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GB/T 214-2007: Determination of total sulfur in coal 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 214: Historical versions
GB/T 214-2007: Determination of total sulfur in coal---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/GBT214-2007NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 75.160.10 D 21 Replacing GB/T 214-1996, GB/T 18856.8-2002 Determination of Total Sulfur in Coal (ISO 334.1992, Solid Mineral Fuels - Determination of Total Sulfur - Eschka Method, NEQ; ISO 351.1996, Solid Mineral Fuels – Determination of Total Sulfur – High Temperature Combustion Method, NEQ) Issued on. NOVEMBER 01, 2007 Implemented on. JUNE 01, 2008 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of PRC. Table of ContentsForeword... 3 1 Scope... 5 2 Normative References... 5 3 Eschka Method... 5 4 Coulometric Titration Method... 8 5 High Temperature Combustion Neutralization Method... 12 6 Test Report... 18ForewordThis Standard corresponds to the following international standards, the consistency is inequivalent. ISO 334.1992 Solid Mineral Fuels – Determination of Total Sulfur – Eschka Method; and ISO 351.1996 Solid Mineral Fuels – Determination of Total Sulfur – High Temperature Combustion Method. The major differences between this Standard and the internal standards are as follows. --- Add the coulometric titration; --- Modify the Eschka method as follows. The burnt material shall be treated by hot water rather than concentrated hydrochloric; Change maintaining for 30min in the boiling water after adding precipitant into taking heat preservation for 2h under the slightly boiling condition; Change the precision (repeatability limit of 0.05%; reproducibility critical difference of 0.1%) into expression by the sulfur content classification (3.6 of this Edition); --- Modify the high temperature combustion neutralization method as follows. Change the additive from Al2O3 to WO3; Change the combustion temperature from 1350°C to (1200±10) °C; Change the standard solution from Na2B4O7 to NaOH; Change the precision (repeatability limit of 0.05%; reproducibility critical difference of 0.1%) into expression by the sulfur content classification (5.6 of this Edition); This standard replaced GB/T 214-1996 Determination of Total Sulfur in Coal; and GB/T 18856.8-2002 Test Methods for Quality of Coal Water Mixture – Part 8.Determination of Total Sulfur in Coal Water Mixture. The major differences between this Standard and GB/T 214-1996 are as follows. --- Add the coke to the scope; --- Add the “Normative References”; --- Modify and supplement the Eschka method as follows. Modify and supplement the sampling quantity of the high-sulfur coal (NOTE in 2.4.1 of 1996 Edition; NOTE in 3.4.1 of this Edition); Modify the methyl orange indicator concentration; --- Modify and supplement the coulometric titration as follows. Modify the temperature range and length of the high-temperature constant temperature zone of the tubular high-temperature furnace (3.3.1 of 1996 Edition; 4.3.1 of this Edition); Correct the errors in the calculation formula for the results of the high temperature combustion neutralization method (molar mass value of sulfur; 4.5.1 of 1996 Edition; 5.5.1 of this Edition); Modify the precision of the method (3.6 of 1996 Edition; 5.6 of this Edition); Add the instrument calibration and calibration validity check (4.4.2 and 4.4.4 of this Edition); --- Modify and supplement the high temperature combustion neutralization method as follows. Modify the length of the high temperature constant temperature zone of the tubular high temperature furnace (4.3.1 of 1996 Edition; 5.3.1 of this Edition); Correct the errors in the calculation formula (molar mass value of sulfur; 4.5.1 of 1996; 5.5.1 of this Edition); Add the preparation and calibration of sodium carbonate purity reference material (5.2.11 of this Edition) and sulfuric acid standard solution (5.2.12 of this Edition). This Standard was proposed by China National Coal Association. This Standard shall be under the jurisdiction of National Technical Committee for Standardization of Coal. Drafting organization of this Standard. Coal Analysis Laboratory of China Coal Research Institute. Chief drafting staffs of this Standard. Pi Zhongyuan, Jia Yan, and Duan Yunlong. The historical editions replaced by this Standard are as follows. --- GB 214-1964, GB 214-1983, GB/T 214-1996; --- GB/T 18856.8-2002. Determination of Total Sulfur in Coal1 ScopeThis Standard specifies the method principle, reagents and materials, apparatus, test procedures, results calculation and precision, etc. of the Eschka method, coulometric titration, high temperature combustion neutralization method for the determination of sulfur in coal. For the arbitration analysis, the Eschka method shall be taken. This Standard is applicable to the lignite, bituminous coal, anthracite, and coke; it is also applicable to the dry coal samples of the water-coal-slurry.2 Normative ReferencesThe 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 212 Proximate Analysis of Coal (GB/T 212-2001, eqv ISO 11722.1999; eqv ISO 1171.1997; eqv ISO 562.1998) GB/T 483 General Rules for Analytical and Testing Methods of Coal3 Eschka Method3.1 Principle The coal sample was mixed with the Eschka reagent and burned. The sulfur in the coal was converted into sulfate; and then the sulfate ion generated the barium sulfate precipitate. The total sulfur content in the coal shall be calculated based on the mass of the barium sulfate. 3.2 Reagents and Materials 3.2.1 Eschka reagent (hereinafter referred to as Drinox). evenly mix the 2 pieces of the mass of chemically pure light magnesium oxide (GB/T 9857) and 1 piece of mass of chemically pure anhydrous sodium carbonate (GB/T 639); and grind them to the substance with the particle size of less than 0.2mm; then store in a sealed container. 