MT 158-1987 English PDFUS$439.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. MT 158-1987: Rock meal and floating dust ingredients used under coal mines Detection method Status: Obsolete
Basic dataStandard ID: MT 158-1987 (MT158-1987)Description (Translated English): Rock meal and floating dust ingredients used under coal mines Detection method Sector / Industry: Coal Industry Standard Classification of Chinese Standard: C70 Word Count Estimation: 11,10 Date of Issue: 9/30/1987 Date of Implementation: 11/1/1987 Regulation (derived from): Development-Reform-Office-Industry (2006) 97 Summary: This standard applies to coal mine dust measurement of rock powder materials and. In addition to free silica, other projects determination applies only to limestone. MT15:---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.Rock meal and floating dust ingredients used under coal mines Detection method Ministry of Coal Industry Standards MT/T 158-87 Rock dust and floating dust composition for underground coal mine test methods Published 1987-09-30 1987-11-01 implemented Published by the Ministry of Coal Industry of the People's Republic of China Contents1 Determination of free silica 1 2 Qualitative determination of arsenic 2 3 Determination of calcium oxide 3 4 Determination of phosphorus pentoxide 4 5 Determination of combustibles 5 Appendix A Method for Determination of Free Silica by Treating Precipitates with Hydrofluoric Acid (Supplementary) 8 A.1 Appliance 8 A.2 Reagent 8 A.3 Determination step 8 A.4 Calculation of results 8 Rock dust and floating dust composition for underground coal mine test methods This standard applies to the determination of rock powder raw materials and floating dust in coal mines. Except for free silica, the determination of other items is only applicable to stone Limestone.1 Determination of free silicaMain points of the method. At 240 ± 5 ℃, pyrophosphoric acid can dissolve silicates and metal oxides, but is insoluble to free silica. use After pyrophosphate treatment of rock samples, the mass of the obtained residue is the amount of free silica. 1.1 Instruments and equipment a. Analytical balance. Sensitivity 0.1mg; b.Box-shaped electric furnace. with a thermocouple pyrometer, which can heat up to 900 ℃, and can adjust the temperature and have good ventilation; c. Shake the heating device. 240 ± 5 ℃; d. Erlenmeyer flask. 50ml; e. Long neck funnel. 75mm in diameter; f. beaker. 250ml, 400ml; g.Dryer. Built-in color-changing silica gel or anhydrous calcium chloride; h. Porcelain crucible. 20 ~ 25ml. 1.2 Reagents a. Phosphoric acid (GB 1282-77). chemically pure, with a concentration of more than 85%; b. Hydrochloric acid (GB 622-77). analytical grade; c. Ammonium nitrate (GB 659-77). analytical grade; d. litmus test paper (or extensive test paper); e. Water. Distilled water. 1.3 Determination steps 1.3.1 Accurately weigh 0.1 to 0.2 g of the sample passing through a.200 mesh sieve (weighing to 0.0002 g) (for coal dust or dust containing coal dust, it should be Ashing at a temperature of 625 ± 25 ℃, weigh the gray sample), put it into a 50ml conical flask, add 15ml phosphoric acid and about 5mg ammonium nitrate, Place the conical flask on a shaking device to heat (if conditions are not available, artificial shaking can also be used. Use a 2 ° C thermometer with a graduation value of 0 ~ 300 ° C. During the arbitration, a shaking heating device shall be used) and maintained at 240 ± 5 ℃ for 10 minutes. 1.3.2 Remove the conical flask, cool to about 60 ° C, and slowly move the contents into a 250ml beaker containing 40ml of distilled water at about 80 ° C. Stir, mix thoroughly, and wash the Erlenmeyer flask several times with hot water or 0.1mol/L (original 0.1N) HC1, so that the final volume is 150 ~.200ml. 1.3.3 Filter with a slow quantitative filter paper and wash it with hot water until the filtrate is neutral (checked with litmus paper or extensive test paper) and free of chloride ions until. 