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GB/T 3558-2014: Determination of Chlorine 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 3558: Historical versions
GB/T 3558-2014: Determination of Chlorine 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/GBT3558-2014GB ICS 73.040 D 21 National Standard of the People's Republic of China Replacing GB/T 3558-1996 Determination of chlorine in coal (ISO 587.1997, Solid mineral fuels - Determination of chlorine using Eschka mixture, NEQ) Issued on. JUNE 09, 2014 Implemented on. OCTOBER 01, 2014 Issued by. General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) of the People's Republic of China; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1.Scope... 4 2.Normative references... 4 3.Method A. High temperature combustion hydrolysis - potentiometric titration... 4 4.Method B. Eschka mixture melt sample – potassium hydrogen sulfate titration... 12 5.Test report... 15 Annex A... 16ForewordThis Standard is drafted according to the rules given by GB/T 1.1-2009. This Standard replaces GB/T 3558-1996 Determination of chlorine in coal. Compared with GB/T 3558-1996, except the editorial modifications, the main changes are as follows. -- Change the preparation concentration (see 3.2.2, or 2.2.2 in 1996 version) and adding amount (see 3.4.2, or 2.4.2 in 1996 version) of the sulfuric acid solution; -- Change the concentration of the silver nitrate standard solution (see 3.2.6 or 2.2.9 in 1996 version); -- Add a potentiometric titration assembly, using the silver-silver chloride reference electrodes available on the market (see 3.3.2). Using re-drafting method, this Standard is compiled with reference to ISO 587.1997 Solid mineral fuels – Determination of chlorine using Eschka mixture. This Standard is not equivalent to ISO 587.1997. Determination of chlorine in coal 1.Scope This Standard specifies the summary of method, reagents and materials, apparatus, test procedure, calculation of results and precision for the determination of total chlorine content in coal using the high temperature combustion hydrolysis - potentiometric titration and Aldrin melt sample - potassium hydrogen sulfate titration. This Standard is applicable to brown, bituminous coal and anthracite. 2.Normative references The following documents are indispensable for the application of this Standard. For dated reference, the versions dated apply to this Standard. For undated references, the latest edition of the normative document (including all modifications) referred to applies. GB/T 483 General rules for analytical and testing methods of coal 3.Method A. High temperature combustion hydrolysis - potentiometric titration 3.1 Summary of method A coal sample is combusted and hydrolyzed in the mixed gas flow of oxygen and water vapor. All chlorines contained in the coal are converted to chlorides and dissolved in the water quantitatively. Titrate the concentration of chlorine ions in the condensate directly by silver nitrate potentiometric method. Use the silver as an indicator electrode and the silver- silver chloride as a reference electrode. Calculate the total chlorine content in the coal sample according to the consumed volume of silver nitrate standard solution. 3.2 Reagents and materials During analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or deionized water or water of equivalent purity. 3.3 Instruments and equipment 3.3.1 High temperature combustion hydrolysis device (Figure 1) 3.3.1.4 Water vapor generator. It is consisted of a 500 mL flat bottom flask and an adjustable electric disc furnace (0.5 kW, AC 0 V ~ 220 V, adjustable continuously). 3.3.1.5 Absorber. It is consisted of two 250 mL conical flasks, glass tubes and rubber stopper. 3.3.1.6 Oxygen flow meter. 1 000 mL/min at full scale, having the minimum division value of 10 mL/min. 3.3.2 Potentiometric titration assembly. as shown in Figure 4, using the self-made silver- silver chloride reference electrodes. The silver-silver chloride reference electrodes available on the market may also be used, and the potentiometric titration assembly is shown in Figure 5. 3.4 Combustion hydrolysis coal sample 3.4.1 Preparation of apparatus Assemble the apparatus as shown in Figure 1.Stuff a little of refractory wool into the gas outlet of combustion tube. Connect the electric circuit, gas circuit and condensate water. Add about 30 mL of distilled water to No.1 absorption flask, and about 20 mL to No.2 absorption flask. Raise the high temperature furnace to 1 100°C. Mark the 300°C, 600°C and 800°C zones of the combustion tube. Plug up the rubber stopper of sample injection rod. Regulate the flow rate of oxygen to 500 mL/min and the evaporation capacity of water vapor generator to about 2 mL/min. Check if there is gas leakage. 