3.2.2 Hydrochloric acid solution. (1+1), add 1 volume of water to the 1 volume of hydrochloric acid (GB/T 622); and mix them evenly. 3.3 Apparatus 3.3.1 Analytical balance. sensitivity of 0.1mg. 3.3.2 Muffle furnace. equipped with temperature control device; can heat up to 900°C; then the temperature can be adjusted and ventilate. 3.4 Test Procedures 3.4.1 Take (1.00±0.1) g1) (accurate to 0.0002g) of air-dried coal sample with a particle size of less than 0.2mm in a 30mL porcelain crucible; and take 2g (accurate to 0.1g) of Drinox (3.2.1); carefully mix them evenly; then use 1g (accurate to 0.1g) of Drinox to cover the coal sample.4 Coulometric Titration Method4.1 Principle The coal sample is burnt and decomposed in the air stream under the role of catalyst. The sulfur in the coal generates the sulfur oxides. Thereof, the sulfur dioxide is absorbed by the potassium iodide solution. Titrate by the iodine produced by the electrolysis of potassium iodide solution; the total sulfur content in the coal shall be based on the power consumed by the electrolysis. 4.2 Reagents and materials 4.3 Apparatus Coulomb sulfur analyzer. it mainly consists of the following parts. 4.3.1 Tubular high temperature furnace It can be heated to more than 1200°C and has a high temperature constant temperature zone (1150±10) °C about at least 70mm long. It has a platinum rhodium- platinum thermocouple temperature measurement and temperature control device. The furnace is equipped with a reducing combustion tube that can resist the temperature at 1300°C above. 4.3.2 Electrolytic cell and electromagnetic stirrer The electrolytic cell has a height of (120~180) mm, a capacity of no less than 400mL; 4.4 Test procedures 4.4.1 Test preparation 4.4.1.1 Raise the temperature of tubular high temperature furnace to 1150°C; use another set of platinum rhodium-platinum thermocouple pyrometer to determine the position ad length of high temperature zone, and the position at 500°C. 4.4.2 Instrument calibration 4.4.2.1 Calibration method. use a certified coal reference material to calibrate the sulfur analyzer according to one of the following methods. 4.4.2.1.1 Multi-point calibration method. use at least 3 certified coal reference materials with sulfur content that can cover the sulfur content range of the tested sample for calibration. 4.4.2.1.2 Single-point calibration method. use the reference material that has similar sulfur content with the test sample for calibration. 4.4.2.2 Calibration procedure 4.4.2.3 Verification of calibration validity Additionally select (1 ~ 2) coal reference materials or other control samples, and use the calibrated sulfur tester to determine their total sulfur contents according to the procedure 4.4.3.If the difference between the measured value and the standard value (control value) is within the uncertainty range (control limit) of the standard value (control value), the calibration is valid. Otherwise, the cause should be found and recalibrated. 4.4.3 Measurement procedures 4.4.4 Calibration inspection During the measurement of the instrument, coal reference materials or other control samples should be used regularly (after every 10 ~ 15 measurements are recommended) to verify the stability and validity of the sulfur analyzer. 4.6 Precision of method The repeatability and reproducibility for the determination of total sulfur by Coulometric titration method can refer to the provisions of Table 2.5 High Temperature Combustion Neutralization Method5.1 Principle The coal sample is burned in an oxygen stream under the action of a catalyst. The sulfur in the coal generates sulfur oxides, which are absorbed by the hydrogen peroxide solution to form sulfuric acid. Titrate with sodium hydroxide solution. Calculate the total sulfur content in coal according to the consumed sodium hydroxide standard solution. 5.2 Reagents and materials 5.2.1 Oxygen (GB/T 3863). 99.5%. 5.2.2 Alkali asbestos. chemically pure, granular. 5.2.3 Tungsten trioxide (HG10-1129). 5.2.11 Sodium carbonate purity reference material. GBW 06101, please refer to the reference material certificate for the usage method. 5.2.12 Sulfuric acid standard solution. c (1/2H2SO4) = 0.03mol/L. 5.3 Apparatus 5.3.1 Tubular high-temperature furnace. it can be heated to 1250°C and has a high temperature constant temperature zone about 80mm long at (1200±10) °C; equipped with a platinum rhodium-platinum thermocouple temperature measurement and temperature control device. 5.3.8 Acid burette. 25mL and 10mL. 5.3.9 Alkali burette. 25mL and 10mL. 5.3.10 Nichrome wire hook. made of Nichrome wire with a diameter of about 2mm; about 700mm long; bent at one end into a small hook. 5.4 Test procedures 5.4.1 Test preparation 5.4.1.1 Insert the combustion tube into the high-temperature furnace so that the end of the small-diameter tube extends out of the furnace mouth 100mm, and connect a section of silicone rubber tube with a length of about 30mm. 5.4.2 Measurement procedures 5.4.3 Blank measurement Put a thin layer of tungsten trioxide (without coal sample) in the combustion boat and measure the blank value according to the above procedures. 5.5 Result calculation 5.5.1 Calculation of total sulfur content in coal 5.6 Precision of method The repeatability and reproducibility for the total sulfur determination by high temperature combustion neutralization method can refer to provisions of Table 2.6 Test ReportThe test report shall contain at least the following information. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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