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Stationary source emission-Determination of beryllium -Graphite
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HJ 684-2014
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Standard similar to HJ 684-2014 HJ 511 HJ 945.3 HJ 943 Basic data | Standard ID | HJ 684-2014 (HJ684-2014) | | Description (Translated English) | Stationary source emission-Determination of beryllium -Graphite | | Sector / Industry | Environmental Protection Industry Standard | | Regulation (derived from) | Ministry of Environmental Protection Notice No. 4 of 2014 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 684-2014: Stationary source emission-Determination of beryllium -Graphite---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.
(Stationary source emission - beryllium - Determination - graphite furnace atomic absorption spectrophotometry)
National Environmental Protection Standard of the People's Republic
Determination of enthalpy of fixed pollution source
Graphite furnace atomic absorption spectrophotometry
Stationary source emission-Determination of beryllium -Graphite
Oven atomic absorption spectrophotometric method
Published on January 13,.2014
2014-4-1 implementation
release
Ministry of Environmental Protection
Content
Preface II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 Interference and elimination 1
5 reagents and materials 1
6 Instruments and equipment 2
7 sample 2
8 Analysis steps.3
9 Calculation and representation of results. 3
10 precision and accuracy. 4
11 Quality Assurance and Quality Control..4
12 Notes. 4
Foreword
To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution
This standard is formulated to ensure human health and standardize the determination method of cesium in fixed pollution source exhaust gas.
This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of antimony in particulates in fixed source exhaust gases.
This standard is the first release.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. China Environmental Monitoring Center.
This standard is verified by. Anhui Environmental Monitoring Center, Chongqing Environmental Monitoring Center, Jiangsu Environmental Monitoring Center,
Henan Environmental Monitoring Center Station, Liaoning Provincial Environmental Monitoring Center Station, Nanjing Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on January 13,.2014.
This standard has been implemented since April 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Determination of enthalpy of fixed pollution sources - Graphite furnace atomic absorption spectrophotometric method
WARNING. Helium and its compounds are toxic and should be tested in a well ventilated environment.
1 Scope of application
This standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of antimony in fixed source exhaust gas.
This standard applies to the determination of helium in fixed source exhaust gas.
When the sampling volume is 0.5 m3 and the volume is 50 ml, the detection limit of 铍 is 0.03 μg/m3, and the lower limit is
0.12 μg/m3.
2 Normative references
The contents of this standard refer 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 373 Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Source Monitoring (Trial)
HJ/T 48 soot sampler technical conditions
3 Principle of the method
The quartz fiber filter cartridge is used to collect the particulate matter in the fixed pollution source exhaust gas, and is prepared into a solution by digesting with nitric acid-hydrogen peroxide.
The ruthenium in this solution is atomized in a graphite furnace atomizer, and the characteristic spectrum of the ground state ytterbium atom emitted to the hollow cathode lamp
The line (234.9 nm) produces absorption, and within a certain range, its absorbance value is linear with the mass concentration.
4 interference and elimination
1000 mg/L of copper and nickel in the sample solution does not interfere with the determination of strontium. 1000 mg/L of sodium and potassium will reduce the absorption of strontium from
As a result, the measured value is low. The addition of aluminum nitrate as a matrix modifier can effectively eliminate matrix interference.
5 reagents and materials
The reagents used in this standard are analytically pure reagents and deionized water or equivalent pure according to national standards unless otherwise stated.
Degree of water.
5.1 Hydrogen peroxide. w(H2O2) = 30%.
5.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 Nitric acid solution, 1 1.
5.4 Nitric acid solution, 1 99.
5.5 铍 standard stock solution. ρ (Be) = 1000 mg/L.
Accurately weigh 11.6060 g of barium sulfate (BeSO4), dissolve it with nitric acid solution (5.3) and dilute to 1000 ml. Transfer into poly
The vinyl plastic bottle is stored in a refrigerator and stored at least for one month. You can also purchase commercially available certified standard samples/objects
quality.
5.6 铍 standard intermediate solution. ρ (Be) = 10 mg/L
Accurately absorb 1.00ml of standard stock solution (5.5) in a 100ml volumetric flask, dilute to the mark with nitric acid solution (5.4), shake well.
