HJ 540-2016 (HJ540-2016) & related versions
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Stationary source emission - Determination of arsenic- Silver diethyldithiocarbamate spectrophotometric method
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HJ 540-2016
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HJ 540-2016
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| HJ 540-2009 | English | 359 |
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Ambient air and waste gas. Determination of arsenic. Silver diethyldithiocarbamate spectrophotometric method
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HJ 540-2016: PDF in English
HJ 540-2016
(Determination of arsenic in fixed sources - Silver diethyldithiocarbamate spectrophotometric method)
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 540-2009
Determination of arsenic in fixed source
Silver dimethyldithiocarbamate spectrophotometric method
Stationary source emission - Determination of arsenic-Silver
Diethyldithiocarbamate spectrophotometric method
2016-07-26 release
2016-10-01 implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
Interference and elimination
5 reagents and materials 2
6 instruments and equipment 3
7 Sample 3
8 Analysis steps
The results are calculated and expressed
10 Precision and Accuracy
Quality assurance and quality control
12 Waste treatment
Preface
In order 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,
Environment, the protection of human health, regulate the fixed source of waste gas in the form of particulate matter and the determination of arsenic and its compounds,
Develop this standard.
This standard specifies the determination of fixed sources of waste gas in the form of particulate matter and its compounds of diethyldisulfide
Substituted carbamate spectrophotometric method.
This standard is for the determination of "ambient air and waste arsenic, silver diethyldithiocarbamate spectrophotometric (provisional)"
(HJ 540-2009).
This standard was first published in.2009, the original standard drafting unit for the Beijing Environmental Protection Monitoring Center. This is the first
The main contents of the amendment are as follows.
- According to the scope of application of the standard, the original standard name "Ambient air and arsenic determination of diethyldithioamino
Formic acid silver spectrophotometric method (tentative) "modified to" fixed source of waste gas arsenic determination of diethyldithiocarbamate silver
Spectrophotometry";
- the contents of the ambient air and so on have been removed from the original standard;
- Based on the experimental results, the detection limit was revised from 0.00 μg/m3 to 0.004 mg/m3 and the lower limit of determination was 3.5 μg/m3
Revised to 0.016 mg/m3;
- the collection of samples and the preparation of samples and other content has been revised;
- increased precision and accuracy and other content;
- improve the quality assurance and quality control content;
- Increased waste disposal.
Since the implementation of the standard date, the original standard "Determination of ambient air and arsenic arsenic diethyldithiocarbamate
Photometric method (provisional) "(HJ 540-2009) abolished.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The drafting of this standard. Beijing Environmental Protection Monitoring Center, Beijing Xicheng District Environmental Protection Monitoring Station.
The standard verification unit. Yunnan Honghe State Environmental Monitoring Station, Beijing Changping District Environmental Protection Monitoring Station, Beijing Feng
Taiwan Environmental Protection Monitoring Station, Beijing Xicheng District Environmental Protection Monitoring Station, Beijing China measured North Detection Technology Co., Ltd.
The environmental protection department of this standard approved on July 26,.2016.
This standard has been implemented since October 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of arsenic in fixed source
Silver dimethyldithiocarbamate spectrophotometric method
Warning. arsine is a highly toxic gas, before the test must check whether the arsine generator is connected to prevent leakage or reaction
The bottle was disintegrated. The reaction shall be carried out in a fume hood, and the operator shall wear protective equipment.
1 Scope of application
This standard specifies the determination of fixed sources of waste gas in the form of particulate matter arsenic and its compounds diethyldithio
Silver phthalate spectrophotometric method.
This standard is applicable to the determination of arsenic and its compounds in the form of particulate matter in fixed waste gas.
When the sampling volume is 0.4 m3 (standard state), the volume of the volume is 50.0 ml, the detection limit of this method is 0.004 mg/m3,
The lower limit of determination is 0.016 mg/m3 (both in As).
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is applicable
In this standard.
Determination of particulate matter and sampling method of gaseous pollutants in exhaust gas of fixed pollution sources GB/T 16157
HJ/T 373 fixed pollution source monitoring quality assurance and quality control technical specifications (Trial)
HJ/T 48 smoke and dust sampler technical conditions
HJ 77.2 Ambient air and exhaust dioxins Determination of isotope dilution High resolution gas chromatography - High resolution mass spectrometry
3 Principle of the method
Using quartz fiber filter cartridge to collect fixed sources of waste gas containing arsenic particles, nitric acid, sulfuric acid, hydrogen peroxide digestion after preparation
The solution of pentavalent arsenic in this solution was reduced to trivalent arsenic with potassium iodide (KI) and stannous chloride (SnCl2 · 2H2O)
Zinc particles and acid, resulting in new ecological hydrogen, the trivalent arsenic further reduced to gaseous arsine (AsH3), and dissolved in trichloromethyl
(CH5H10AgNS2) in the alkylene chloride (CHCl3) to form a magenta complex at 510 nm
Absorbance measured at the wavelength, within a certain range of its absorbance and arsenic content is proportional to.
