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HJ 1007-2018: Stationary source emission - Determination of alkali mist - Inductively coupled plasma optical emission spectrometry method
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Stationary source emission - Determination of alkali mist - Inductively coupled plasma optical emission spectrometry method
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HJ 1007-2018
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PDF similar to HJ 1007-2018
Standard similar to HJ 1007-2018 HJ 1013 HJ 836 HJ 734 HJ 1131 HJ 1006 Basic data | Standard ID | HJ 1007-2018 (HJ1007-2018) | | Description (Translated English) | Stationary source emission - Determination of alkali mist - Inductively coupled plasma optical emission spectrometry method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Word Count Estimation | 9,938 | | Date of Issue | 2018-12-26 | | Date of Implementation | 2019-06-01 | | Regulation (derived from) | Ministry of Ecology and Environment Announcement No. 71 of 2018 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1007-2018: Stationary source emission - Determination of alkali mist - Inductively coupled plasma optical emission spectrometry method
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Stationary source emission - Determination of alkali mist - Inductively coupled plasma optical emission spectrometry method
National Environmental Protection Standard of the People's Republic
Determination of alkali mist of fixed pollution source
Inductively coupled plasma optical emission spectrometry
Stationary source emission-Determination of alkali mist
-Inductively coupled plasma optical emission spectrometry method
Published on.2018-12-26
2019-06-01 Implementation
Ministry of Ecology and Environment released
i directory
Foreword...ii
1 Scope...1
2 Normative references...1
3 Terms and Definitions...1
4 Principles of the method...1
5 Reagents and materials...1
6 Instruments and Equipment...2
7 samples... 2
8 Analysis steps...3
9 Calculation and representation of results...4
10 Precision and Accuracy...4
11 Quality Assurance and Quality Control...4
12 Waste treatment...5
Foreword
To protect the "Environmental Protection Law of the People's Republic of China" and the "Air Pollution Control Law of the People's Republic of China"
This standard is formulated to ensure the health of human body and to standardize the determination method of alkali mist in fixed pollution source exhaust gas.
This standard specifies the inductively coupled plasma optical emission spectrometry for the determination of alkali mist in a fixed source of exhaust gas.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Harbin Environmental Monitoring Center Station.
This standard is verified by. Heilongjiang Provincial Environmental Monitoring Center Station, National Environmental Analysis and Testing Center, Beijing Environmental Protection
Monitoring Center, Tianjin Ecological Environment Monitoring Center, Hangzhou Environmental Monitoring Center Station and Changchun Environmental Monitoring Center Station.
This standard is approved by the Ministry of Ecology and Environment on December 26,.2018.
This standard has been implemented since June 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Determination of alkali mist of fixed pollution source
Inductively coupled plasma optical emission spectrometry
1 Scope of application
This standard specifies the inductively coupled plasma optical emission spectrometry for the determination of alkali mist in a fixed source of exhaust gas.
This standard applies to the determination of alkali mist in the fixed source of waste gas in the steel industry.
When the sampling volume is.200 L (standard dry volume), the method detection limit is 0.2 mg/m3, and the lower limit of determination is 0.8 mg/m3.
2 Normative references
This standard refers to the following documents or their terms. For undated references, the valid version applies to this
standard.
GB/T 16157 Determination of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants
HJ/T 48 soot sampler technical conditions
HJ/T 373 Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Source Monitoring (Trial)
HJ/T 397 Fixed Source Exhaust Gas Monitoring Technical Specification
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
Alkali mist
The alkali mist measured by this standard refers to droplets and particulate matter containing sodium and its compounds produced during the production process (with NaOH).
meter).
4 Principle of the method
The alkali mist in the fixed pollution source exhaust gas is trapped in the quartz fiber filter cartridge by means of constant velocity sampling. Sampling cartridge
Extracted with water, the sodium in the extract is determined by inductively coupled plasma optical emission spectrometry, based on sodium content and sampling
The dry volume of the standard is used to calculate the concentration of the alkali mist.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. Experimental water is resistivity ≥
18 MΩ·cm of deionized water.
5.1 Sodium chloride (NaCl).
25.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 Sodium standard stock solution. ρ (Na ) = 1000 mg/L.
After burning at 400-450 ° C to constant weight, accurately weigh 2.5421 g of sodium chloride (5.1), dissolve in water and dilute to 1000 ml.