Transfer to a polyethylene plastic bottle and store in a refrigerator for at least one month.
5.7 铍 standard use solution. ρ (Be) = 100 μg/L
Accurately absorb 铍 standard intermediate solution (5.6) 1.00 ml in a 100 ml volumetric flask, dilute to the mark with nitric acid solution (5.4), shake
uniform.
5.8 Aluminum nitrate solution (Al(NO3)3). ρ(Al(NO3)3) =1000 mg/L
Weigh 1.76 g of Al(NO3)3·9H2O, dissolve it with nitric acid solution (5.4), dilute to 1000 ml, and shake well.
5.9 99.999% high purity argon.
6 Instruments and equipment
Unless otherwise stated, Class A glassware in accordance with national standards was used for the analysis.
6.1 Graphite furnace atomic absorption spectrophotometer with background correction function.
6.2 graphite tube, pyrolytic coated graphite tube
6.3 铍 element hollow cathode lamp
6.4 Soot sampler, sampling flow rate is (5~80) L/min, other performance and technical indicators are in accordance with HJ/T 48.
6.5 quartz fiber filter cartridge
The cerium content is not more than 0.015 μg. The barrier efficiency of the particles having a particle diameter of more than 3 μm is not less than 99.9%.
6.6 Adjustable temperature electric heating plate, (40~200) °C...
6.7 Filter unit, 0.45 μm acetate or similar filter.
6.8 Teflon scissors.
6.9 Common instruments and equipment used in general laboratories.
7 samples
7.1 Sample collection
According to the relevant requirements of GB 16157, sample collection was performed by constant velocity sampling method.
7.2 Field blank
At least two batches of the same batch number filter cartridge are taken for each sampling, and taken to the sampling site as a blank sample on site.
7.3 Preservation of samples
After sampling, carefully remove the filter cartridge and fold the seal inward, put it back into the original filter cartridge box, and store it in a desiccator.
7.4 Preparation of samples
The filter cartridge was cut with Teflon scissors, placed in a 250 ml Erlenmeyer flask, wetted with a small amount of water, and added to 50 ml of nitrate.
Acid solution (5.3), 15 ml hydrogen peroxide (5.1), inserted into a small funnel, heated to a slight boiling on a hot plate for 2 h, to be cold
Then carefully add 5 ml of hydrogen peroxide (5.1), add a small amount of water if necessary, continue to boil for half an hour, cool and filter.
The filtrate was transferred to a beaker, and the conical flask, the filter residue and the filter flask were washed three times with a nitric acid solution (5.4), and the washing liquid and the filtrate were washed.
Combine and place on a hot plate to slightly boil to near dryness, then add 2 ml of nitric acid solution (5.3), heat to dissolve the residue, all turn
Move to a 50 ml volumetric flask, dilute to volume (V) with water, shake well, and test.
7.5 Preparation of laboratory blank samples
Take two blank cartridges of the same batch number and prepare laboratory blank samples according to 7.4 method.
8 Analysis steps
8.1 Graphite furnace atomic absorption spectrophotometer working conditions
According to the instrument manual, set the working conditions of the instrument. Table 1 and Table 2 can be used as reference for working conditions.
Table 1 Graphite furnace working conditions
Step drying 1 drying 2 ashing atomization removal
Temperature (°C) 85~150 150~500 1100 2300 2500
Heating time (s) 15 10 18 0.7 0.5
Hold time (s) 3 5 2 3 2
Argon flow rate (ml/s) 50 50 50 stop gas 50
Table 2 Atomic absorption spectrometer working conditions
Wavelength (nm) Slit (nm) Lamp Current (mA) Negative High Voltage (V) Measurement Mode Background Correction
234.9 1.0 5.0 300-400 Peak height Zeeman correction or xenon lamp correction
8.2 Calibration
Take 7 100 ml volumetric flasks and take the standard use solution (5.7) 0.00, 0.50, 1.00, 2.00, 3.00, 4.00, respectively.
5.00 ml, diluted to the mark with nitric acid solution (5.4), the standard series 铍 concentration is 0.00, 0.50, 1.00, 2.00, 3.00,
4.00, 5.00 μg/L.