3.4.2 High temperature hydrolysis sample 3.5.2 Potentiometric calibration of end point 3.5.2.1 Preparation of blank solution. Same as 3.4.2, except that no coal sample is added. 3.5.2.2 Potentiometric calibration of titration end point. Place a beaker containing the blank solution on a titration set. Drip the silver nitrate standard solution that has a definite dripping quantity at a rate of 0.03 mL/s. Record the potential value at this point. Carry out the potential determinations twice as above. The difference between the measured values shall not exceed ±3 mV. 3.5.3 Titration for sample solution Place a beaker containing the sample solution on a titration set. Firstly, drip the silver nitrate standard solution at a rate of 0.05 mL/s; 3.6 Calculation of results The chlorine content of the coal is calculated according to Formula (1), and is recorded with the mean of two repeated determinations by rounding off to the third decimal places in according with GB/T 483. 3.7 Precision of this method The precision of this method for the determination of chlorine in coal is shown in Table 1. 4.Method B. Eschka mixture melt sample – potassium hydrogen sulfate titration 4.1 Summary of method Mix the coal sample and Eschka mixture. Melt them in a muffle furnace. Convert the chlorine to chlorides. 4.2 Reagents and materials During analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or deionized water or water of equivalent purity. 4.2.1 Eschka mixture. Weigh two portions of mass of magnesium oxide AND one portion of mass of anhydrous sodium carbonate. Grind to the granularity less than 0.2 mm. Mix well. Or, the Eschka mixture available on the market may be used. 4.2.2 Nitric acid. ρ20°C=1.40 g/mL. 4.2.3 Hexyl alcohol. chemically pure. 4.2.4 Saturated ammonium iron sulfate solution. add the ammonium iron sulfate to a certain amount of water till it does not dissolve anymore, and there is certain amount of solid ammonium iron sulfate in the solution. Add several milliliters of nitric acid to remove the brown colour. Take the supernatant liquid for use. 4.2.5 Silver nitrate solution. 10 g/L. Weigh out 1 g of the silver nitrate and dissolve in 100 mL of water, and add several milliliters of nitric acid. 4.2.6 Silver nitrate standard solution. c(AgNO3) = 0.025 00 mol/L. Weigh out accurately 4.247 2 g of reference reagent silver nitrate that has been pre-dried at 110°C for 1 h and cooled to room temperature in a drier. Dissolve in a little of water. Then transfer to a 1 000 mL brown measuring flask. Dilute to scale with water. 4.2.7 Potassium hydrogen sulfate standard solution 4.2.8 Sodium chloride standard solution. the concentration of chloride ion is 0.10 mg/mL. Weigh out accurately 0.329 8 g of reagent grade sodium chloride that has been pre-burned at 500°C ~ 600°C for 1 h and cooled to room temperature in a drier. Dissolve in a little of water. Then transfer to a 2 000 mL measuring flask. 4.2.10 Crucible. made of porcelain, having a 30 mL ~ 50 mL capacity. 4.2.11 Titration tube. 10 mL, grade A. 4.2.12 One-mark pipette. 50 mL and 10 mL, grade A. 4.3 Apparatus 4.3.1 Muffle furnace. having a thermocouple pyrometer and temperature control device, capable of being maintained at a temperature of 800°C, and with good circulation of air. 4.3.2 Electromagnetic stirrer. having a rotating speed of 500 r/min, adjustable continuously. 4.3.3 Analytical balance. sensitivity is 0.1 mg. 4.4 Procedure 4.4.1 Weigh (1 ± 0.1)g of the coal sample (accurate to 0.000 2 g) for general analytic test. Place in a crucible in where 3 g (to the nearest 0.1 g) of the Eschka mixture is contained. Mix thoroughly. Then, cover with a further 2 g of the Eschka mixture. Place the crucible in the muffle furnace. Keep the furnace door half-opened. Raise the temperature to (680 ± 20)°C. Maintain this temperature for 3 h. 4.4.5 Determination of blank value Determine each lot of coal samples. Carry out two or more blank determinations by using the same procedure as described in 4.4.1 ~ 4.4.4.Take the mean as the blank value (V4). 4.5 Calculation of results The chlorine content of the coal is calculated according to Formula (3) and is recorded with the mean of two repeated determinations by rounding off to the third decimal places in according with GB/T 483. 4.6 Precision of this method Same as 3.7. 5.Test report The test report shall include 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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