MT 137.1-1986 English PDF

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MT 137.1-1986: Harmful gas existing in mine air Detection method of carbon monoxide
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Basic data

Standard ID: MT 137.1-1986 (MT137.1-1986)
Description (Translated English): Harmful gas existing in mine air Detection method of carbon monoxide
Sector / Industry: Coal Industry Standard
Classification of Chinese Standard: N56
Word Count Estimation: 9,959
Date of Issue: 3/5/1986
Date of Implementation: 4/1/1986
Summary: This standard applies to coal mine air (or gas) concentration of carbon monoxide was measured.

MT13:

---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.
Harmful gas existing in mine air Detection method of carbon monoxide Ministry of Coal Industry Standards MT/T 137.1-1986 Method for determination of harmful gas carbon monoxide in mine air Published 1986-03-05 1986-04-01 implementation Published by the Ministry of Coal Industry of the People's Republic of China

Contents

1 General requirements 1 2 Determination method 1 Method for determination of harmful gas carbon monoxide in mine air This standard applies to the determination of carbon monoxide concentration in the air (or gas) in coal mines.

1 General requirements

1.1 Carbon monoxide concentration is expressed in ppm (volume/volume). 1ppm = 0.0001%. 1.2 Calibration gas 1.2.1 Prepared by static gas distribution method. The preparation method is performed according to Appendix A of MT 67-82 "Longer Carbon Monoxide Calibration Tube". 1.2.2 Order a carbon monoxide standard gas sample according to the measurement range. 1.3 When the measurement results are in dispute, a carbon monoxide standard gas sample is used for arbitration. 1.4 When collecting gas samples with a bladder, it should not exceed 12 hours from the sampling to the completion of the measurement. The sampling volume is 3000 ~ 6000 ml. 1.5 Measured by the calibration tube method, when the carbon monoxide concentration exceeds the relevant provisions of the Coal Mine Safety Regulations or the carbon monoxide cannot be measured by the calibration tube method At that time, the gas sample shall be taken to the ground laboratory for measurement by the method specified in Article 2.2 or 2.3 of this standard. 1.6 When using the mercury replacement method (mercury oxide-selenium test paper method), when the selenium test paper is left for a long time or the instrument used and the selenium test paper are used for calibration The type of the device is different, and the selenium test paper needs to be re-calibrated with the calibration gas before being used. 1.7 Using gas chromatography, in order to ensure the accuracy of the measurement results, repeated injections are not allowed (that is, the chromatographic peak of the previous gas sample cannot be Take the next gas sample). When using a calibration curve for quantification, the accuracy of the calibration curve should always be checked with a calibration gas.