Mix in a volumetric flask. Transfer to a polyethylene bottle, refrigerate at 4 ° C or less, and seal for 6 months. Can also be purchased commercially available
Standard solution.
5.4 Sodium standard use solution. ρ (Na ) = 100 mg/L.
Pipette 10.00 ml of sodium standard stock solution (5.3), dilute with water to a volume of 100 ml volumetric flask, mix, use
Match.
5.5 Nitric acid solution. 1 1.
5.6 Quartz fiber filter cartridge. The filter cartridge has a barrier efficiency of not less than 99.9% for particles larger than 0.5 μm.
5.7 Filter membrane. 0.45 μm inorganic water microporous membrane.
5.8 Carrier gas. Argon, purity ≥99.9%.
6 Instruments and equipment
6.1 Smoke sampler. Performance and technical indicators shall comply with HJ/T 48.
6.2 Inductively coupled plasma optical emission spectrometer.
6.3 Analytical balance. The calibration scale value is 0.1 mg.
6.4 Ultrasonic cleaner. The ultrasonic frequency range is 40-100 kHz, and the ultrasonic power range is 100-600 W.
6.5 Electric heating plate. Temperature control accuracy is better than ±5 °C.
6.6 Stuffed conical flasks.
6.7 Common instruments and equipment used in general laboratories.
7 samples
7.1 Sample Collection
The monitoring points, frequency and exhaust parameters of fixed pollution source exhaust gas are measured in accordance with GB/T 16157, HJ/T 373 and
The relevant provisions of HJ/T 397 are implemented.
Before sampling, the sampler should be subjected to flow calibration and airtightness check of the sampling system. The instrument automatically adjusts the flow during the sampling process.
The amount maintains constant velocity sampling. After sampling, clean the sampling nozzle and the inner wall of the elbow with water into a conical flask (6.6), and seal the bottle.
mouth.
7.2 Sample storage
After the sample of the filter cartridge is collected, the seal is folded inward and placed vertically in a filter cartridge to be sealed and stored. Clear in a conical flask
The washing solution is sealed and stored.
The sample is stored in a dry, dark, room temperature environment.
7.3 Preparation of samples
37.3.1 Ultrasonic extraction
Cut the sampled filter cartridge into small pieces, place it in a stoppered flask containing the cleaning solution, and dip the filter cartridge with an appropriate amount of water.
The stoppered conical flask was placed in an ultrasonic cleaner and ultrasonically extracted for 10 min. Filter through filter (5.7), wash the filter with water and
Stir the flask, add 2 ml of nitric acid solution (5.5) to the filtrate, and dilute to 100 ml volumetric flask with water.
7.3.2 Heating leaching method
Cut the sampled filter cartridge into small pieces, place it in a stoppered conical flask containing the cleaning solution, and dip the filter cartridge with a proper amount of water.
Place a glass funnel on the mouth and heat it to a near boiling point on an electric furnace or a hot plate. After about 10 minutes, remove it and cool to room temperature. Filter membrane (5.7)
Filter, wash the filter with water and a conical flask, add 2 ml of nitric acid solution (5.5) to the filtrate, and dilute to 100 ml with water.
In the volumetric flask.
7.4 Preparation of blank samples
Take the same batch of filter cartridges for sampling, and prepare at least 2 empty according to the same steps as the preparation of the sample (7.3.1 or 7.3.2).
White sample.
8 Analysis steps
8.1 Instrument reference analysis conditions
Use the instrument operating parameters recommended by the instrument's instruction manual. Table 1 gives the measurement reference analysis conditions.
Table 1 Reference analysis conditions of inductively coupled plasma optical emission spectrometer
Plasma flow
(L/min)
Carrier gas flow
(L/min)
Auxiliary gas flow
(L/min)
Injection volume
(ml/min)
High frequency power
(kW)
Direction of observation
Observation distance
(mm)
Measuring wavelength
(nm)
1.5 0.55 0.22 1.0 1.4 Radial 15 589.592
8.2 Establishment of the standard curve
Accurately remove 0.00 ml, 1.00 ml, 2.00 ml, 5.00 ml, 10.00 ml, 20.00 ml of sodium standard solution (5.4)
Place in a set of 100 ml volumetric flasks, add 2 ml of nitric acid solution (5.5), dilute to volume with water and mix. Formulated separately
The sodium standard series are 0 mg/L, 1.00 mg/L, 2.00 mg/L, 5.00 mg/L, 10.0 mg/L, 20.0 mg/L. Electricity
Inductively coupled plasma emission spectrometer was used to determine the sodium element mass concentration as the abscissa and the response value as the ordinate.
standard curve line.
