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DL/T 2029-2019: Determination of total moisture in coal by automatic instrumental method
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Basic data

Standard ID DL/T 2029-2019 (DL/T2029-2019)
Description (Translated English) Determination of total moisture in coal by automatic instrumental method
Sector / Industry Electricity & Power Industry Standard (Recommended)
Classification of Chinese Standard D21
Classification of International Standard 27.100
Word Count Estimation 14,121
Date of Issue 2019-06-04
Date of Implementation 2019-10-01
Regulation (derived from) Natural Resources Department Announcement No. 7 of 2019
Issuing agency(ies) National Energy Administration
Summary This standard specifies methods for automatically determining the total moisture in coal using various special instruments and equipment. This standard stipulates that the nitrogen drying method is applicable to anthracite, bituminous coal and lignite; the air drying method is applicable to anthracite and dry bituminous coal with a volatile content of less than 20%.

DL/T 2029-2019: Determination of total moisture in coal by automatic instrumental method

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Determination of total moisture in coal by automatic instrumental method ICS 27.100 D 21 Record number. 63143-2018 People's Republic of China Electric Power Industry Standard Automatic instrument method for determination of total moisture in coal 2019-06-04 released 2019-10-01 implementation Issued by National Energy Administration

Table of contents

Foreword...I 1 Scope...1 2 Normative references...1 3 Terms and definitions...1 4 Method summary...1 5 Reagents and materials...2 6 Equipment...3 7 Laboratory conditions...5 8 Specimen...6 9 Measurement procedure...6 10 Result calculation...9 11 Method precision...10 12 Water loss compensation...10 13 Test report...10 Appendix A (informative appendix) Schematic diagram of the structure of the automatic determination of total moisture...11

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009 "Guidelines for Standardization Work Part 1.Standard Structure and Compilation". Please note that certain contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents. This standard was proposed by the China Electricity Council. This standard is under the jurisdiction of the Electric Power Plant Chemical Standardization Technical Committee. Drafting organizations of this standard. Xi'an Thermal Power Research Institute Co., Ltd., State Grid Hubei Electric Power Co., Ltd. Electric Power Research Institute, Changsha Kaiyuan Instrument Co., Ltd., Guodian Nanjing Coal Quality Supervision and Inspection Co., Ltd., Huadian Electric Power Research Institute Co., Ltd. The main drafters of this standard. Zhang Taiping, Du Xiaoguang, Zhu Qini, Ma Jun, Wen Sheng, Zhou Jiwen, Lu Maorong, Qin Tao, Zhu Qing, He Wen Li, Zhang Ming, Xu Chao This standard is formulated for the first time. The opinions or suggestions during the implementation of this standard are fed back to the Standardization Management Center of China Electricity Council (No. 2 Baiguang Road, Beijing) Number One, 100761) Automatic instrument method for determination of total moisture in coal

1 Scope

This standard specifies methods for automatically determining the total moisture in coal using various special instruments and equipment. The nitrogen drying method specified in this standard is applicable to anthracite, bituminous coal and lignite; the air drying method is applicable to anthracite and dry ash-free base volatilization Less than 20% bituminous coal.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. GB/T 211-2017 Method for determination of total moisture in coal GB/T 474 Coal sample preparation method GB/T 18510 Coal and Coke Test Alternative Method Confirmation Criteria GB/T 19494.2 Coal mechanized sampling Part 2.Preparation of coal sample GB/T 19494.3 Mechanized coal sampling Part 3.Precision measurement and bias test

3 Terms and definitions

The following terms and definitions apply to this document. 3.1 Full automatic instrument After the full moisture sample of the specified particle size and quality is placed in the specified position during the test, all test operation packages can be automatically completed according to the specified procedure Including equipment for sample mixing, aliquoting, weighing, drying, result calculation and reporting. 3.2 Semi automatic instrument In the test, in addition to the mixing, dividing and weighing of the full moisture sample, the other test operations include drying and drying of the sample. The subsequent weighing, result calculation and report can be automatically completed in accordance with the specified procedures. 3.3 Thermo gravimetric analyzer Under program temperature control, an analytical instrument that determines the relationship between the mass of a sample and the temperature and time changes. 3.4 Full automatic thermo gravimetric analysis instrument A fully automatic instrument for measuring total moisture in coal using a thermogravimetric analyzer. 3.5 Buoyancy effect When an object that does not undergo chemical changes under the action of heat is heated to a high temperature, it is affected by the shape of the object, gas density, flow rate and temperature. The phenomenon that the apparent quality of the object changes relative to the normal temperature conditions in the laboratory under the influence of factors such as temperature.