1.3.4 Move the precipitate together with the filter paper into a porcelain crucible of known quality, first ash the filter paper at low temperature, and then at a temperature of 850 ± 10 ℃ After burning in a box-shaped electric furnace for 40 minutes, take out the crucible, cool it a little in the air, then put it in a desiccator to cool it to room temperature and weigh it. Ruo Shen When the precipitate is not white after burning, it can be treated by the method in Appendix A, and the loss after hydrofluoric acid treatment is used as the free silica. The amount. 1.3.5 For each batch of reagents, blank measurement should be performed without samples in accordance with 1.3 of this standard. White value. 1.4 Calculation of results The measurement result is calculated according to formula (1). 1.5 Allowance The difference measured in parallel in the same laboratory shall not exceed the following table.2 Qualitative determination of arsenicMethod points. After the sample is decomposed by heating with potassium chlorate and hydrochloric acid, pentavalent arsenic is reduced to trivalent, and zinc particles are added to cause arsenic to be analyzed in the form of arsenic It was absorbed in iodine solution, and finally developed in the form of arsenic molybdenum blue, and compared with the blank measurement results to determine the presence or absence of arsenic in the sample. 2.1 Instruments and equipment a. Analytical balance. Sensitivity 0.1mg; b. Spectrophotometer. wavelength range 360 ~ 800nm; c. colorimetric tube. 25ml; d. Erlenmeyer flask. 150ml; e. Arsenic generating device. (pictured). 1-conical flask; 2-rubber stopper; 3-glass tube; 4-latex tube; 5-glass capillary; 6-color tube Schematic diagram of arsenide generator MT/T 158-87 2.2 Reagents a. Hydrochloric acid (GB 622-77). analytically pure, density 1.19g/ml; b. Sulfuric acid (GB 625-77). analytical grade, concentration (H2SO4) 2.5mol/L (formerly 5N); c. Potassium chlorate (GB 645-77). analytical grade; d. Potassium iodide (GB 1272-77). analytically pure, 15% aqueous solution; e. Tartaric acid (GB 1294-77). analytically pure, 15% aqueous solution; f. stannous chloride (GB 638-78). analytical grade, 20% hydrochloric acid solution; Weigh 20 g of stannous chloride in 100 ml of hydrochloric acid. g. Iodine (GB 675-77). analytical grade; h. Sodium tetraborate (GB 632-78). analytical grade; i. Absorption solution. After dissolving 5g iodine and 10g potassium iodide with a small amount of water, add 5.7g sodium tetraborate and 12ml sulfuric acid, and dilute with water Release to 2L; j. Arsenic-free metal zinc (HGB 3073-59). analytically pure, granular, with a particle size of about 5mm; k. Potassium antimony tartrate. chemically pure, 0.55% aqueous solution; l. Ammonium molybdate (GB 657-79). analytically pure, 4% aqueous solution; m. Ascorbic acid. analytically pure, 3% aqueous solution (currently used now); n. Mixed developer. 50ml 2.5mol/L sulfuric acid solution (see 2.2b), add 30ml ascorbic acid solution (see 2.2m), 15ml Ammonium molybdate solution (see 2.21), 5ml potassium antimony tartrate solution (see 2.2k), and mix well (use the current preparation). 2.3 Determination steps 2.3.1 Weigh a sample of 0.5 g (weighed to 0.0002 g) that passed 160 mesh and dried at 105 ~ 110 ° C for 1 h in a 150 ml conical flask. Add 0.2 g of potassium chlorate and 10 ml of hydrochloric acid and shake well. Put it on a hot plate and heat for 1 ~ 2min, until there is no yellow gas in the bottle, and the solution is bubbling. Remove immediately. 2.3.2 After cooling, add 2ml of hydrochloric acid, 10ml of sulfuric acid and 25ml of distilled water, and then add 2ml of potassium iodide solution and tartaric acid solution 2 in that order. ml, stannous chloride solution 1ml (each reagent must be shaken). 