2 Measurement method

2.1 Specific length test tube method 2.1.1 Principle of the method. The gas sample passes through a glass tube equipped with an indicator gel for adsorbing diiodine pentoxide, and carbon monoxide is reacted with diiodine pentoxide to form The tan (or green-brown) discoloration layer of free iodine, the height of the discoloration layer represents the concentration of carbon monoxide. 2.1.2 Appliance 2.1.2.1 Calibration tube. The calibration tube shall meet the relevant regulations of MT 67-82. According to the range of measuring carbon monoxide concentration, the calibration tube is generally divided into Three models (see Table 1). Table 1 Types of calibration tubes The calibration tube is used under the environment temperature of 15 ~ 35 ℃, atmospheric pressure of 700 ~ 800 mmHg, and the interference gas can be removed. Before using the calibration tube, check its quality with a calibration gas and find that it does not meet the relevant regulations of MT 67-82. 2.1.2.2 Calibrator. There are four kinds of calibrators used in conjunction with the calibration tube (see Figure 1), which can be selected according to specific conditions. Phase of calibrator volume The deviation must not exceed ± 5% of the nominal volume. 2.1.3 Preparation before measurement Figure 1 Schematic diagram of the calibrator 2.1.3.1 Airtightness check of the calibrator. Insert the unopened calibration tube into the calibrator's exhaust gas (or (Intake) port to check the airtightness of the calibrator, if it is found that air leakage is not allowed to use. 2.1.3.2 Appearance inspection of the verification tube. When using, check whether the pipe tip of the verification tube is broken; whether the medicine is loose, mixed or discolored; Whether it is clear and whether the zero mark line coincides with the interface between the indicator glue and the insulation layer. 2.1.4 Measurement steps. The measurement steps should be carried out in strict accordance with the instruction manual, and two test tubes should be used for each measurement. 2.1.5 Processing of measurement results 2.1.5.1 When the allowable difference between the measured values of the two verification tubes meets the requirements of Table 2 of this standard, the arithmetic average value shall be taken as the measurement result. If not In accordance with the provisions of Table 2, the third measurement shall be performed, and the arithmetic mean of the two measured values within the tolerance shall be taken. Table 2 Allowable difference of test tube test value 2.1.5.2 Choosing the average The type 1 test tube is calculated to one decimal place, and the whole number is reported after rounding off according to the number rounding rules. The type 2 verification tube is calculated to the single digit, and the ten-digit number is reported after the contract is rounded according to the digital rounding rule. The type 3 verification tube is calculated to the ten digits, and the hundred digits are reported after the contract is rounded according to the digital rounding rules. 2.2 Mercury replacement method (mercury oxide-selenium test paper method) 2.2.1 Principle of the method. At a certain temperature, carbon monoxide reacts with mercury oxide to generate mercury vapor, which then reacts with selenium on the selenium test strip to produce Hg selenide was formed, and the length of the black scar was measured to calculate the carbon monoxide concentration in the gas sample. The measuring range of this method is 0 ~ 100ppm, and the sensitivity is 2ppm. 2.2.2 Instrumentation 2.2.2.1 Fixed measuring device (Figure 2). Gas sample measuring tube 1 is an eight-ball measuring tube with a water jacket, with a volume of 50 ± 1 ml per ball, a four-way piston A with a 90 ° passage at the upper end of the measuring tube, and a lower end of the measuring tube. There is a three-way pipe, the upper branch of the pipe has a two-way piston B, the upper pipe is connected to the measuring tube, and the right branch pipe has a two-way piston C, which is connected to a water source for conveying gas samples. The level bottle 2 has a volume of 450 ~ 500 ml. The gas drying tube 4 contains anhydrous calcium chloride. The gas drying tube 5 contains magnesium perchlorate. The activated carbon tube 6 contains granular activated carbon. The dimensions of the U-shaped reaction tube are shown in Figure 2. Mercury oxide is placed on the left tube and selenium test paper is placed on the right tube. Mercury thermometers 8 and 9 range from 0 to 360 ° C. Tubular heating furnaces 10 and 11 have an inner diameter of 30 mm and a height of 130 mm, and the center distance between the two furnaces is 60 mm. Hot wire, two furnaces each have a transformer to control the furnace temperature. Insulation box 12 has a volume of 250 × 180 × 180 mm and contains asbestos ash (or ceramic wool) insulation material inside. 2.2.2.2 Portable measuring device (Figure 3). 1-Power switch; 2-Terminal; 3-Fuse; 4-Temperature regulator; 5-Float flowmeter; 6-air inlet; 7-needle flow regulating valve; 8-U-shaped reaction tube; 9-metal three-way valve Figure 3 Portable measuring device The adjustment range of the temperature regulator 4 is 0 ~ 300 ° C, and the accuracy is 2.5. The range of the float flowmeter 5 is 0 ~ 50ml/min. 0 ~ 500 ml/min. 2.2.3 Reagents and materials 2.2.3.1 Reagents a. Anhydrous calcium chloride. chemically pure, granular; b. Magnesium perchlorate. chemically pure, granular; c. Activated carbon. industrial, granular; d. Mercury oxide. chemically pure, granular, orange-red in color, rich in pores, and no metallic mercury luster; e. Discoloration silica gel. industrial, granular. 