HJ 543-2009_English: PDF (HJ543-2009)
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Stationary source emission. Determination of mercury. Cold atomic absorption spectrophotometry
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HJ 543-2009
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Standards related to: HJ 543-2009
| Standard ID | HJ 543-2009 (HJ543-2009) | | Description (Translated English) | Stationary source emission. Determination of mercury. Cold atomic absorption spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Classification of International Standard | 13.040.40 | | Word Count Estimation | 9,969 | | Date of Issue | 2009-12-30 | | Date of Implementation | 2010-04-01 | | Quoted Standard | GB/T 16157; HJ/T 373; GB/T 6682 | | Drafting Organization | Beijing Municipal Environmental Monitoring Center | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 74 of 2009 | | Summary | This standard specifies the determination of stationary source emissions of mercury cold vapor atomic absorption spectrophotometry. This standard applies to stationary source emission determination of mercury. |
HJ 543-2009
Stationary source emission.Determination of mercury.Cold atomic absorption spectrophotometry
National Environmental Protection Standard of the People's Republic
Determination of mercury in fixed pollution source
Cold atomic absorption spectrophotometry (provisional)
Stationary source emission-Determination of mercury
-Cold atomic absorption spectrophotometry
Released.2009-12-30
2010-04-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 74 of.2009
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve the lead gas of fixed pollution sources.
The four standards, such as the determination of flame atomic absorption spectrophotometry (tentative), are national environmental protection standards and are released.
The standard name and number are as follows.
I. Determination of lead in fixed pollution sources - Flame atomic absorption spectrophotometry (tentative) (HJ 538-2009);
2. Determination of lead in ambient air by graphite furnace atomic absorption spectrophotometry (tentative) (HJ 539-2009);
III. Determination of arsenic in ambient air and exhaust gases - Spectrophotometric method of silver diethyldithiocarbamate (interim) (HJ 540-2009);
4. Determination of gaseous arsenic in the production of yellow phosphorus - Determination of silver diethyldithiocarbamate spectrophotometry (interim) (HJ 541-2009);
V. Determination of mercury in ambient air - Enrichment of sulfhydryl cotton - Cold atomic fluorescence spectrophotometry (interim) (HJ 542-2009);
VII. Determination of Sulfuric Acid Fog of Fixed Pollution Sources by Ion Chromatography (Provisional) (HJ 544-2009);
VIII. Determination of gaseous total phosphorus in fixed pollution sources - Determination of quinolinol ketone capacity (provisional) (HJ 545-2009);
IX. Determination of Phosphorus Pentoxide in Ambient Air Ascorbic Acid Reduction - Molybdenum Blue Spectrophotometry (Provisional) (HJ 546-2009);
X. Determination of chlorine gas from fixed pollution sources, iodometric method (provisional) (HJ 547-2009);
XI. Determination of hydrogen chloride in fixed source pollution. Silver nitrate capacity method (provisional) (HJ 548-2009);
12. Determination of hydrogen chloride in ambient air and exhaust gas Ion chromatography (interim) (HJ 549-2009);
XIII. Determination of total cobalt in water quality 5-chloro-2-(pyridylazo)-1,3-diaminobenzene spectrophotometry (provisional) (HJ 550-2009);
14. Determination of Chlorine Dioxide in Water Quality Iodometric Method (Provisional) (HJ 551-2009).
The above standards have been implemented since April 1,.2010 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
Special announcement.
December 30,.2009
Content
Foreword..iv
1 Scope..1
2 Normative references..1
3 method principle..1
4 interference.1
5 Reagents and materials.1
6 instruments and equipment.2
7 samples. 2
8 Analysis steps..3
9 result calculation..3
10 Quality Assurance and Quality Control.3
Foreword
To protect the environment and protect people 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 Air Pollution
This standard is formulated for physical health and monitoring methods for monitoring mercury in waste gas from stationary sources.
This standard specifies the cold atomic absorption spectrophotometric method for the determination of mercury in exhaust gases from stationary sources.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard was drafted. Beijing Environmental Protection Monitoring Center.
This standard was approved by the Ministry of Environmental Protection on December 30,.2009.
This standard has been implemented since April 1,.2010.
This standard is explained by the Ministry of Environmental Protection.
Iv
Determination of mercury in fixed pollution sources - Cold atomic absorption spectrophotometric method (provisional)
Warning. Mercury and its compounds are very toxic and should be ventilated during operation; the mercury-containing exhaust gas after the reaction is discharged before discharge.
Adsorption with iodine-activated carbon to avoid contamination of the air; residual residue after detection should be properly and safely disposed.