4 Method summary

4.1 Overview A certain mass of all-moisture sample is heated and dried to a constant mass under the specified temperature and atmosphere conditions, according to the mass change of the sample before and after drying Calculate the total moisture. 4.2 Method A (automatic instrument method) 4.2.1 Method A1.Nitrogen drying Use a fully automatic instrument to automatically mix, divide and accurately weigh a certain mass of 6mm full moisture sample in a shallow pan, and send it to the drying oven Inside, heated at (105~110)℃, dry and oxygen-free nitrogen stream to a constant mass, according to the mass change and buoyancy effect of the sample before and after drying The value is calculated for total moisture. 4.2.2 Method A2.Air drying Use a fully automatic instrument to automatically mix, divide and accurately weigh a certain mass of 13mm or 6mm full moisture sample in a shallow dish, and send it Put it into the drying box and heat it to a constant mass at (105~110)℃ in a stream of dry air. According to the mass change and buoyancy effect of the sample before and after drying Calculate the total moisture by value. 4.3 Method B (Semi-automatic instrument method) 4.3.1 Method B1.Nitrogen drying Using a semi-automatic instrument, accurately weigh a certain mass of 6mm full moisture sample in a crucible and place it on the sample holder in the drying room. Heated at (105~110)℃, dry oxygen-free nitrogen flow until the mass is constant, calculated according to the mass change before and after drying and the value of buoyancy effect Full moisture. 4.3.2 Method B2.Air drying Using a semi-automatic instrument, accurately weigh a certain mass of a 6mm or 13mm full moisture sample with a particle size and place it on the sample holder in the drying room. Heated at (105~110)℃ in a stream of dry air to a constant mass, calculate the total water based on the mass change before and after drying and the buoyancy effect value Minute. 4.4 Method C (Automatic Thermogravimetric Method) 4.4.1 Method C1.Nitrogen drying Using a fully automatic thermogravimetric instrument, accurately weigh a certain mass of 6mm full moisture sample with a particle size and send it to the balance pan in the drying chamber of the thermogravimetric analyzer Above, heat to a constant mass at a specified temperature and in a dry oxygen-free nitrogen stream, and calculate the total mass according to the mass change before and after drying and the buoyancy effect value. Moisture. 4.4.2 Method C2.Air drying Using a fully automatic thermogravimetric instrument, accurately weigh a certain mass of 6mm full moisture sample with a particle size and send it to the balance pan in the drying chamber of the thermogravimetric analyzer Above, it is heated to a constant mass at the specified temperature and air flow, and the total moisture is calculated according to the mass change before and after the sample is dried and the buoyancy effect value.

5 Reagents and materials

5.1 Pure nitrogen [GB/T 8979]. The purity is greater than 99.99%, and the oxygen content is less than 0.01%. 5.2 Color-changing silica gel [HG/T 2765.4]. Irregular spherical shape, particle size (2~5) mm.

