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HJ 917-2017: Stationary source emission--Determination of total gaseous mercury --Carbon sorbent traps / thermal cracking atomic absorption spectrophotometric method
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Stationary source emission--Determination of total gaseous mercury --Carbon sorbent traps / thermal cracking atomic absorption spectrophotometric method
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HJ 917-2017
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PDF similar to HJ 917-2017
Standard similar to HJ 917-2017 HJ 1013 HJ 836 HJ 734 HJ 973 HJ 547 HJ 545 Basic data | Standard ID | HJ 917-2017 (HJ917-2017) | | Description (Translated English) | Stationary source emission--Determination of total gaseous mercury --Carbon sorbent traps / thermal cracking atomic absorption spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Word Count Estimation | 10,142 | | Date of Issue | 2017-12-28 | | Date of Implementation | 2018-04-01 | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 85 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 917-2017: Stationary source emission--Determination of total gaseous mercury --Carbon sorbent traps / thermal cracking atomic absorption spectrophotometric method
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People's Republic of China national environmental protection standards
Stationary source emission-Determination of total gaseous mercury
-Carbon sorbent traps/thermal cracking atomic absorption
spectrophotometric method
2017-12-28 Published
2018-04-01 implementation
Directory
Foreword .ii
1 scope of application .1
2 Normative references .1
3 method principle .1
4 Interference and elimination .1
5 Reagents and materials .1
6 instruments and equipment .2
7 samples .3
8 Analysis steps .4
9 Results Calculation and Presentation .4
10 precision and accuracy 5
11 Quality Assurance and Quality Control .5
12 Waste treatment 6
13 Matters needing attention 6
Foreword
In order to implement the Law of the People's Republic of China on Environmental Protection and the Law of the People's Republic of China on Prevention and Control of Atmospheric Pollution,
Habitat, to protect human health, standardize the determination of gaseous mercury in the exhaust gas pollution sources, the development of this standard.
This standard specifies the determination of gaseous fixed-source emissions of mercury in activated carbon adsorption/thermal cracking atomic absorption spectrophotometry.
This standard is released for the first time.
This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop.
This standard was drafted. National Environmental Analysis Test Center.
This standard verification unit. Beijing Environmental Protection Monitoring Center, Xinjiang Uygur Autonomous Region Environmental Monitoring Station, China Central
Environmental Science Research Institute, Tsinghua University, Chaoyang District, Beijing Environmental Protection Monitoring Station and Binhai New Area, Tianjin Environmental Protection Monitoring Station.
This standard MEP approved on December 28,
This standard since April 1,.2018 come into operation.
This standard is interpreted by the MEP.
Stationary source emissions - Determination of gaseous mercury - Activated carbon adsorption/thermal cracking
Atomic absorption spectrophotometry
Warning. The sulfuric acid used in the experiment has a strong corrosive, HgCl2 standard solution is toxic, reagent preparation process
Should be carried out in the fume hood, operation should be required to wear protective equipment, to avoid inhalation of the respiratory tract and skin, clothing.
1 scope of application
This standard specifies the determination of gaseous fixed-source emissions of mercury in activated carbon adsorption/thermal cracking atomic absorption spectrophotometry.
This standard applies to the installation of denitration, dust removal, desulfurization of coal-fired power plant emissions of mercury in the determination of gaseous mercury.
When the sampling volume is 10 L (dry flue gas under standard conditions), the detection limit is 0.1 μg/m3 and the lower limit of determination is 0.4 μg/m3.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this book
standard.
Determination of Particulate Matter and Gaseous Pollutants in Exhaust of Fixed Pollution Sources GB/T 16157
3 method principle
Through this standard sampling system, the exhaust gas in the effective enrichment of gaseous mercury in the iodine or other halogen and its compounds
Treated activated carbon material, using direct pyrolysis atomic absorption spectrophotometry Determination of activated carbon in the adsorbent tube of mercury in the material
Content, based on the sampling volume, calculate the concentration of gaseous mercury.
4 Interference and elimination
SO2, NOX will inhibit the capture of mercury on the activated carbon, carbon dioxide compounds in the front of the adsorption tube to remove acid gas interference.
5 Reagents and materials
Unless otherwise specified, all analytical reagents used in the analysis are in accordance with national standards. The experimental water is freshly prepared deionized water or distilled water.
5.1 Mercury chloride (HgCl2).
5.2 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml.
5.3 sulfuric acid solution. c (1/2 H2SO4) = 0.5 mol/L.
