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GB/T 5686.7-2022 English PDF (GBT5686.7-2022)
GB/T 5686.7-2022 English PDF (GBT5686.7-2022)
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GB/T 5686.7-2022: Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal -- Determination of sulfur content -- Infrared absorption method and combustion-neutralization method
GB/T 5686.7-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
CCS H 11
Replacing GB/T 5686.7-2008
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of
Sulfur Content - Infrared Absorption Method and
Combustion-neutralization Method
ISSUED ON: DECEMBER 30, 2022
IMPLEMENTED ON: JULY 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 8
2 Normative References ... 8
3 Terms and Definitions ... 9
4 Method 1 - Infrared Absorption Method ... 9
5 Method 2 - Combustion-neutralization Method ... 14
6 Test Report ... 21
Appendix A (normative) Specimen Analysis Result Acceptance Procedure Flow Chart
... 22
Appendix B (informative) Additional Information on Joint Precision Test ... 23
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of
Sulfur Content - Infrared Absorption Method and
Combustion-neutralization Method
WARNING---the personnel using this document shall have practical experience in formal
laboratory work. This document does not point out all possible safety issues. It is the user’s
responsibility to take appropriate safety and health measures and ensure compliance with
the conditions stipulated in relevant national regulations.
1 Scope
This document describes the method of determining the sulfur content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal, using the
infrared absorption method and combustion-neutralization method.
This document is applicable to the determination of sulfur content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal. For Method
1, the determination range (mass fraction) is: 0.003% ~ 0.120%; for Method 2, the
determination range (mass fraction) is: 0.015% ~ 0.120%. Method 2 is not suitable for the
determination of sulfur content in nitrogen-bearing ferromanganese.
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 6379.1 Accuracy (trueness and precision) of Measurement Methods and Results - Part 1:
General Principles and Definitions
GB/T 6379.2 Accuracy (trueness and precision) of Measurement Methods and Results - Part 2:
Basic Method for the Determination of Repeatability and Reproducibility of a Standard
Measurement Method
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 8170 Rules of Rounding off for Numerical Values and Expression and Judgement of
Limiting Values
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Method 1 - Infrared Absorption Method
4.1 Principle
The test portion is burned in a high-frequency induction furnace with oxygen flow, and the
sulfur is oxidized into sulfur dioxide, which is carried to the infrared absorption cell with the
oxygen flow. The infrared detector measures its absorption of infrared rays of a specific
wavelength. The absorption value is proportional to the flowing sulfur dioxide, and the sulfur
content can be determined in accordance with the changes in energy received by the detector.
4.2 Reagents and Materials
4.2.1 Acetone, the residue after evaporation contains less than 0.0005% sulfur.
4.2.2 Magnesium perchlorate, anhydrous, granular.
4.2.3 Caustic soda asbestos, granular.
4.2.4 Glass wool.
4.2.5 Tungsten particles, with sulfur content less than 0.0005% and a particle size 0.8 mm ~ 1.4
mm.
4.2.6 Tin particles, with sulfur content less than 0.0005% and a particle size 0.4 mm ~ 0.8 mm.
If necessary, acetone (see 4.2.1) shall be used to clean the surface.
4.2.7 Oxygen, with a purity greater than 99.95%. Other grades of oxygen may also be used if a
low and consistent blank can be obtained.
4.2.8 Power gas source, nitrogen, argon or compressed air, with impurity (water and oil) content
less than 0.5%.
4.3 Instruments and Equipment
4.3.1 High-frequency infrared carbon and sulfur analyzer or infrared absorption sulfur
analyzer
4.3.1.1 High-frequency infrared carbon and sulfur analyzer or infrared absorption sulfur
analyzer (with a sensitivity of 0.0001%). The device connection is shown in Figure 1.
4.3.1.2 Gas cleaning bottle, filled with caustic soda asbestos (see 4.2.3).
regulator and a timing control part that ensures appropriate pressure and rated flow.
4.3.3 High-frequency induction furnace
It shall satisfy the requirements for the melting temperature of the test portion.
4.3.4 Control System
4.3.4.1 The microprocessor system includes a central processing unit, memory, keyboard input
device, information center display screen, analysis result display screen and analysis result
printer, etc.