4 interference and elimination
Mercury, manganese, copper, nickel, cobalt, lead and iron, 100 μg or less of cadmium and antimony below 50 μg, bismuth below 30 μg,
20 μg or less of chromium, 10 μg of the following selenium, no significant interference with the determination. When the content of antimony in the sample is greater than 50 μg, the interference
Arsenic determination, adding 3 ml of stannous chloride and 5 ml of potassium iodide solution, can inhibit 300 μg of antimony interference. Sulfide interference,
Can be removed with lead acetate cotton.
5 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The experimental water is a freshly prepared deionized water
Or distilled water.
5.1 Arsenic free zinc tablets. 10 mesh to 20 mesh.
Note 1. The rate of occurrence of arsine is affected by the size, surface state and dosage of the zinc particles, the reaction acidity and the temperature. Zinc tablets to 10 to 20
The purpose of the surface rough zinc particles to restore the high efficiency, the amount of 3 g ~ 5 g between the effect is better.
5.2 Potassium iodide (KI).
5.3 Stannous chloride (SnCl2 · 2H2O).
5.4 Lead acetate [Pb (CH3COO) 2].
5.5 Diethyldithiocarbamate (C5H10AgNS2).
5.6 Arsenic trioxide (As2O3). Reference reagent.
Before use, in 105 ℃ ~ 110 ℃ bake 2 h, stored in the dryer cooling, spare.
5.7 Sodium hydroxide (NaOH).
5.8 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.9 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.10 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.11 Trichloromethane (CHCl3).
5.12 Triethanolamine [(HOCH2CH2) 3N].
5.13 Hydrogen peroxide. ω (H2O2) = 30%, excellent grade pure.
5.14 sulfuric acid solution. 1 1.
Prepared with sulfuric acid (5.9).
5.15 Potassium iodide solution. ρ (KI) = 150 g/L
Weigh 15 g of potassium iodide (5.2), dissolved in water and diluted to 100 ml beaker.
5.16 Stannous chloride solution. ρ (SnCl2 · 2H2O) = 400 g/L.
Weigh 48 g of stannous chloride (5.3), add 50 ml of hydrochloric acid (5.10), dissolve it by heating, and then diluted with water to 100 ml
Beaker, ready for use.
5.17 lead acetate solution. ρ [Pb (CH3COO) 2] = 100 g/L.
Weigh 10 g of lead acetate (5.4), dissolve in water and dilute to 100 ml beaker.
5.18 Silver diethyldithiocarbamate Absorbate. ω (C5H10AgNS2) = 0.25%.
Weigh 1.25 g of silver diethyldithiocarbamate (5.5), add 100 ml of trichloromethane (5.11) and 4 ml of tri
Alcohol (5.12) was stirred and diluted to 500 ml with trichloromethane (5.11), shaken, left overnight, filtered with absorbent cotton
In the brown reagent bottle, in the 4 ℃ below the cold, dark can be stored for 3 months.
5.19 Sodium hydroxide solution. ω (NaOH) = 40%.
Weigh 40 g of sodium hydroxide (5.7), dissolve with water and dilute to 100 ml beaker.
5.20 arsenic standard stock solution. ρ (As) = 1.00 mg/ml.
Accurately weigh 0.0660 g (accurate to 0.0001 g) arsenic trioxide (5.6), add 10 ml of sodium hydroxide solution (5.19),
Dissolved in heat. The whole volume into the 100 ml volumetric flask, dilute the volume to the mark with water. Store in a brown reagent bottle at 4 ° C or lower
Refrigerated, sealed for 3 months. You can also purchase commercially available certified materials.
5.21 arsenic standard use of liquid. ρ (As) = 1.00 μg/ml.
Arsenic standard stock solution (5.20) placed in room temperature, diluted with water preparation, temporary with the allocation.
5.22 lead acetate
10 g of absorbent cotton immersed in 100 ml of lead acetate solution (5.17), 30 min after the removal, at room temperature to dry, dark
Preserved in the grinding glass bottles, the preservation period of 1 year.