Pipette 6.9 ml sulfuric acid (5.2) slowly adding an appropriate amount of water, diluted after cooling, constant volume to 500 ml, mix.
5.4 Mercury standard stock solution. ρ (Hg) = 1000 mg/L.
Weigh 0.1354 g mercuric chloride (5.1), with sulfuric acid solution (5.3) dissolved and diluted to a constant volume of 100 ml. Can also be used
Mercury certified reference material on the market.
5.5 Mercury standard solution. ρ (Hg) = 10.0 mg/L.
Remove the standard stock solution of mercury (5.4) 1.00 ml, dilute it with sulfuric acid solution (5.3) to make a volume of 100 ml. Pro use now with.
6 instruments and equipment
6.1 Sampling System
6.1.1 Sampling system components
Typical gaseous mercury sampling systems typically include activated carbon sorbent tubes, sampling probes, temperature sensors, dehumidification units,
Sampling controller, sampling pump, see Figure 1.
Figure 1 Typical gaseous mercury sampling system
6.1.2 activated carbon adsorption tube
6.1.2.1 two-stage
The adsorption tube contains two sections of specially prepared activated carbon treated with iodine or other halogen and its compounds and each section can be divided
Analysis, see Figure 2.
Figure 2 two-stage activated carbon adsorption tube
6.1.2.2 Three-stage type
Adsorption tube equipped with three sections of special activated carbon, which plus the standard section of activated carbon to add a known quality of mercury, can also be used on the market
Activated carbon tubes have been spiked, see Figure 3.
Figure 3 Three-stage activated carbon adsorption tube
6.1.3 Sampling probe
Probe with heating function (heating temperature not less than 120 ℃), to prevent flue gas condensation.
6.1.4 Temperature sensor
Measurement accuracy within ± 1.5 ℃.
6.1.5 dehumidification device
Before the airflow enters the sampling controller, the dehumidifier should be used to remove the water vapor from the airflow.
6.1.6 Sampling controller
Used to determine the total volume of dry flue gas, you can control the sampling flow to maintain within ± 10%.
6.1.7 Sampling pump
Power should be able to meet the system flow range requirements.
6.2 mercury analyzer
Has a thermal cracking unit, the sample of mercury atomized to form gaseous mercury, atomic absorption spectrophotometric quantitative analysis
Mercury, the detection limit should be less than 2.0 μg/kg.
6.3 Other
Common laboratory equipment and equipment.
7 samples
7.1 Sample Collection
Fixed pollution source sampling and laying of sampling points should be consistent with GB/T 16157 in the relevant provisions. Before and after sampling should be
Airtight testing. For each sampling, two activated carbon adsorption tubes (6.1.2.1) must be used for parallel and dual sampling,
With a flow rate of 0.2 L/min ~ 0.6 L/min, the sampling time should not be less than 30 min. After sampling, record the sampling time, the atmosphere
Pressure Remove the sampled activated carbon tube and seal both ends to wipe off the deposits on the outer wall of the tube.
At least one blank activated carbon adsorption tube (6.1.2.1) shall be taken for each sampling, taken to the sampling site as a complete program empty
White samples are stored with the collected samples and brought back to the laboratory for analysis.
7.2 Sample Storage
All samples should be stored in sealed sample storage container at room temperature, the sample can be stored for 14 d.
7.3 Dynamic spiked samples
Take a three-stage adsorption tube (6.1.2.2) and perform dynamic spiking of the sample according to the same procedure (7.1) as for sample collection
Of the collection, the standard addition should be 50% of the actual amount of mercury samples to 150%, each batch should be collected a dynamic spiked samples.
7.4 Laboratory blank samples
Blank activated carbon adsorption tubes (6.1.2.1) were used as laboratory blank samples.
8 Analysis steps
8.1 Instrument analysis reference conditions
Optimize assay conditions or parameters based on instrument user's manual. Thermal cracking temperature should be greater than 650 ℃.
8.2 standard curve established
Pipette Mercury standard solution (5.5) 0 μl, 10.0 μl, 20.0 μl, 40.0 μl, 60.0 μl, 80.0 μl and 100 μl
To the sample boat, the mercury contents were 0 ng, 100 ng,.200 ng, 400 ng, 600 ng, 800 ng and 1000 ng
Standard series. According to mercury analyzer operating procedures were measured, the instrument response to mercury content to establish a standard curve.