2.3.3 After 15 minutes, add 4g zinc particles, and quickly connect the Erlenmeyer flask with the colorimetric tube containing 10ml absorption solution as shown in the figure. After 1 hour, remove the catheter, rinse the glass catheter with a small amount of water, add 4ml of mixed developer to the colorimetric tube, and immediately dilute to the mark with water and shake well. 2.3.4 After 2h, compare the color at 700nm with the blank solution developed according to the same measurement procedure above to determine the presence of arsenic in the sample.3 Determination of calcium oxideThe main points of the method. mask the iron, aluminum, titanium, manganese ions with triethanolamine, and use calcein thymolphthalein at a pH greater than 12.5. Mix indicator and titrate with EDTA standard solution. 3.1 Instruments and equipment a. Analytical balance. Sensitivity 0.1mg; b. Burette. 50ml. 3.2 Reagents a. Hydrochloric acid (GB 622-77). analytical grade, 11, 12 solution; b. Triethanolamine. analytically pure, 12 aqueous solution; c. Potassium chloride (GB 646-77). analytical grade; d. Calcium carbonate (HG3-1066-77). excellent grade pure; e. Disodium ethylenediamine tetraacetate (GB 1401-78). analytical grade; f. Potassium hydroxide (GB 2306-80). analytically pure, 30% aqueous solution, stored in polyethylene bottles; g. Calcein and thymolphthalein mixed indicator. Weigh 0.20g of calcein and 0.12g of thymolphthalein (HG3-961-76), and Grind and mix 4g of potassium chloride (see 3.2C) dried at 105 ~ 110 ℃ in advance, store it in a grind bottle, and store in a desiccator; h. Calcium oxide standard solution. equivalent to 1mg of calcium oxide per milliliter. Accurately weigh the superior grade pure carbon that has been dried for 1 hour at 130 ± 5 ℃ 1.7848g of calcium acid (see 3.2d) in a 400ml beaker, add about 100ml of water, cover the table, and slowly add 1ml 1ml of hydrochloric acid 10ml, until dissolved When complete, boil off the carbon dioxide, rinse the watch glass and cup wall with water, remove and cool, transfer to a 1000 ml volumetric flask, and add water to dilute Degrees, shake well. 1. EDTA standard solution. concentration (C10H14N2O3Na2 · 2H2O) 0.008mol/L (previously 0.008M). Weigh analytical pure EDTA (See 3.2e) 3.0g in a 250ml beaker, dissolved in water and diluted to 1000ml, shake well, the calibration method is as follows. Accurately pipette 10ml of calcium oxide standard solution into a 250ml beaker, dilute with water to about 100ml, and add triethanolamine aqueous solution 3ml, use potassium hydroxide solution to adjust the Congo red test paper to red and then excess 3 ~ 5ml, add a little calcein and thymolphthalein Agent (stir after each reagent). Place on a black base plate and titrate with EDTA standard solution until the green fluorescence disappears and it appears bright purple until. Do a blank test at the same time. The titer of EDTA standard solution to calcium oxide is calculated according to formula (2). 3.3 Determination steps 3.3.1 Weigh a sample of 0.5 g (weighed to 0.0002 g) that passed 160 meshes and dried at 105 to 110 ° C for 1 h in a 150 ml beaker. Wet a small amount of water, cover with a watch glass, and slowly add 25 ml of 12 hydrochloric acid. After the reaction stops, put it on a hot plate and boil for 15-20 minutes. After cooling down, transfer the solution and residue into a 100ml volumetric flask, dilute with water to the mark, and shake well. 3.3.2 Take 20ml of the clarified or dry-filtered analytical solution prepared above in a 250ml beaker, dilute with water to about 100ml, add three 3ml of ethanolamine, adjusted to Congo red test paper with potassium hydroxide solution, and an excess of 3 ~ 5ml, add a little calcein thymolphthalein Mix indicator (should mix well after adding each reagent). On a black base plate, titrate with EDTA standard solution until the green fluorescence completely disappears. Lost bright magenta as the end point. 