8.3 Sample determination
The measurement of the sample was carried out according to the same instrument reference analysis conditions (8.1) and analysis steps as the establishment of the standard curve.
Note. If the sodium concentration exceeds the standard curve, the sample should be diluted and measured, and the dilution factor (D) recorded.
8.4 Blank test
The measurement of the blank sample was carried out in the same manner as the measurement of the sample.
49 Calculation and representation of results
9.1 Calculation of results
The alkali mist concentration in the exhaust gas is calculated by the following formula.
1 0( ) 1.74
Nd
ρ ρ V
ρ D
− ×
= × × (1)
Where. ρ--the concentration of alkali mist in the exhaust gas (calculated as NaOH), mg/m3;
- sodium (Na) concentration in the sample, mg/L;
- the average sodium (Na) concentration in the blank sample, mg/L;
-- sample volume, ml;
Nd
- the sampling volume of dry flue gas under standard conditions, m3;
D--sample dilution factor;
1.74 - molar mass of NaOH/molar mass of Na.
Note. The blank sample is diluted as many times as the actual sample.
9.2 Results representation
The retention of the number of digits after the decimal point of the measurement result is consistent with the method detection limit, and up to three significant digits are reserved.
10 Precision and accuracy
10.1 Precision
6 laboratories for uniform blank filtration of sodium content 0.50 mg, 1.50 mg, and 3.40 mg (calculated as NaOH)
The tube was spiked and the test was repeated 6 times. The relative standard deviations in the experimental room are. 1.9% to 11%, 0.6% to 8.7%.
And 1.3% to 9.2%; the relative standard deviations between laboratories were 6.4%, 4.3%, and 2.8%, respectively; the repeatability limits were. 0.5
Mg/m3, 0.9 mg/m3 and 2.0 mg/m3; reproducibility limits were 0.7 mg/m3, 1.3 mg/m3 and 2.3 mg/m3, respectively.
10.2 Accuracy
6 laboratories unified the basic fog (additional amounts of 0.35 mg, 1.00 mg and 1.40 mg) (calculated as NaOH)
The sample was tested for spiked recovery. The recoveries of spiked standards were 82.5%~96.5%, 90.1%~108% and 95%~
105%; the final values of the spiked recovery were 91.2% ± 10%, 98.2% ± 14% and 102% ± 8%, respectively.
11 Quality Assurance and Quality Control
11.1 Sampling Process Control
511.1.1 Regularly calibrate flow meters, pitot tubes, temperature sensors, etc.
11.1.2 The sampling nozzle should be inserted into the pipeline in the direction of the airflow. The sampling nozzle must be aligned with the airflow direction during sampling.
Over 10°. The velocity of the gas entering the sampling nozzle should be equal to the velocity of the flue gas at the sampling point, and the relative error should be within 10%.
11.1.3 The sampling rate of the sampling process is required to reach 1.0±0.1, otherwise it should be resampled.
11.2 blank
At least 2 blank samples of the same batch should be analyzed for each batch of samples. Blank cartridge ultrasonic extract or heated sodium in the leachate
The measured value of NaOH should be less than 1 mg/m3, otherwise it cannot be used.
11.3 Standard curve
A standard curve is required before each batch of samples is determined, and the correlation coefficient is greater than 0.999. Every 20 samples (or each sample)
(product) should have a standard curve intermediate concentration check point, the relative error between the measured value of the intermediate concentration check point and its concentration value should be
Within ±10%. Otherwise, the standard curve should be re-established.
11.4 Accuracy Control
At least 10% of certified standard samples or laboratory-manufactured quality control should be determined for every 20 samples (or each batch)
The sample, the test result of the certified standard sample shall be within the uncertainty range given by the laboratory, and the quality control sample prepared by the laboratory itself shall be
The recovery rate should be between 80% and 110%.
12 Waste treatment
The waste generated during the experiment should be collected and collected in a centralized manner according to relevant requirements.
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