2.2.3.2 Materials a. Selenium test paper. There are two types of selenium test paper for activation and measurement, the paper strip is 140 mm long and 3 mm wide; b. Latex tube. 5 ~ 7 mm inner diameter. 2.2.4 Air tightness check. After the measuring device is assembled, the gas outlet of the system is blocked. If the flowmeter returns to zero, it means that the air tightness is good. Otherwise it should Segmented processing. 2.2.5 Measurement operation 2.2.5.1 Operation of the stationary measuring device a. Mercury oxide activation and blank measurement. The temperature of the incubator in Figure 2 was raised, and a concentrated selenium test paper for activation was inserted into the paper tube. The degree is 180 mm from the end of the tube, and then the clean air is started to enter the U-shaped reaction tube through the tubes c and d, and the air velocity is controlled to be about 250 millimeters. Liters/minute. A transformer was used to maintain the temperature of the mercury oxide tube at 250 ± 1 ° C and the temperature of the test paper tube at 140 ± 2 ° C. Continue to clean air, selenium test strip When the black marks will reach the top, replace with new paper. When black marks are formed very slowly it is a sign that activation is about to be completed. Then cool the mercury oxide tube furnace, Maintain the temperature of the mercury oxide tube at 180 ± 1 ℃, change the net air flow rate to 10 ± 0.5 ml/min, and remove the concentrated selenium test paper for activation. Insert the selenium test strip (the insertion depth is 180 mm from the end of the tube) and continue aeration for 5 minutes. There are no black marks on the bars, indicating that activation has been completed. Newly installed mercury oxide can be activated normally within 4 ~ 6 hours.In the future, it will be activated for 1 hour according to the above method before the start of daily measurement. After the white pass, the measurement can be performed. When not measured, mercury oxide should be activated once a week. When used for a long time, it must be activated the day before. b. Gas sample measurement. After the mercury oxide is activated, maintain the temperature of the mercury oxide tube at 180 ± 1 ℃ and the temperature of the paper tube at 140 ± 2 ℃. Measuring When taking a gas sample, first flush the instrument with the gas sample. Inhale the gas sample into the measuring tube 1 from the branch tube a of the piston A, and use 350 ~ 400 ml of gas sample. Pass the tube d through the instrument to eliminate the remaining previous gas sample, and then inhale the gas sample for formal determination. When measuring, first insert a measuring selenium into the test paper tube Test strip, after passing 50 ml of gas sample through the mercury oxide reaction tube at a flow rate of 10 ± 0.5 ml/min, close C, stop the air flow, and remove the reaction Insert another selenium test strip into the completed paper strip, and then continue the measurement. There are 3 general gas samples and 6 important gas samples. Measure every The length of the black mark on a piece of paper is taken as its arithmetic mean. After the last measurement of each day, power off and cool down, pass the instrument with clean air of 40-50ml/min, remove the mercury vapor in the tube, and After the temperature of the mercury oxide tube dropped to 100 ° C, the air flow was stopped and the test paper tube was closed. 2.2.5.2 Operation of the portable measuring device a. Mercury oxide activation and blank measurement. insert a U-shaped reaction tube containing mercury oxide into the heating device, and then place the heating device in Insulated container. The inlet end of the U-shaped reaction tube is connected to the flow meter and needle valve through a metal three-way valve. The flow rate of each minute is passed into clean air or pure oxygen. Insert a concentrated selenium test strip at the outlet of the U-shaped tube and adjust the temperature regulator to make the temperature indicator 250 ℃, turn on the power and start heating. After reaching the given temperature in 2 to 3 minutes, stop heating and maintain it at the given temperature. Every few days Change the test strip once every minute, and the interval between subsequent strip changes will be lengthened. After a certain period of time, the inserted test strips are light gray and stable. The timing indicates that the activation of mercury oxide has been completed. Then adjust the temperature to 180 ° C. After 15-20 minutes, the temperature can be blanked after the temperature is constant. Determination. When measuring, first turn the three-way valve so that the inlet end of the U-shaped reaction tube is in communication with the flowmeter for measurement. Adjust the needle valve so that A flow rate of ± 1.0 ml/min entered the mercury oxide tube. After adjusting the flow rate, close the three-way valve, remove the concentrated selenium test strip, and insert a selenium test Paper strip (the lower end of the paper strip is 10 mm from the mercury oxide), turn the three-way valve, and immediately start the stopwatch, wait for 2.5 minutes to ventilate 50 ± 2.5 ml, and close Three-way valve, remove the paper strip and insert another selenium test strip to continue the measurement. Measure 3 strips in succession. When the test strip has no black marks, it is blank and qualified. Otherwise, it needs to be reactivated. b. Gas sample measurement. Gas sample measurement is the same as blank measurement. Connect the air inlet to the gas sample to be measured, and insert a concentrated selenium at the outlet of the U-shaped tube Test strip, adjust the needle valve, let the gas sample flow into the gas sample at a flow rate of 80 to 100 mm/min for 5 to 8 minutes, and exclude the previous gas remaining in the gas path. body. Then, measure 3 (or 6) strips according to the blank measurement method, measure the length of the black mark, and take the arithmetic average value. Turn off the power after the gas sample is measured, and pass in clean air for 15-20 minutes at a flow rate of about 100 ml/min. Close the gas path and put the instrument in place. 