3.4 Calculation of results and tolerances 3.4.1 The calcium oxide content is calculated according to formula (3). The calculation result is rounded to one decimal place, and rounded to the single digit according to the rounding rule. 3.4.2 The allowable difference between the results of parallel determination of calcium oxide in the same laboratory is 0.4%.4 Determination of phosphorus pentoxideThe main points of the method. decompose the sample with acid (or the preparation solution for measuring calcium oxide with 3.3.1), eliminate the interference of silicon with tartaric acid, and add the test solution Ammonium molybdate and ascorbic acid were used to form phosphoro-molybdenum blue for colorimetric determination. 4.1 Instruments and reagents a. Analytical balance. Sensitivity 0.1mg; b. Spectrophotometer. wavelength range 360 ~ 800nm; c. Tartaric acid (GB 1294-77). analytically pure, 20% aqueous solution; d. sulfuric acid (GB 625-77). analytical grade, 13 solution; e. Ascorbic acid. analytically pure, 2% aqueous solution (currently used now); f. Ammonium molybdate (GB 657-79). analytical grade; g. Potassium dihydrogen phosphate (GB 1274-77). excellent grade pure; h. Ammonium molybdate sulfate mixed solution. 4g ammonium molybdate is dissolved in 100ml sulfuric acid (see 4.1d); i. Phosphorus standard stock solution. Accurately weigh 0.4392g of potassium dihydrogen phosphate dried at 105 ~ 110 ℃ for 1h, dissolve in water and transfer to In a 1000ml volumetric flask, dilute to the mark and shake well. This solution contained 0.1 mg of phosphorus per milliliter. Phosphorus standard working solution. 0.01mg of phosphorus per milliliter. 4.2 Drawing of standard curve Pipette 0, 1.0, 2.0, 3.0, 4.0, 5.0 ml of phosphorus standard working solution into a 50 ml volumetric flask, add about 30 ml of water, and tartrate to dissolve 2ml of liquid, 5ml of ammonium molybdate sulfate mixed solution, rinse the bottle mouth with a small amount of water, and then add 5ml of ascorbic acid (each reagent should be shaken uniform). Place the volumetric flask in a boiling water bath and heat for 5 min, take it out to cool to room temperature, dilute with water to the mark, and shake well. Use reagent blank solution as Measure the absorbance at 680nm and draw a standard curve. 4.3 Determination steps Divide 20 ml of the preparation solution for measuring calcium oxide (see 3.3.1) into a 50 ml volumetric flask, and add 2 ml of tartaric acid.The following steps are the same as the standard The curve is drawn (see 4.2), and the blank of the sample is determined at the same time. After color development, the absorbance of the reagent blank solution was used as a reference to determine the absorbance. Find phosphorus content online. 4.4 Calculation of results and tolerances 4.4.1 The content of phosphorus pentoxide is calculated according to formula (4). The calculation results are rounded to three decimal places, and rounded to the next two decimal places according to the rounding rules. 4.4.2 The allowable difference of the results of the parallel determination of phosphorus pentoxide in the same laboratory is 0.003%.5 Determination of combustiblesThe amount of ignition loss in a sample minus the content of carbonate carbon dioxide in the sample is the content of combustibles in the sample. 5.1 Determination of loss on ignition The main points of the method. Weigh a certain amount of sample in a porcelain crucible and burn it at a certain temperature. The lost mass is the loss on ignition. 5.1.1 Instruments and equipment a. Analytical balance. Sensitivity 0.1mg; b. Silicon carbon rod high temperature electric furnace. with temperature control device, can maintain 1000 ± 20 ℃, and is accompanied by platinum rhodium platinum thermocouple and corresponding high temperature millivolt meter. 5.1.2 Determination procedure 5.1.2.1 Weigh 1g (weighed to 0.0002g) of a sample that has passed through 160 meshes and dried at 105 ~ 110 ° C for 1h in a constant weight ceramic crucible Medium, put it in a high-temperature electric furnace, slowly raise the temperature from low temperature to 1000 ± 20 ℃, and burn it at this temperature for 1 hour. Weigh quickly at room temperature. 