5.23 quartz fiber filter cartridge
Should be pre-baked in the muffle furnace at 300 ℃ for 3 h, placed in a dryer to cool to room temperature. The arsenic in the digestion of the blank filter cartridge
The amount of not more than 1.3 μg. The particle size of particles with particle size greater than 0.3 μm is not less than 99.9%.
6 instruments and equipment
Unless otherwise stated, all Class A glass gauges conforming to national standards are used for analysis.
6.1 dust sampler. sampling flow range 5 L/min ~ 80 L/min, other performance and technical indicators in line with the provisions of HJ/T 48.
6.2 Visible Spectrophotometer. 10 mm cuvette.
6.3 adjustable thermoelectric plate. 40 ℃ ~.200 ℃.
6.4 polytetrafluoroethylene scissors.
6.5 arsine generation and absorption device. see Figure 1, airway and absorption tube before use in the application of anhydrous ethanol and experimental water followed
Cleaning, drying after use.
1-absorbent tube (inner diameter 8mm, 5ml); 4-acetate lead cotton filter
Figure 1 arsine generation and absorption device
6.6 Ultrasonic scrubber. ultrasonic frequency range of 30 KHz ~ 80 KHz.
6.7 Common laboratory equipment and equipment.
7 samples
7.1 Collection of samples
In accordance with the relevant provisions of GB/T 16157 implementation. Place the sampler with the quartz fiber filter cartridge into the sampling point in the exhaust cylinder
Constant speed sampling. Select the appropriate sampling time according to the concentration of arsenic, sample for 1 hour, or at 1 hour intervals
Collected three to four samples, while measuring temperature, pressure and other parameters. After sampling, carefully remove the cartridge, the seal inward
Folded, put back into the original filter box. Samples of particulate matter were collected using a soot sampler with a total sample volume of not less than 0.4 m3
(Standard state).
When the flue gas temperature is higher than 100 ℃, should take the cooling measures, so that the flue gas into the filter before the temperature is below 100 ℃, the specific side
The reference can be made to HJ 77.2.
7.2 Preservation of samples
The collected samples should be stored in a desiccator and completed within 7 days.
7.3 Preparation of samples
Use a polytetrafluoroethylene scissors (6.4) to cut the filter sample into flakes (do not shake off the dust), place it in a.200 ml Erlenmeyer flask,
Add 20 ml water infiltration. Adding 20 ml of nitric acid (5.8), 4 ml of sulfuric acid (5.9) and 2 drops to 3 drops of hydrogen peroxide (5.13)
Bottle into the glass funnel, heated in the hot plate (6.3) to the state of micro-boiling to maintain 2 h ~ 3 h, remove the funnel, with the appropriate amount of experiment
Rinse the funnel with water to the conical flask and continue heating in the slightly boiling state until the solution is near dry and allowed to cool. Add to the conical flask
25 ml of water (to be immersed in the sample), placed in the ultrasonic scrubber (6.6) for 5 min, remove the conical flask, with medium-speed quantitative filter
Paper filter; this step (plus 25 ml of water, ultrasound and filtration) repeated 5 times to 6 times. Combine the filtrate in a beaker and place it in electricity
Hot plate (6.3) to drain nitric acid until the solution remains about 4 ml. After cooling, add a small amount of experimental water to wash the beaker
Wall, the whole solution will be transferred to the arsenide bottle (6.5), add water to 50 ml, shake.
Note 2. nitric acid, sulfuric acid, hydrogen peroxide digestion of the sample, the organic matter must be completely decomposed, otherwise the results are low. The content of organic matter in the sample is higher than that in the sample
For a long time, should be added again hydrogen peroxide heating digestion to precipitate into gray, and the liquid level is calm, no longer produce nitrogen oxide brown smoke so far. Together
And then the filtrate must be evaporated to produce white smoke to drive nitric acid, otherwise the addition of zinc particles will produce brown gas, resulting in measurement failure, in case of
Resampling analysis.
7.4 Preparation of blank sample
7.4.1 Preparation of laboratory blanks
Take the same batch of filter cartridges and prepare a laboratory blank sample according to the same procedure as for sample preparation (7.3).
7.4.2 Preparation of full program blank samples
Each sampling at least take the same batch of blank filter cartridge two, to the sampling site as a whole program blank sample. Follow the sample with
Preparation of the procedure (7.3) The same procedure to prepare a full program blank sample.
8 Analysis steps
8.1 Calibration curve
8.1.1 Take 7 hydrogen arsenic vials, add 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 10.00 ml, 15.00 ml
And 25.00 ml of arsenic standard using liquid (5.21), add 7 ml of sulfuric acid solution (5.14), add water to 50 ml, then add 5 ml
Potassium iodide solution (5.15) and 3 ml stannous chloride solution (5.16), shake and let stand for 15 min. This standard series of arsenic content points
Do not be 0.00 μg, 1.00 μg, 3.00 μg, 5.00 μg, 10.0 μg, 15.0 μg, 25.0 μg.