1 Scope of application
This standard specifies the cold atomic absorption spectrophotometric method for the determination of mercury in exhaust gases from stationary sources.
This standard applies to the determination of mercury in fixed pollution source exhaust gas.
The detection limit of the method is 0.025 μg/25 ml. When the sampling volume is 10 L, the detection limit is 0.002 5 mg/m3.
Limited to 0.01 mg/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)
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle of the method
Mercury in the exhaust gas is absorbed by the acidic potassium permanganate solution and oxidized to form mercury ions, which are reduced to atomic mercury by stannous chloride.
The gas is blown from the solution into the mercury analyzer and measured by cold atomic absorption spectrophotometry.
4 interference
Organic substances such as benzene, acetone, etc. interfere with the determination.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. Experimental water, GB/T 6682, second grade.
5.1 Concentrated hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.2 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.3 Potassium permanganate (KMnO4). excellent grade pure.
5.4 Mercuric chloride (HgCl2). excellent grade.
5.5 Sulfuric acid solution. φ (H2SO4) = 10%.
Measure 10. 0 ml of sulfuric acid (5.2) into 100 ml of water.
5.6 Sulfuric acid solution. c (1/2 H2SO4) = 0.5 mol/L.
Add 6.9 ml of sulfuric acid (5.2) to 400 ml of water, cool and dilute to 500 ml with water.
5.7 Sulfuric acid solution. c(1/2 H2SO4) = 1.0 mol/L.
Add 13.8 ml of sulfuric acid (5.2) to 400 ml of water, cool and dilute to 500 ml with water.
5.8 Potassium permanganate solution. c (1/5KMnO4) = 0.1 mol/L.
Weigh 3.2 g of potassium permanganate (5.3), dissolve in water and dilute to 1 000 ml. After filtration, the filtrate was stored in a brown bottle for use.
5.9 Absorbent
Mix 0.1 mol/L potassium permanganate solution (5.8) with 10% sulfuric acid solution (5.5) in an equal volume and prepare before use.
5.10 Stannous chloride glycerol solution. w (SnCl2 · 2H2O) = 25%.
Weigh 25.0 g of stannous chloride (SnCl 2 · 2H 2 O) in a 150 ml beaker, add 10.0 ml of concentrated hydrochloric acid (5.1), stir and dissolve.
Add 90 ml of glycerin, cool and store in a brown bottle.
Note. The stannous chloride glycerol solution is poured into the mercury reaction bottle before use, and the background mercury is removed by blowing nitrogen gas until the mercury meter reading returns to zero.
5.11 Hydroxylamine hydrochloride solution. w (NH2OH·HCl) = 10%.
Weigh 10.0 g of hydroxylamine hydrochloride (NH2OH·HCl) dissolved in a small amount of water and diluted to 100 ml with water.
5.12 Mercury standard stock solution. ρ (Hg) = 1 000 μg/ml.
Weigh 0.135 4 g of mercury chloride (5.4), dissolve it in 0.5 mol/L sulfuric acid solution (5.6), and transfer it to a 100 ml volumetric flask to 0.5 mol/L.
The sulfuric acid solution (5.6) is diluted to the mark. This solution contains 1 000 μg of mercury per ml.
A commercially available certified standard solution can also be used as a standard stock solution for mercury.
5.13 Mercury standard intermediate. ρ (Hg) = 10.0 μg/ml.
Pipette 1.00 ml of the standard stock solution of mercury chloride (5.12), transfer it to a 100 ml volumetric flask, and dilute with 0.5 mol/l sulfuric acid solution (5.6).
To the mark, this solution is equivalent to 10.0 μg of mercury per milliliter.
5.14 Mercury standard use solution. ρ (Hg) = 1.00 μg/ml.
Before use, draw 10.00 ml of mercury chloride standard intermediate solution (5.13), transfer it to a 100 ml volumetric flask, and use 0.5 mol/L sulfuric acid solution.
(5.6) Dilute to the marking. This solution is equivalent to 1.00 μg of mercury per milliliter.
5.15 Iodine - activated carbon
Weigh 10 g of iodine (I2) and 20 g of potassium iodide (KI) in a beaker, then add.200 ml of distilled or deionized water to form a solution.
Then add about 100 g of activated carbon to the solution, stir vigorously until the solution is decolorized, then pour out the solution, and dry the activated carbon at 100-110 ° C.
Use in a desiccator.
5.16 Nitrogen (N2). purity φ (N2) = 99.999%.
Note. If air is used as the carrier gas, it should be purified by activated carbon.
6 Instruments and equipment
Unless otherwise stated, the analysis used a Class A glass instrument in accordance with national standards.