5.1.2.2 Then check the burning for 30min, until the mass change is less than 0.001g. Use the one that loses mass after burning Calculate Loss on Ignition for one mass. 5.1.3 Calculation of results and tolerances 5.1.3.1 Loss on ignition is calculated according to formula (5). 5.1.3.2 The allowable difference between the results of parallel measurement of the loss on ignition in the same laboratory is 0.2%. 5.2 Determination of carbon dioxide This method is suitable for relatively pure limestone. If the total content of ferric oxide and alumina in the limestone is greater than 3%, this method should not be used. The method can be determined by GB 218-83 "Determination method of carbon dioxide content of carbonate in coal", and the mass of the sample is changed to 0.3 ~ 0.5g. The main points of the method. After the sample is dissolved with a certain amount of sulfuric acid standard solution, the excess acid, using methyl orange as an indicator, and sodium hydroxide standard solution Liquid titration to calculate the carbon dioxide content. 5.2.1 Instruments and reagents a. Analytical balance. Sensitivity 0.1mg; b. Sulfuric acid (GB 625-77). analytical grade, concentration (H2SO4) 0.1mol/L (formerly 0.2N); c. Potassium hydrogen phthalate (GB 1257-77). excellent grade pure; d. phenolphthalein (HGB 3039-59). 1% ethanol solution; e. methyl orange (HGB 3089-59). 0.2% aqueous solution; f. Sodium hydroxide (GB 629-81). analytically pure, concentrated (NaOH) 0.15mol/L (original 0.15N) aqueous solution; g. Water. Carbon dioxide-free distilled water. Calibration. Accurately weigh 0.5g potassium hydrogen phthalate dried at 105 ~ 110 ℃ for 1h (weigh to 0.0002g) in a 250ml conical flask , Dilute to 100ml with cold distilled water to remove carbon dioxide, add 10 drops of titanium phenoxide indicator, and titrate to light red with sodium hydroxide standard solution The color does not disappear after about 30s is the end point. The concentration of sodium hydroxide standard solution is calculated according to formula (6). 5.2.2 Determination procedure 5.2.2.1 Weigh 0.2g (weighed to 0.0002g) of 160 mesh sample dried at 105 ~ 110 ℃ for 1h in a 250ml conical flask Wet with a little water, then add 25ml of sulfuric acid standard solution accurately, and cover the conical flask with a porcelain crucible lid. Heated at 70 ~ 80 ℃ for half a minute Take off and cool in cold water. Rinse the porcelain crucible lid with a little water, add 2 ~ 3 drops of methyl orange indicator, and titrate with sodium hydroxide standard solution To yellow. 5.2.2.2 At the same time, take 25ml of sulfuric acid standard solution and measure its blank value according to the above method. 5.2.3 Calculation of results and tolerances 5.2.3.1 The carbon dioxide content is calculated according to formula (7). CO2 (%) = c × (V2-V1) × 0.0220 m × 100 (7) Where. c --- concentration of sodium hydroxide standard solution, mol/L; V1 --- Volume of sodium hydroxide standard solution consumed by the sample, ml; V2 --- 25ml volume of sodium hydroxide standard solution consumed by sulfuric acid standard solution, ml; 0.0440-millimolar mass of carbon dioxide (the mg-equivalent value of the original carbon dioxide is 0.0220), g/mmol; MT/T 158-87 m --- sample mass, g. The calculation result is rounded to one decimal place, and rounded to the single digit according to the rounding rule. 5.2.3.2 The allowable difference of the results of parallel measurement of carbon dioxide in the same laboratory is 0.5%. 5.3 Calculation of combustibles The combustibles are calculated according to formula (8). KRW (%) = Loss (%)-CO2 (%) (8) In the formula. KRW (%) --- the content of combustibles,%; Loss (%) --- Loss on ignition,%; CO2 (%) --- carbon dioxide content,%. MT/T 158-87Appendix AMethod for determining free silica by treating precipitate with hydrofluoric acid (Supplement) The main points of the method. the loss of impure silica after hydrofluoric acid treatment is the amount of pure free silica. A.1 Appliance a. Platinum crucible with lid. 25ml; b. Crucible forceps. platinum tip; c. 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