir it, slowly
add 35 mL of sulfuric acid (see 4.2.5), add 10 mL of sodium sulfite solution (see 4.2.6), stir it,
until the solution is clear. Transfer it into a 200 mL volumetric flask, use running water to cool
it to room temperature. Use water (see 4.2.1) to dilute it to the scale and mix it well.
4.6 Calculation of Analysis Results
In accordance with Formula (1), calculate the silicon content wSi in the specimen, expressed in
mass fraction (%).
5 Method 2.Silicon Potassium Fluoride Titrimetric Method
5.1 Principle
The test portion is decomposed with nitric acid and hydrofluoric acid, convert silicon into
fluorosilicic acid, add potassium fluoride and potassium nitrate to generate a precipitate of
potassium fluorosilicate. After filtering and washing, use alkali to neutralize the free acid
remaining on the filter paper and the precipitate.
5.2 Reagents and Materials
Unless otherwise specified, only reagents that are confirmed to be analytically pure are used in
the analysis.
5.2.1 Water, GB/T 6682, Grade-3.
5.2.2 Nitric acid, is approximately 1.42 g/mL.
5.2.3 Hydrofluoric acid, is approximately 1.15 g/mL.
5.2.7 Urea solution, 50 g/L.
5.2.8 Potassium nitrate solution, 50 g/L.
Intra-laboratory Allowable Difference (r) Inter-laboratory Allowable Difference (R) Silicon Content (mass fraction)
5.2.9 Potassium nitrate-ethanol solution, 40 g/L. Weigh-take 40 g of potassium nitrate and
dissolve it in 1,000 mL of ethanol solution (1 + 4).
5.2.10 Phenolphthalein indicator solution, 5 g/L, prepared with ethanol solution (1 + 1).
5.2.11 Sodium hydroxide standard titration solution, c (NaOH) = 0.18 mol/L. Weigh-take 7.2 g
5.3 Instruments
In the analysis, only common laboratory instruments are used. The burettes used shall comply
with the provisions of GB/T 12805.
5.4 Sampling and Sample Preparation
In accordance with the provisions of GB/T 4010, conduct sampling and sample preparation.
The specimens shall all pass the 0.125 mm sieve mesh.
5.5 Analytical Steps
5.6 Calculation of Analysis Results
In accordance with Formula (3), calculate the silicon content wSi in the specimen, expressed in
mass fraction (%).
6 Method 3.Perchloric Acid Dehydration Gravimetric Method
6.1 Principle
The test portion is dissolved with nitric acid, hydrochloric acid or sodium peroxide. Use
perchloric acid to evaporate and smoke to dehydrate silicic acid. After filtering and washing,
burn the precipitate at 1,100 C to a constant mass. Add hydrofluoric acid to volatilize and
eliminate the silicon as silicon tetrafluoride, then, burn it to a constant mass. Based on the mass
difference before and after hydrofluoric acid treatment, calculate the mass fraction of silicon.
6.2 Reagents and Materials
Unless otherwise specified, only reagents that are confirmed to be analytically pure are used in
the analysis.
6.2.9 Hydrochloric acid, 1 + 1.
6.2.10 Hydrochloric acid, 1 + 10.
6.2.11 Sulfuric acid, 1 + 3.
6.2.12 Ammonium thiocyanate solution, 50 g/L.
6.2.13 Silver nitrate solution, 10 g/L.
6.3 Instruments
In the analysis, only common laboratory instruments are used.
6.4 Sampling and Sample Preparation
In accordance with the provisions of GB/T 4010, conduct sampling and sample preparation.
The specimens shall all pass the 0.125 mm sieve mesh.
6.5 Analytical Steps
6.5.4 Determination
6.5.4.1 Decomposition of ferromanganese-silicon test portion
6.5.4.2.1 Place the test portion (see 6.5.2) in a 300 mL beaker, use a small amount of water (see
6.2.1) to moisten it, use a watch glass to cover it, and slowly add 20 mL of nitric acid (see 6.2.8)
and 5 mL ~ 10 mL of hydrochloric acid (see 6.2.4).
6.6 Calculation of Analysis Results
In accordance with Formula (4), calculate the silicon content wSi in the specimen, expressed in
mass fraction (%).
6.7 Allowable Difference
The difference in the analysis results shall be not greater than the allowable difference listed in
Table 5.Otherwise, the number of additional measurements and the analysis results shall be
determined as specified in Appendix A.
7 Test Report
The test report shall include the following content.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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