4.3.4.2 The control functions include automatic loading and unloading of crucibles and furnace
table lifting, automatic cleaning, analysis condition selection and setting, analysis process
monitoring and alarm interruption, analysis data collection, calculation, correction and
processing, etc.
4.3.5 Measurement system
It is mainly composed of an electronic balance (with a sensitivity not greater than 0.001 g)
controlled by a microprocessor, an infrared analyzer and electronic measuring elements.
4.3.6 Ceramic crucible
The size of the ceramic crucible is 23 mm 23 mm or 25 mm 25 mm. It is burned in a
high-temperature heating furnace above 1,200 C for 4 hours or burned with oxygen, until the
blank value is the lowest.
4.4 Sampling and Specimen Preparation
In accordance with the stipulations of GB/T 4010, take and prepare specimens. The
ferromanganese-silicon specimens shall pass a 0.125 mm sieve, the ferromanganese and
nitrogen-bearing ferromanganese specimens shall pass a 0.149 mm sieve, and the manganese
metal specimens shall pass a 0.177 mm sieve.
4.5 Analytical Procedures
4.5.1 Number of determinations
For the same specimen, carry out at least 2 independent determinations.
4.5.2 Amount of test portion
The amount of test portion is weighed in accordance with Table 1 and the category of the
specimen to be tested, accurate to 0.001 g.
Table 1 -- Amount of Test Portion
Category Amount of Test Portion
Under the reproducibility conditions, two different operators from different laboratories use the
routine and correct operation of this method to conduct two independent determinations on the
same specimen, the absolute difference shall not be greater than the reproducibility limit R, and
the situation of exceeding the reproducibility limit R shall not exceed 5%.
5 Method 2 - Combustion-neutralization Method
5.1 Principle
The test portion is burned with oxygen at high temperature to oxidize all the sulfur into sulfur
dioxide, which is absorbed into the hydrogen peroxide solution and turned into sulfuric acid,
which is titrated with sodium hydroxide standard solution. Calculate the sulfur content.
5.2 Rea...
Get QUOTATION in 1-minute: Click GB/T 5686.7-2022
Historical versions: GB/T 5686.7-2022
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GB/T 5686.7-2022: Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal -- Determination of sulfur content -- Infrared absorption method and combustion-neutralization method
GB/T 5686.7-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
CCS H 11
Replacing GB/T 5686.7-2008
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of
Sulfur Content - Infrared Absorption Method and
Combustion-neutralization Method
ISSUED ON: DECEMBER 30, 2022
IMPLEMENTED ON: JULY 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 8
2 Normative References ... 8
3 Terms and Definitions ... 9
4 Method 1 - Infrared Absorption Method ... 9
5 Method 2 - Combustion-neutralization Method ... 14
6 Test Report ... 21
Appendix A (normative) Specimen Analysis Result Acceptance Procedure Flow Chart
... 22
Appendix B (informative) Additional Information on Joint Precision Test ... 23
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of
Sulfur Content - Infrared Absorption Method and
Combustion-neutralization Method
WARNING---the personnel using this document shall have practical experience in formal
laboratory work. This document does not point out all possible safety issues. It is the user’s
responsibility to take appropriate safety and health measures and ensure compliance with
the conditions stipulated in relevant national regulations.
1 Scope
This document describes the method of determining the sulfur content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal, using the
infrared absorption method and combustion-neutralization method.
This document is applicable to the determination of sulfur content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal. For Method
1, the determination range (mass fraction) is: 0.003% ~ 0.120%; for Method 2, the
determination range (mass fraction) is: 0.015% ~ 0.120%. Method 2 is not suitable for the
determination of sulfur content in nitrogen-bearing ferromanganese.
