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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 Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 5686.2: Historical versions
Similar standardsGB/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 ContentsForeword... 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... 21ForewordThis 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 ScopeThis 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 ReferencesThe 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 Pipettes3 Terms and DefinitionsThis document does not have terms or definitions that need to be defined.4 Method 1.Molybdenum Blue Spectrophotometric Method4.1 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 Method5.1 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 Method6.1 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 ReportThe 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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