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GB/T 5686.7-2022 PDF English

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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
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GB/T 5686.7: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB/T 5686.7-2022English260 Add to Cart 0-9 seconds. Auto-delivery Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal - Determination of sulfur content - Infrared absorption method and combustion-neutralization method Valid
GB/T 5686.7-2008English150 Add to Cart 0-9 seconds. Auto-delivery Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal -- Determination of sulfur content -- Infrared absorption method and combustion-neutralization method Obsolete
GB/T 5686.7-1988English199 Add to Cart 2 days Methods for chemical analysis of silicomanganese alloy--The infrared absorption method for the determination of sulfur content Obsolete

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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



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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

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 & 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. 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. 4.3 Instruments and Equipment 4.3.1 High-frequency infrared carbon and sulfur analyzer or infrared absorption sulfur analyzer 4.3.2 Gas source 4.3.2.1 The carrier gas system includes an oxygen container, a two-stage pressure regulator and a timing control part that ensures appropriate pressure and rated flow. 4.3.2.2 The power gas source system includes power gas (see 4.2.8), a two-stage pressure 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 4.4 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. 4.5.3 Blank test Weigh-take 1.80 g of tungsten particles (see 4.2.5) and place them in a crucible (see 4.3.6) containing 0.30 g of tin particles (see 4.2.6) in advance and determine in accordance with 4.5.5. Repeat enough times, record the smallest, relatively stable and consistent 3 readings, calculate the average value and enter it into the instrument. When determining the specimens, the instrument will automatically deduct the blank value. 4.5.4 Analysis preparation 4.5.5 Calibration test 4.6 Expression of Analysis Results If the absolute value of the difference between two independent analysis results of the same specimen is not greater than the repeatability limit r, then, take the arithmetic mean as the analysis result. 4.7 Precision The precision data of this Part was determined by 10 laboratories conducting joint tests on the sulfur content in 8 different levels of ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal from November to December 2020.Each laboratory independently tested the sulfur content of each level 3 times (see Table B.1 in Appendix B for the original data of the precision test). In accordance with the statistical methods of GB/T 6379.1 and GB/T 6379.2, the precision determined is shown in Table 2.

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. 5.2.3 Silica gel, activated alumina or magnesium perchlorate. Silica gel, bead-shaped particles, no adhesion, consistent in color. Activated alumina has a particle size less than 80 mesh; it is firstly soaked in 1 mol/L hydrochloric acid for several hours, then, rinsed several times with clean water. Each time, the fine particles that have not settled within 10 seconds after shaking are discarded, then, set aside. Magnesium perchlorate, anhydrous, granular. 5.2.4 Soda lime or sodium hydroxide, granular. 5.2.10 Sodium hydroxide standard titration solution, cNaOH = 0.005 mol/L. Weigh-tale 0.2000 g of sodium hydroxide and dissolve it in 1,000 mL of water. Add 1 mL of newly prepared barium hydroxide saturated solution, mix it well; isolate the carbon dioxide and leave it for 2 days ~ 3 days. When using, take the upper part of settled solution. Adopt the following two methods to calibrate the sodium hydroxide standard titration solution. 5.3 Instruments and Equipment 5.3.1 Sulfur analyzer. Its device connection is shown in Figure 2. 5.3.2 Absorption bottle, see Figure 3. 5.4 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. 5.5 Analytical Procedures 5.5.1 Number of determinations For the same specimen, carry out at least 2 independent determinations. 5.5.4 Analysis preparation 5.5.4.2 Transfer-take 40 mL of the absorption solution (see 5.2.6) into the absorption bottle (see 16 in Figure 2), add 5 drops of mixed indicator (see 5.2.7). At a flow rate of 700 mL/min ~ 900 mL/min, introduce oxygen for about 5 minutes, so as to drive out the carbon dioxide in the solution. At this time, if the solution turns red purple, then, dropwise add the sodium hydroxide standard titration solution (see 5.2.10), until the solution turns bright green. 5.5.5 Determination 5.5.5.1 Place the test specimen (see 5.5.2) in the porcelain boat (see 5.3.4), push it into the 5.6 Allowable Differences The differences in the analysis results among laboratories shall not be greater than the allowable differences listed in Table 4 (see Table B.2 in Appendix B for raw test data).

6 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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