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 6379.1 Accuracy (trueness and precision) of Measurement Methods and Results - Part 1:
General Principles and Definitions
GB/T 6379.2 Accuracy (trueness and precision) of Measurement Methods and Results - Part 2:
Basic Method for the Determination of Repeatability and Reproducibility of a Standard
Measurement Method
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 8170 Rules of Rounding off for Numerical Values and Expression and Judgement of
Limiting Values
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Method 1 - Infrared Absorption Method
4.1 Principle
The test portion is burned in a high-frequency induction furnace with oxygen flow, and the
sulfur is oxidized into sulfur dioxide, which is carried to the infrared absorption cell with the
oxygen flow. The infrared detector measures its absorption of infrared rays of a specific
wavelength. The absorption value is proportional to the flowing sulfur dioxide, and the sulfur
content can be determined in accordance with the changes in energy received by the detector.
4.2 Reagents and Materials
4.2.1 Acetone, the residue after evaporation contains less than 0.0005% sulfur.
4.2.2 Magnesium perchlorate, anhydrous, granular.
4.2.3 Caustic soda asbestos, granular.
4.2.4 Glass wool.
4.2.5 Tungsten particles, with sulfur content less than 0.0005% and a particle size 0.8 mm ~ 1.4
mm.
4.2.6 Tin particles, with sulfur content less than 0.0005% and a particle size 0.4 mm ~ 0.8 mm.
If necessary, acetone (see 4.2.1) shall be used to clean the surface.
4.2.7 Oxygen, with a purity greater than 99.95%. Other grades of oxygen may also be used if a
low and consistent blank can be obtained.
4.2.8 Power gas source, nitrogen, argon or compressed air, with impurity (water and oil) content
less than 0.5%.
4.3 Instruments and Equipment
4.3.1 High-frequency infrared carbon and sulfur analyzer or infrared absorption sulfur
analyzer
4.3.1.1 High-frequency infrared carbon and sulfur analyzer or infrared absorption sulfur
analyzer (with a sensitivity of 0.0001%). The device connection is shown in Figure 1.
4.3.1.2 Gas cleaning bottle, filled with caustic soda asbestos (see 4.2.3).
regulator and a timing control part that ensures appropriate pressure and rated flow.
4.3.3 High-frequency induction furnace
It shall satisfy the requirements for the melting temperature of the test portion.
4.3.4 Control System
4.3.4.1 The microprocessor system includes a central processing unit, memory, keyboard input
device, information center display screen, analysis result display screen and analysis result
printer, etc.
4.3.4.2 The control functions include automatic loading and unloading of crucibles and furnace
table lifting, automatic cleaning, analysis condition selection and setting, analysis process
monitoring and alarm interruption, analysis data collection, calculation, correction and
processing, etc.
4.3.5 Measurement system
It is mainly composed of an electronic balance (with a sensitivity not greater than 0.001 g)
controlled by a microprocessor, an infrared analyzer and electronic measuring elements.
4.3.6 Ceramic crucible
The size of the ceramic crucible is 23 mm 23 mm or 25 mm 25 mm. It is burned in a
high-temperature heating furnace above 1,200 C for 4 hours or burned with oxygen, until the
blank value is the lowest.
4.4 Sampling and Specimen Preparation
In accordance with the stipulations of GB/T 4010, take and prepare specimens. The
ferromanganese-silicon specimens shall pass a 0.125 mm sieve, the ferromanganese and
nitrogen-bearing ferromanganese specimens shall pass a 0.149 mm sieve, and the manganese
metal specimens shall pass a 0.177 mm sieve.
4.5 Analytical Procedures
4.5.1 Number of determinations
For the same specimen, carry out at least 2 independent determinations.
4.5.2 Amount of test portion
The amount of test portion is weighed in accordance with Table 1 and the category of the
specimen to be tested, accurate to 0.001 g.
Table 1 -- Amount of Test Portion
Category Amount of Test Portion
Under the reproducibility conditions, two different operators from different laboratories use the
routine and correct operation of this method to conduct two independent determinations on the
same specimen, the absolute difference shall not be greater than the reproducibility limit R, and
the situation of exceeding the reproducibility limit R shall not exceed 5%.
5 Method 2 - Combustion-neutralization Method
5.1 Principle
The test portion is burned with oxygen at high temperature to oxidize all the sulfur into sulfur
dioxide, which is absorbed into the hydrogen peroxide solution and turned into sulfuric acid,
which is titrated with sodium hydroxide standard solution. Calculate the sulfur content.
5.2 Rea...
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