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GB/T 37355-2019

Chinese Standard: 'GB/T 37355-2019'
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GB/T 37355-2019English169 Add to Cart Days<=3 Test method of mercury removal rate for activated carbon mercury removal catalyst Valid GB/T 37355-2019
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Detail Information of GB/T 37355-2019; GB/T37355-2019
Description (Translated English): Test method of mercury removal rate for activated carbon mercury removal catalyst
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G74
Classification of International Standard: 71.100.99
Word Count Estimation: 10,136
Date of Issue: 2019-03-25
Date of Implementation: 1/2/2020
Drafting Organization: Sinopec Nanjing Chemical Research Institute Co., Ltd., Wuhan Kelin Fine Chemical Co., Ltd., Beijing Sanju Environmental Protection New Material Co., Ltd., Xi-An Xiangyang Aerospace Materials Co., Ltd., Shandong Xunda Chemical Group Co., Ltd.
Administrative Organization: National Chemical Standardization Technical Committee (SAC/TC 63)
Proposing organization: China Petroleum and Chemical Industry Federation
Issuing agency(ies): State Administration of Markets and China National Standardization Administration


GB/T 37355-2019
Test method of mercury removal rate for activated carbon mercury removal catalyst
ICS 71.100.99
G74
National Standards of People's Republic of China
Test method for mercury removal rate of activated carbon mercury removal catalyst
Published on.2019-03-25
2020-02-01 implementation
State market supervision and administration
China National Standardization Administration issued
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Petroleum and Chemical Industry Federation.
This standard is under the jurisdiction of the National Chemical Standardization Technical Committee (SAC/TC63).
This standard was drafted. Sinopec Nanjing Chemical Research Institute Co., Ltd., Wuhan Kelin Fine Chemical Co., Ltd., Beijing Sanju Environmental Protection New
Materials Co., Ltd., Xi'an Xiangyang Aerospace Materials Co., Ltd., Shandong Schindler Chemical Group Co., Ltd.
The main drafters of this standard. Li Zhongyu, Chen Yanhao, Zhang Xianmao, Zhao Wentao, Xu Longlong, Hu Wenbin, Li Xingjian, Sun Guoshuang, Feng Chao, Wang Ze.
Test method for mercury removal rate of activated carbon mercury removal catalyst
1 Scope
This standard specifies the test method for mercury removal rate of activated carbon mercury removal catalyst.
This standard is applicable to activated carbon as the carrier, with elemental sulfur, sulfide and metal oxide as active components, mainly used for removing natural gas.
Activated carbon mercury removal catalyst for mercury in syngas, refinery gas, and industrial tail gas.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 6003.1 Test sieves - Technical requirements and testing - Part 1
GB/T 6679 Solid Chemical Products Sampling General
GB/T 16781.1 Determination of mercury content of natural gas - Part 1
3 Principle
The trace amount of mercury in the raw material gas is removed by physical adsorption and chemical reaction under the action of the catalyst. By measuring the reactor in and out
The mass concentration of mercury in the mouth is used to calculate the mercury content of the catalyst to characterize the mercury removal rate of the catalyst.
4 test device
4.1 device
The flow chart of the mercury removal rate test device for activated carbon mercury removal catalyst is shown in Figure 1.
Description.
1---nitrogen steel cylinder;
2---Rotor flowmeter;
3---mercury generator;
4---water bath;
5---mixer;
6---reactor;
7---absorber;
8---wet gas flow meter.
Figure 1 Schematic diagram of the test device
4.2 Main performance
The main performance design parameters of the mercury removal rate test device for activated carbon mercury removal catalyst are shown in Table 1.
Table 1 Main performance design parameters of the test device
Serial number item parameter
1 Specifications of the reaction tube in the reactor/mm φ6.0 × 0.5
2 use pressure/MPa atmospheric pressure
3 maximum operating temperature/° C 80
4 Recurrence (relative error) /% ≤5
4.3 Checking
Under normal circumstances, the reproducibility of the test device is measured at least once a year with reference samples or retained samples. The measurement method is according to Chapter 6,
The provisions of Chapter 7.