2.2.5.3 Measurement of black mark length After the reaction between carbon monoxide and mercury oxide, the shape of the black mark on the test strip is roughly as follows (Figure 4). Figure 4 Schematic diagram of black marks When measuring the length of the mark, place the test strip on a measuring ruler and carefully observe the orthogonal distinction between the black and light colors of the black mark on the test strip, except for the a shape. In addition, other shapes can be estimated so that the area of the protruding black marks is sufficient to compensate the area of the notch, and is reduced to orthogonality to determine the orthogonal distinguishing line. Orthogonal division line The length of the light-colored tail line can be halved to add the length of the black mark when measuring. The black marks on the front and back of the selenium paper strip need to be measured. 2.2.6 result processing 2.2.6.1 Black mark measurement reads 0.5 mm. The average is rounded to one decimal place. 2.2.6.2 Substitute the measured average black mark length into the test paper calibration formula to calculate the carbon monoxide concentration in the gas sample. Calculated value is smaller After the number is rounded up, the number is rounded up according to the number rounding rules. Note. The test strip calibration formula is given by the manufacturer. 2.3 Gas chromatography 2.3.1 Principle of the method. After the gas sample is separated by a chromatographic column in a hydrogen stream, it enters a conversion furnace filled with a nickel catalyst, and carbon monoxide reacts with hydrogen. It should be converted into methane and measured with a hydrogen flame ionization detector. The measuring range of this method is 0 ~ 100ppm and 0 ~ 1000ppm, the sensitivity is 0.5ppm and 5ppm. 2.3.2 Device. a gas chromatograph with a hydrogen flame ionization detector and a carbon monoxide conversion furnace. The measurement process is shown in Figure 5. Figure 5 Schematic diagram of the chromatographic determination process MT/T 137.1-1986 2.3.3 Determination of reference conditions Chromatographic column. a stainless steel tube with an inner diameter of 3 mm and a length of 1.0 m, containing 60 to 80 mesh TDX-01 (carbon molecular sieve), and a column temperature of 50 ° C; Detection room temperature. 120 ° C; Conversion column. U-shaped stainless steel tube with an inner diameter of 3 mm and a length of 250 mm, with a nickel catalyst inside, and a column temperature of 360 ° C; Pre-column pressure. 1.9 kg/cm2; Carrier gas hydrogen flow. 42 ml/min; Assist gas flow. 600 ml/min; Auxiliary gas and nitrogen flow. 34 ml/min; Injection volume. 1 ml; Recording paper speed. 300 mm/hour. 2.3.4 Measurement operation a. When the instrument is stable, connect the calibration gas sample to the six-way valve of the process system (Figure 5), use a 1 ml quantitative tube, and flush the calibration gas sample. After washing the sample gas path, turn the six-way valve to make the calibration gas sample enter the chromatographic column and the conversion column, and measure the chromatographic peak height (3 consecutive measurements, take the arithmetic level Mean value), the carbon monoxide concentration is divided by the peak height to obtain a quantitative correction value. b. According to the above steps, under the same measurement conditions, the gas sample to be measured is entered into the chromatographic column and the conversion column, and the chromatographic peak height is measured. 2.3.5 Result calculation 2.3.6 Processing of measurement results 2.3.6.1 Each gas sample is measured twice, and the arithmetic mean is taken as the measurement result when the allowable difference of the measured values meets the requirements of Table 3. Otherwise, For the third measurement, take the arithmetic mean of the two measured values within the allowable difference. Table 3 Chromatographic determination tolerance 2.3.6.2 Choosing the average When the measurement range is from 0 to 100 ppm, the average value is calculated to two decimal places, and the decimal place is reported after rounding off according to the rounding rules. When the measurement range is 0 ~ 1000ppm, the average value is calculated to one decimal place, and the whole number is reported after rounding off according to the number rounding rules. Additional information. This standard was proposed by Fushun Institute of Coal Science Research Institute. This standard was drafted by Fushun Institute of Coal Science Research Institute and Hebi Mining Bureau. The main drafters of this standard are Yang Wenzheng, Chen Xingye, Ye Zhanying, Zhou Jicong, and Chang Shuhua. ......

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