6 Equipment

6.1 Fully automatic instrument 6.1.1 General The fully automatic instrument is mainly composed of a sample reduction device, a manipulator, a drying oven, an electronic balance and a control device, etc., see Appendix A Figure A.1a), b) as shown. It shall be capable of realizing local or remote status monitoring, automatic emergency shutdown, automatic control and feedback, automatic diagnosis and alarm, automatic acquisition Collection and data management functions. 6.1.2 Divider The scaler should meet the following basic requirements. a) The design and manufacture should meet the relevant requirements of GB/T 19494.2; b) Bias and precision tests should be carried out in accordance with the relevant provisions of GB/T 19494.3 to prove that there is no total moisture bias, and the reduction and test variances are not Greater than 0.03; c) The reduction ratio can be adjusted so that the remaining sample volume after the sample is reduced is as follows. when the sample size is 6mm, the mass is (100~150)g; When the sample size is 13mm, the mass is (500~550)g. 6.1.3 Manipulator It should be able to move in three-dimensional space, and can automatically complete operations such as taking and sending the tray and sample at the specified position; the movement is positioned when the tray is transferred It should be accurate and error-free; it should have travel limit protection, anti-collision protection and other functions. 6.1.4 Drying box 6.1.4.1 Nitrogen drying oven The nitrogen-passing drying oven used in Method A1 should meet the following basic requirements. a) There should be a small free space that can accommodate 1 to 4 shallow trays. Stainless steel is used on the inner surface, with nitrogen inlet and outlet. dry The box temperature field and temperature should be calibrated once a year. Each instrument and equipment can be arranged in multiple nitrogen drying ovens; b) It should be equipped with a temperature measurement and temperature control device, which can control the temperature at (105~110) ℃, with a temperature control accuracy of ±1 ℃, and has an over-temperature alarm protection function can; c) It should be equipped with a nitrogen gas device, including a pressure reducing valve, a pressure gauge, a pressure-resistant air pipe, a dryer equipped with color-changing silica gel, a flowmeter and an The gas distributor installed in the box. The scale value of the flowmeter should not be greater than 0.5L/min and the range should meet the needs of measuring nitrogen flow; The distributor should make the nitrogen flow evenly into the box to fully contact the sample and effectively replace the oxygen in the box. 6.1.4.2 Air drying oven The air drying oven used for Method A2 should meet the following basic requirements. a) It should have a large enough volume, built-in multi-layer sample plate shelf, and several shallow plates can be placed on the plate shelf. The inner surface is made of stainless steel. Air inlet and outlet; the temperature field and temperature of the drying oven should be calibrated once a year; b) Same as 6.1.4.1b); c) It should be equipped with a blower or suction pump and a flow meter. The blower or suction pump's blast suction volume and the range of the flow meter should meet the hourly change The air volume is not less than 5 times; it can make the temperature in the box uniform, air convection, and the scale value of the flowmeter is not more than 0.5L/min. 6.1.5 Electronic balance The measuring range is 2kg, and the weighing accuracy is 0.01g. It is easy to disassemble, easy to maintain and calibrate. Can be in the environment temperature (5~40) ℃, relatively humid Normal use when the degree is (40~80)%. It should be placed on a sturdy and stable table and far away from vibration sources. If necessary, the balance can be installed in shock absorption On the stage, it can effectively eliminate vibrations with a frequency of (10-50) Hz in the environment. Electronic balances should be verified/calibrated regularly. 6.1.6 Control device The hardware devices and software shall meet the requirements of instrument operation control and relevant regulations of this standard. 6.2 Semi-automatic instruments 6.2.1 General The semi-automatic instrument is mainly composed of a drying room, a sample support device, an electronic balance and a control device, etc. See Appendix A, Figure A.2. 6.2.2 Drying room 6.2.2.1 Nitrogen drying room The nitrogen-passing drying chamber used for method B1 should meet the following basic requirements. a) It should have a small enough free space and be able to accommodate the round (ring) crucible holder. The inner surface should be clean and tidy without falling off. Should have There are nitrogen inlet and outlet and weighing rod connecting port. The dry room temperature field and temperature should be calibrated once a year. b) Same as 6.1.4.1b); c) Same as 6.1.4.1c). 6.2.2.2 Air drying room The air drying chamber used for method B2 should meet the following basic requirements. a) It has a certain volume and can hold a round (ring) crucible holder; the inner surface should be clean and tidy without falling off. Should have air in and out Port and weighing rod installation port; dry room temperature field and temperature should be calibrated once a year; b) Same as 6.1.4.2b); c) Same as 6.1.4.2c). 