8.1.2 Add 3 g to 4 g of arsenic-free zinc pellets (5.1) to solution (8.1.1) and immediately with argon with lead acetate (5.22)
The tube was connected to an absorption tube containing 5.0 ml of silver diethyldithiocarbamate absorption solution (5.18). After 1 h of reaction, the absorption was removed
Tube, along the airway wall by adding trichloromethane (5.11) and fixed to the absorption tube 5.0 ml scale, to be measured.
Note 3. High temperature in summer, too fast response, incomplete absorption, the results are low. If the room temperature is higher than 30 ℃, the bottle can be placed in the ice bath
cool down.
8.1.3 at the wavelength of 510 nm, with 10 mm cuvette to chloroform (5.11) as a reference, measured absorbance to arsenic
Content (μg) for the abscissa, absorbance value for the vertical axis, draw the calibration curve.
8.2 Determination of sample
Add 5 ml of potassium iodide solution (5.15) and 3 ml of stannous chloride solution (5.16) to the sample (7.3) and shake well. Stand still
After 15 min, the absorbance of the sample was measured according to the same procedure (8.1.2 to 8.1.3) as the plot of the calibration curve.
8.3 Determination of blank sample
The laboratory blank sample (7.4.1) and the whole program blank sample (7.4.2) were measured in the same manner as in the determination of the sample (8.2)
Of the absorbance.
9 Results calculation and representation
9.1 Results calculation
Calculate the concentration of arsenic in the particulate matter of the fixed source of pollution according to the formula (1), mg/m3.
0
Nd
AA a
As
B V 1000
(1)
Where the concentration of arsenic in the particulate matter of the fixed source (in As), mg/m3;
A - the absorbance of the sample;
0A - absorbance of laboratory blank samples;
A - the intercept of the calibration curve;
B - the slope of the calibration curve;
NdV - the sampling volume of the dry flue gas under the standard state (273 K, 101.325 kPa), m
3.
9.2 The result is shown
When the measured value is less than 0.1 mg/m3, the result is three after the decimal point; when the measured value is greater than or equal to 0.1 mg/m3,
The result retains three significant digits.
10 precision and accuracy
10.1 Precision
(5.00 μg/50 ml, 10.00 μg/50 ml and 15.00 μg/50 ml) in the three laboratories
A standard blank filter cartridge was loaded with 6 samples in parallel. The relative standard deviations in the laboratory were 2.8% ~ 4.6%
1.1% ~ 6.8% and 1.1% ~ 7.5% respectively. The relative standard deviations were 7.6%, 2.7% and 1.2%, respectively. The repeatability limits were
0.49 μg/50 ml, 1.3 μg/50 ml and 1.6 μg/50 ml, respectively. The reproducibility limits were 1.1 μg/50 ml, 1.4 μg/50 ml and 1.5 μg/50
Ml.
10.2 Accuracy
(5.00 μg/50 ml, 10.00 μg/50 ml and 15.00 μg/50 ml) in the three laboratories
A standard blank filter cartridge was loaded with 6 samples in parallel. The relative errors in the laboratory were -19.0% -0.4%
-5.1% ~ -1.0% and -2.9% ~ 0.3%; the relative error of the final value were -4.6% ± 14.5%, -1.4% ± 5.4%
-0.9% ± 2.4%.
11 quality assurance and quality control
11.1 Each batch of samples should be at least two laboratory blanks and two full program blanks, the determination of the results should be lower than the lower limit of determination.
Otherwise, look for the cause, re-sampling analysis.
11.2 The calibration curve shall be plotted for each analysis, and the correlation coefficient of the calibration curve should be greater than or equal to 0.999.
11.3 Other quality assurance and quality control shall comply with the requirements of HJ/T 373 and shall be avoided by finger touch during sampling and analysis
Filter to prevent contamination.
12 Waste treatment
The waste liquid produced in the experiment should be collected collectively in a covered container and labeled and labeled.
Line processing.
......
| Standard ID | HJ 540-2016 (HJ540-2016) | | Description (Translated English) | Stationary source emission - Determination of arsenic- Silver diethyldithiocarbamate spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 10,187 | | Date of Issue | 2016-07-26 | | Date of Implementation | 2016-10-01 | | Older Standard (superseded by this standard) | HJ 540-2009 | | Regulation (derived from) | Ministry of Environmental Protection Notice No.52 of 2016 |
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