5 samples
5.1 Laboratory samples
Obtained according to the provisions of GB/T 6679.
5.2 Sample
Take appropriate amount of laboratory samples and place them in a porcelain mortar. The test sieves with a hole diameter of 0.380mm and 0.830mm
Screening of R40/3 series in GB/T 6003.1). Take samples with a particle size of 0.380mm~0.830mm and measure them according to the provisions of Appendix A.
Tight stack density.
5.3 Samples
According to the tight packing density of the sample, 3.0 mL of the corresponding mass of the sample was weighed to the nearest 0.01 g, and was used.
6 test steps
Warning---The test raw material gas and tail gas (including mercury) involved in this standard have poisoning hazards to human health and safety, and must be strict.
The system is leaking, and there is no open fire on the site. It should be equipped with necessary fire-fighting equipment and ventilation equipment.
6.1 Preparation of raw material gas
The liquid mercury is placed in a mercury generator, and the nitrogen gas is passed through the mercury generator to carry out the gaseous mercury, and the water bath temperature and the nitrogen flow rate are controlled.
The mass concentration of mercury in the gas is 20.0 mg/m3 to 25.0 mg/m3.
6.2 Filling of samples
A layer of glass cloth is placed on the bottom of the reaction tube, and 10 mL of pre-treated clean quartz sand with a particle size of 0.380 mm to 0.830 mm is used.
Tightly stack the method into the reaction tube, then place a layer of glass cloth on the quartz sand, slowly pour the sample (see 5.3) into the reaction tube, and add a wooden rod
Gently tap the wall of the reaction tube to fill the sample tightly, evenly and evenly, then pad a layer of glass cloth and fill it with quartz sand to the inlet of the reaction tube.
The reaction tube is connected to the system at a position of about 5 mm.
6.3 System leak test
Close all outlet and vent valves of the system, pass nitrogen, boost the system to 0.1 MPa, and close the system inlet valve. Check with soapy water
Check the joints of each joint for leak testing. After the test leak meets the requirements, open the system outlet valve exhaust to reduce the system to normal pressure.
6.4 Mercury absorption
The temperature of the water bath was raised to 35 ° C and kept at a constant temperature. The system is purged with nitrogen, and the system pressure is controlled and regulated to normal pressure, and the reactor temperature is
At 25 ° C, the volumetric airspeed is 10000 h-1 (see Appendix B for gas-related flow correction) and the initial reading of the wet gas flow meter is recorded.
After several hours (depending on the mercury removal rate of the mercury removal catalyst), the mass concentration of mercury in the inlet and outlet of the reactor is measured, and the measurement is performed every 2 hours.
Times. When the mass concentration of mercury in the exhaust gas is found to be increased, it is measured once every 30 minutes; when the mass concentration of mercury exceeds 100 μg/m3,
Immediately measure twice in a row; if the measurement still exceeds 100 μg/m3, immediately turn off the mercury generator and record the wet gas flow.
The termination reading of the meter.
6.5 Determination of mercury mass concentration
6.5.1 Imported mercury mass concentration
Take 30mL potassium permanganate-sulfuric acid solution (a volume of 40g/L potassium permanganate, a volume of 1 1 sulfuric acid solution and two volumes
The absorption bottle of water) absorbs 100 mL of imported gas. After measuring 2.00 mL of the absorption liquid and transferring it to a 100 mL volumetric flask, the volume was adjusted and shaken. then,
The mass concentration of mercury was determined by atomic absorption spectrometry according to the provisions of GB/T 16781.1.
6.5.2 Export mercury mass concentration
Take 30mL potassium permanganate-sulfuric acid solution (a volume of 40g/L potassium permanganate, a volume of 1 1 sulfuric acid solution and two volumes
The absorption bottle of water) absorbs 300 mL of outlet gas. After measuring 10.00 mL of the absorption liquid and transferring it to a 100 mL volumetric flask, the volume was adjusted and shaken. Of course
After that, the mass concentration of mercury was determined by atomic absorption spectrometry according to the provisions of GB/T 16781.1.
6.6 Parking
After the end of the test, the system was replaced with nitrogen, and the replacement was stopped after 15 minutes.