6.2.3 Specimen support device It is composed of a sample weighing rod and a support base, a circular (ring) crucible support and its lifting and rotating mechanism. Metal materials or high temperature resistant materials should be used (Quartz, porcelain), the sample weighing rod and round (ring) crucible holder should not undergo chemical reaction, deformation, and Enough strength. The lifting and rotating mechanism should be positioned accurately, operate flexibly without jamming. 6.2.4 Electronic balance The maximum measuring range is 220g, the graduation value is 0.001g, it is convenient to disassemble, easy to maintain, calibrate and verify. The ambient temperature is (5~40) It can work reliably when ℃ and relative humidity is (40~80)%. It should be placed on a sturdy and stable table and far away from vibration sources. If necessary, the balance can be Installed on a shock absorbing platform, it can effectively eliminate vibrations with a frequency of (10-50) Hz in the environment. Reliable measures should be taken to avoid heat radiation of the heating furnace Use has a significant impact on the performance of the balance. Electronic balances should be verified/calibrated regularly. 6.2.5 Control device The hardware devices and software shall meet the requirements of instrument operation control and relevant regulations of this standard. 6.3 Fully automatic thermogravimetric instrument 6.3.1 General The automatic thermogravimetric instrument is mainly composed of a sample transfer device, a stirring and sampling device, a manipulator, a thermogravimetric analyzer, and a control device. See Appendix A, Figure A.3.It shall be capable of realizing on-site or remote status monitoring, automatic emergency shutdown, automatic control and feedback, automatic diagnosis and alarm, Automatic data collection and management function. 6.3.2 Sample transfer device The fully moisture sample bottle that has been opened can be automatically transported to the designated location. 6.3.3 Stirring and sampling device It can automatically stir and mix the sample in the full moisture sample bottle, and achieve different depth or full depth to obtain the sample, the sample amount should be controlled at (10~18)g, the sample can be automatically placed on the shallow dish and flattened; it should be automatically cleaned after each sampling, and no sample should be left. 6.3.4 Manipulator It can move in the direction of three-dimensional space, and can automatically complete operations such as taking and sending the tray and sample at the specified position; when transferring the tray, the action positioning should be Accurate and error-free; it should have travel limit protection, anti-collision protection and other functions. 6.3.5 Thermogravimetric analyzer It consists of a drying room, a nitrogen gas device, and an electronic balance, which should meet the following requirements. a) Drying room. It should be equipped with a heater and a temperature controller, which can keep the heating temperature of the sample at (105~130) ℃, with gas entering Export; b) Nitrogen venting device. the nitrogen venting device should be equipped with a nitrogen venting device, including a pressure relief valve, pressure gauge, pressure-resistant air pipe, and internal installation Color-changing silica gel dryer, flow meter and gas distributor installed in the drying room; the scale of the flow meter should not be greater than 0.5L/min and the range Should meet the needs of nitrogen flow measurement (the range is generally 5L/min); the gas distributor should allow nitrogen to evenly enter the drying room for effective replacement Indoor oxygen c) Electronic balance. the maximum range is 40g, the division value is 0.001g, it can read and transmit weighing data in real time at least every 10s; sky platform Insulation materials should be installed on the surface to prevent heat radiation from significantly affecting the performance of the balance. The weighing bracket should be made of stainless steel or other high temperature resistant materials. material. It should be placed on a sturdy and stable table and far away from vibration sources. If necessary, the balance can be installed on the shock absorber, which can effectively eliminate the mid-frequency in the environment. The rate is (10-50) Hz vibration. Electronic balances should be verified/calibrated regularly. 6.3.6 Control device The hardware devices and software shall meet the requirements of instrument operation control and relevant regulations of this standard. 6.3.7 Full moisture sample bottle The material is PVC, cylindrical, the volume should be no more than 3000mL, and it can hold (1.25~2.0)kg of full moisture sample. 6.4 Auxiliary equipment 6.4.1 Shallow dish For the square or round sample container made of stainless steel or aluminum, the bottom area should satisfy that the sample volume per unit area does not exceed 1g/cm2, and the height should not exceed 2 to 3 times lower than the nominal maximum particle size of the sample. 6.4.2 Crucible The square or round sample container made of porcelain, glass or aluminum should have a bottom area that does not exceed 2.5g/cm2 per unit area. The degree should not be less than 40mm. 6.4.3 Industrial balance The division value is 0.1g, and the range meets the requirements for weighing all-water samples.