Into the graphite tube, 20 μl of the standard solution and 5 μl of the aluminum nitrate solution (5.8) were injected. According to the selected atomic absorption
The operating conditions of the spectrophotometer were measured for absorbance one by one, and a calibration curve was drawn by absorbance versus radon concentration (μg/L).
Graphite furnace atomic absorption spectrophotometer with automatic dilution preparation calibration curve function with reference to the above standard concentration sequence
Calibration curve.
8.3 Determination
The concentration (ρ) of the sample (7.4) was determined and calculated according to the operating conditions of the instrument when the calibration curve was drawn. When the sample response value
When outside the upper limit of the calibration curve, dilute to a suitable multiple (f) with a nitric acid solution (5.4) to reduce the response.
Within the linear range of the calibration curve.
8.4 Laboratory blank test
Determine the concentration (ߩതതത) of the laboratory blank sample (7.5) by plotting the instrument operating conditions when plotted against the calibration curve.
9 Calculation and representation of results
9.1 Calculation of results
The concentration of cerium in the particulate matter of the fixed source was calculated by the following formula, μg/m3.
×−×=
ndV
ρ(Be) 0
Ρρ f
Where. ρ(Be)-the concentration of cesium in the exhaust gas particles of fixed pollution source, μg/m3
V—the volumetric volume of the sample, ml;
F——the dilution factor of the sample;
Vnd - sampling volume of dry flue gas in standard state (273 K, 101.325 kPa), m3.
9.2 Results representation
When the measured value is less than 1 μg/m3, the result retains two decimal places. When the measured value is greater than 1 μg/m3, the result is in three places.
The effect number is expressed in μg/m3.
10 Precision and accuracy
10.1 Precision
Six laboratories used simulated exhaust gas samples with a concentration of 0.100μg/m3, 0.200μg/m3, and 0.500μg/m3 (sampling)
Precision is measured in 0.5m3 volume.
The relative standard deviations in the experimental room were. 2.0% to 12.3%, 4.3% to 9.9%, and 3.2% to 18.2%;
The relative standard deviations between laboratories were. 18.4%, 16.2%, 18.6%;
The repeatability limit is. 0.017 μg/m3, 0.040 μg/m3, 0.126 μg/m3;
Reproducibility limits are. 0.049 μg/m3, 0.088 μg/m3, 0.253 μg/m3.
10.2 Accuracy
Six laboratories used a unified fly ash sample (without hydrazine) to simulate the actual sample for spiked recovery experiments. Weigh
0.1000g fly ash sample was added to the blank filter cartridge, and 0.050μg, 0.100μg and 0.250μg 铍 standard samples were added, then the standard was added.
When the degrees are 0.100μg/m3, 0.200μg/m3, 0.500μg/m3 (the sample volume is 0.5m3).
The recoveries of standard addition were. 88.2%~112.1%, 92.0%~105.3%, 83.1%~101.2%;
The final recoveries of the spiked recovery were. (99.0% ± 10.1%) 0.050, (97.0 ± 6.9%) 0.100, (95.9% ± 10.1%) 0.250.
11 Quality Assurance and Quality Control
11.1 At least two on-site blank samples should be made for each sampling. The concentration of radon in the blank sample should be lower than the lower limit of the method.
11.2 Each batch of samples (10 to 20 samples as a batch) should have at least two laboratory blanks, and the concentration of lanthanum in the blank sample
Should be lower than the lower limit of the determination of this method.
11.3 During the measurement process, the standard solution at the midpoint of the calibration curve concentration should be retested for every 10 samples measured. The measurement results
The relative deviation from the concentration value at this point on the calibration curve should not exceed ±10%. Otherwise, you should find out the reason and correct it.
The first 10 samples were re-measured after the instrument was stabilized.
11.4 Other quality assurance and quality control requirements and control indicators shall be implemented in accordance with the relevant provisions of HJ/T 373.
12 Precautions
12.1 When the sample solution is steamed to near dryness, the temperature should not be too high to avoid collapse.
12.2 The matrix improver aluminum nitrate solution cannot be added to the sample in advance, and must be injected into the graphite furnace atomizer separately to make the reaction
In the atomizer.
12.3 When the response of the sample solution is outside the upper limit of the calibration curve, dilute with a nitric acid solution (5.4) to make it ring
The value should be moved within the calibration curve.
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