7 test data processing
The mercury removal rate of the catalyst is calculated as the mercury capacity E, calculated according to formula (1).
E=
V(ρ1-ρ2)×10-6
m ×100%
(1)
In the formula.
The value of the gas volume measured by the V--wet gas flow meter, in cubic meters (m3);
Ρ1---The value of the mass concentration of mercury in the inlet gas of the reactor, in micrograms per cubic meter (μg/m3);
2-2 - the value of the mass concentration of mercury in the outlet gas of the reactor, in micrograms per cubic meter (μg/m3);
m---The value of the mass of the catalyst sample, in grams (g).
The arithmetic mean of the results of two consecutive measurements is the measurement result, and the relative error of the two measurement results should be no more than 5%.
Appendix A
(normative appendix)
Determination of compact density of catalyst samples
A.1 Stacking of specimens
Divide the appropriate amount of sample (see 5.2) into several parts, and add them to the 25mL measuring cylinder in turn; each time, the measuring cylinder needs to vibrate up and down several times.
The time until the position of the sample in the measuring cylinder does not change to be tapped, and the operation is repeated until the amount of the sample to be ground is 10 mL.
A.2 Weighing of sample
The mass of the tapped 10 mL sample (see A.1) was weighed to the nearest 0.01 g.
A.3 Calculation of tight bulk density
Tight packing density ρ, the value is expressed in grams per milliliter (g/mL), calculated according to formula (A.1).
ρ=
M2-m1
(A.1)
In the formula.
The value of the mass of the m2---25mL graduated cylinder and the 10mL sample, in grams (g);
The value of the mass of the m1---25mL measuring cylinder in grams (g);
V --- The value of the volume of the sample in milliliters (mL).
The result of the calculation is retained to two decimal places. Taking the arithmetic mean of the parallel measurement results as the measurement result, the phase of the parallel measurement result
The error should be no more than 2.0%.
Appendix B
(normative appendix)
Rotor flowmeter flow correction
B.1 Calibration device
The schematic diagram of the flow calibration device for the wet gas flow meter is shown in Figure B.1.
Description.
1---feed gas inlet valve;
2---gas volume control valve;
3---Rotor flowmeter;
4---water pressure difference meter;
5---thermometer;
6---wet gas flow meter;
7---Stop.
Figure B.1 Schematic diagram of the flow calibration device for the wet gas flow meter
First adjust the level of the wet gas flow meter. Then unscrew the nut of the water level overflow hole and add distilled water to the wet gas flow meter.
When the water overflows from the overflow hole, stop adding water. When the overflow hole does not overflow, tighten the overflow nut.
B.2 Calibration steps
The intake valve is opened, and the raw material gas enters the wet gas flow meter through the rotameter, and the size of the gas flow is adjusted by the cork. Write down the wet gas
The initial reading of the body flow meter, while starting the stopwatch timing, when the wet gas flow meter measures a certain amount of gas volume, press the stopwatch, write down
Intermittent readings of the inter- and wet gas flow meters and calculate the volumetric flow of the gas. Adjust the gas flow rate and repeat the measurement until the gas body
When the accumulated flow rate is Q, the scale position of the upper end surface of the float in the rotor flowmeter is determined.
B.3 Flow calculation
Gas volume flow rate Q, expressed in milliliters per minute (mL/min), calculated according to equation (B.1).
Q=
SvVcatp0T
60pT0
(B.1)
In the formula.
Q --- gas volume flow value in milliliters per minute (mL/min);
Sv --- the value of airspeed, in hours per hour (h-1);
Vcat---the value of the sample volume of the catalyst, in milliliters (mL);
P0 --- the value of atmospheric pressure in the standard state, the unit is Pascal (Pa) (p0 = 101325Pa);
T --- the value of the thermodynamic temperature at room temperature in the determination of Kelvin (K);
p --- the value of the atmospheric pressure at the time of measurement, the unit is Pascal (Pa);
T0 --- The value of the thermodynamic temperature in the standard state, in Kelvin (K) (T0 = 273K).
Related standard:   GB/T 37354-2019  GB/T 37359-2019
   
 
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