Note. The standard curve can also be weighed with different quality soil or sediment containing mercury standard preparation.
8.3 Sample Determination
The activated carbon adsorption tube at both ends of the seal cap is opened, the interval of quartz wool and each section of activated carbon were transferred to the sample boat
, The sample was measured under the same conditions as in the standard curve (8.2).
8.4 Determination of blank samples
8.4.1 Determination of the entire program blank samples
According to the same conditions with the sample (8.3) were measured to determine the entire program blank sample mercury content.
8.4.2 Laboratory blank sample determination
The mercury content of the laboratory blank samples (7.4) was determined according to the same conditions as the samples (8.3).
9 results calculated and expressed
9.1 Calculation Results
The concentration of gaseous mercury in the exhaust gas of fixed sources is calculated according to formula (1)
nd V
mmm 1 2 0
(1)
Where. - Gaseous mercury concentration in dry flue gas at standard conditions (273.15 K, 101.325 kPa), μg/m3;
m1 - the mercury content measured in the first paragraph of the adsorption tube, ng;
m2 - measured in the second paragraph of the adsorption tube mercury content, ng;
m0 - laboratory mercury content in blank samples, ng;
Vnd - the standard state of the sample volume of dry gas, L.
9.2 results indicated
When the test result is less than 100 μg/m3, keep one decimal place; when the test result is greater than or equal to 100 μg/m3,
Keep 3 significant digits.
10 precision and accuracy
10.1 Precision
In six laboratories, gaseous mercury simulated flue gas was repeatedly collected at concentrations of 5.0 μg/m3, 20.0 μg/m3 and 40.0 μg/m3
Six samples were collected for determination. The relative standard deviations in the laboratory were 4.8% -9.7%, 7.5% -9.9% and 7.1% -9.6% respectively.
The relative standard deviations (RSDs) were 4.5%, 4.1% and 4.7%, respectively. The repeatability limits were 1.1 μg/m3 and 5.4 μg/m3,
8.9 μg/m3; reproducibility limits were 1.2 μg/m3, 5.5 μg/m3 and 9.5 μg/m3, respectively.
10.2 Accuracy
In six laboratories, gaseous mercury simulated flue gas was repeatedly collected at concentrations of 2.0 μg/m3, 20.0 μg/m3 and 50.0 μg/m3
Six samples were collected for determination. the relative errors were -9.3% -7.9%, 0.0% -10.0%, -10.0% -2.3%, respectively;
The final error values were -1.8% ± 6.0%, 6.4% ± 4.3%, - 8.5% ± 3.0%.
11 Quality Assurance and Quality Control
11.1 blank sample
The sampling volume of 10L, the whole program blank sample (8.4.1) should not exceed the detection limit; sample body
Product is 10 L, the laboratory blank sample measured value (8.4.2) should not exceed the detection limit.
11.2 standard curve
The correlation coefficient of the standard curve should be ≥0.999.
11.3 Parallel samples
When the mercury concentration > 1 μg/m3, the relative deviation (RD) of the parallel sample determination is less than or equal to 10%; when the mercury concentration is less than or equal to 1 μg/m3,
The relative deviation (RD) of parallel samples was ≤20%.
11.4 penetration rate
When the mercury concentration > 1 μg/m3, the absorption tube penetration B ≤ 10%; when the mercury concentration ≤ 1 μg/m3, the penetration rate
B≤20%. According to the formula (2) Calculate the absorption tube penetration rate.
Where. B-pipe penetration rate,%;
m2 - the second section of the adsorption tube activated carbon measured mercury content, ng;
m1-adsorbed tube in the first paragraph of the activated carbon measured mercury content, ng.
11.5 dynamic spike recovery
The dynamic spiked sample recovery R is between 85% and 115%.
12 Waste treatment
Hg waste gas generated in the experiment before the exclusion of the use of halogen-containing activated carbon adsorption, waste generated by the waste should be concentrated
Set, and make the appropriate logo, commissioned by a qualified unit for processing.
13 Precautions
13.1 Adsorption tube must be installed in the probe so that the flue gas directly into the adsorption tube, to ensure that there is no vent between the probe and the adsorption tube
leak.
13.2 Sampling, the flow rate to be controlled within the specified range, the flow is too high can easily lead to the penetration of activated carbon.
13.3 Sampling process, particulate matter may lead to blockage of the sampling tube and affect the normal sampling work, with a smaller flow, more
Long time sampling, access to a sufficient amount of the test pollutants.
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