7 Laboratory conditions

7.1 Semi-automatic instruments can share the laboratory with other instruments. Fully automatic instruments should be used in a separate laboratory, which can be reasonably arranged in Near the mechanical sampling system. The instrument should avoid direct sunlight and strong air convection, and there should be no strong electromagnetic field, strong electric spark and corrosive surroundings gas. 7.2 The power supply of the automatic moisture instrument should be arranged separately in the laboratory, and the power supply voltage and capacity should meet the requirements of the instrument. 7.3 The temperature and humidity in the laboratory should be kept stable, the temperature should be controlled at (10~30)℃, and the relative humidity should be controlled at (40~70)%.

8 samples

8.1 The full moisture sample should be prepared in accordance with the provisions of GB/T 474 or GB/T 19494.2.The mass of the full moisture sample with a particle size of 13mm is (3.0~4.0) kg, the mass of the total moisture sample with a particle size of 6mm is (1.25~2.0)kg, stored in a non-absorbent and air-tight container, weighed separately The quality and container quality should be weighed to 0.2g and indicated on the label. If the total water content is measured immediately after sample preparation, it is not necessary to weigh it. 8.2 In the case that the full moisture sample is not measured immediately after being loaded into the container, for example, after transporting the sample or storing the sample for a certain period of time, the test room is opened When measuring the total moisture, first check the sealing condition of the sample and its container, then wipe the surface clean, weigh the gross weight, and weigh it to 0.2g. And check the total mass indicated on the container label. If it is found that there is water in the container separated from the coal, the container and the coal should be placed in a drying box at a temperature not exceeding 40℃, according to GB/T 211-2017 7.1 Method A (two-step method) stipulates that the external moisture shall be determined according to Chapter 9 of this standard, and then according to relevant regulations Calculate total moisture. If the weight loss of the weighed sample does not exceed 1% of the total mass of the sample indicated on the label, the test can be confirmed if there is no change in the sealing of the container. The sample has no loss during transportation or storage. The reduced quality should be regarded as the amount of water loss during transportation or storage of the coal sample. Percentage loss, and the water loss compensation shall be carried out as described in Chapter 12 of this standard. If the weight loss of the weighed sample is greater than 1% of the total mass of the sample indicated on the label, it indicates that the coal sample may be transported or stored. In case of abnormal loss, the water loss correction is not required, but the measured water content can be used as the total water content of the sample received in the laboratory. Report results At the same time, it should indicate “the moisture loss during transportation or storage has not been corrected”, and report the container label, sealing condition and quality loss rate together Report.

9 Measurement procedure

9.1 Method A1 (Nitrogen Drying) 9.1.1 Put the clean shallow tray with constant weight into the designated storage area, turn on the power of the computer and equipment, and warm up for more than 30 minutes. 9.1.2 According to the requirements of the manual, enter the instrument test system, check or set various instrument parameters, and enter information such as sample name and serial number. Of course Then put all the samples into the inlet of the instrument and equipment, and place the emptied container at the outlet of the equipment for storing samples. 9.1.3 Start the equipment and operate automatically according to the following procedures. 9.1.3.1 The manipulator takes out the clean platter from the platter area twice in a row, weighs the weight of the empty platter, weighs it to 0.02g, and transfers it to the two outlets of the scaler On the sampling platform at the inlet; 9.1.3.2 Start the dividing unit, and automatically divide two samples with a mass of (100~150)g from the sample to the weighed shallow pan; 9.1.3.3 After the flattening device flattens the sample in the shallow pan, the manipulator transfers the sample tray to the balance to weigh the mass, and the accuracy is 0.02g; 9.1.3.4 Open the door of the drying oven, put the sample tray into the drying oven and close it; according to the flow rate of not less than 30 air changes per hour (should be The residual oxygen concentration of the sample in the drying box at room temperature shall be adjusted to not more than 0.01%), and dry nitrogen gas (2~3) min. The temperature in the drying box rises to (105~110)℃, and it is dried for 2h (the drying time can be adjusted according to different types of samples); 9.1.3.5 The manipulator takes out the shallow pan while it is hot and weighs it to 0.02g; 9.1.3.6 Carry out inspection drying for 15 minutes each time until the mass of the sample is reduced by no more than 0.06% of the sample mass after two consecutive dryings. Or until the quality increases. In the latter case, the previous mass increase is used as the basis for calculation. Automatic according to Chapter 10 Calculate and save the measurement results; 9.1.3.7 The manipulator moves the tray to the sample disposal area to discard the waste samples, clean the tray, and then return it to the tray area for storage and recycling. 9.1.4 Determination of buoyancy effect value 9.1.4.1 Before measuring the total moisture content of the sample, the buoyancy effect value of the shallow pan shall be determined. 9.1.4.2 Without adding the sample, the shallow pan that has been accurately weighed (weighed to 0.02g) at room temperature is sent into the drying box, and the The sample is heated for 1 hour at the drying temperature and ventilation flow rate, and the thermal m...

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