6.1 Flue gas sampler. The flow range is 0~1 L/min.
6.2 Large bubble absorption tube. 10 ml.
6.3 Cold Atomic Absorption Mercury Analyzer.
6.4 Mercury reaction bottle.
6.5 Mercury absorption tower. 250 ml glass drying tower filled with iodine-activated carbon (5.15). To ensure the effect of iodine-activated carbon, use 1 to 2
After the month, it should be replaced again.
7 samples
7.1 Sample collection
Flue gas sampling according to GB/T 16157. Large bubbles absorbed in series with 10 ml of absorbing liquid (5.9) in series on the sampling device
The tube was sampled at a flow rate of 0.3 L/min for 5 to 30 minutes.
Note. The rubber tube has adsorption to mercury, the sampling tube and the absorption tube are connected by polyethylene tube, and the interface is sealed with Teflon raw material tape; when the mercury concentration is high
Large impact absorbing sampling bottles can be used.
7.2 Field blank
Bring two large bubble absorbers with 10 ml of absorbing solution (5.9) to the sampling point, without connecting the flue gas sampler, and with the sample
Store and transport under the same conditions until sent to the laboratory for analysis. Care should be taken to prevent contamination during transportation.
7.3 Preservation of samples
After the sampling is finished, close the inlet and outlet of the absorption tube, transport it in the sample box, and take care to avoid the light. The sample should be analyzed as soon as possible after collection. If
Can not be measured in time, should be stored in the refrigerator at 0 ~ 4 ° C, measured within 5 days.
7.4 Preparation of samples
After sampling, the absorption liquid in the two absorption tubes is combined and transferred into a 25 ml volumetric flask, and the absorption tube is washed 1 to 2 times with the absorption liquid (5.9).
The washing solution was incorporated into a volumetric flask, diluted to the mark with an absorbent (5.9), and shaken.
7.5 Preparation of blank samples
A blank sample was prepared according to the preparation of the sample (7.4).
8 Analysis steps
8.1 Drawing of standard curves
8.1.1 Take 7 mercury reaction bottles and prepare a standard series of mercury according to Table 1.
Table 1 Mercury standard series
Bottle number 0 1 2 3 4 5 6
Mercury standard use solution/ml 0 0.10 0.20 0.40 0.60 0.80 1.00
Absorbent/ml 5.0 4.9 4.8 4.6 4.4 4.2 4.0
Mercury content/μg 0 0.10 0.20 0.40 0.60 0.80 1.00
8.1.2 Shake each bottle for 10 min, and add 10% hydroxylamine hydrochloride solution (5.11) until the purple color and the precipitate completely faded.
8.1.3 Add 1.0 mol/L sulfuric acid solution (5.7) to 25 ml to the bottle, and add 25% stannous chloride glycerol solution (5.10) 3.0 ml.
Cover the stopper tightly.
8.1.4 Determine according to the mercury meter operating procedure, draw a standard curve of the mercury content (μg) with the response value of the instrument, and calculate the standard curve.
Linear regression equation.
Note. Temperature has an influence on the sensitivity of the measurement. When the room temperature is lower than 10 °C, it is not conducive to the volatilization of mercury, and the sensitivity is low. The ambient temperature of the operation room should be increased.
Ways to improve the gasification efficiency of mercury. Also pay attention to the consistency of the standard solution and the sample temperature.
8.2 Preparation of samples
Pipette an appropriate amount of the sample into a mercury reaction bottle and dilute to 5.0 ml with an absorbent (5.9). A blank sample was prepared by the same method.
8.3 Determination of sample
The sample and blank samples were measured according to the drawing procedure of the standard curve (8.1.2 to 8.1.4), and the response value of the instrument was recorded.
9 Calculation of results
Based on the measured values of the sample and the blank sample, the mercury content in the sample and the blank sample was calculated from the linear regression equation. By
(1) Calculate the mass concentration (μg/m3) of mercury in the exhaust gas of a fixed source.
ρ(Hg)= 1 0
Nd a
WWV
VV
T− × (1)
Where. ρ(Hg)--the mass concentration of mercury in the fixed source exhaust gas, μg/m3;
W1--the mercury content in the sample, μg;
W0--the mercury content in the blank sample, μg;
Va--the volume of the sample solution taken during the measurement, ml;
Vt--the total volume of the sample solution, ml;
Vnd - the sampling volume of dry gas in the standard state (101.325 kPa, 273 K), m3.
10 Quality Assurance and Quality Control
10.1 Quality Assurance and Quality Control According to the Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Sources (Trial) (HJ/T 373)
The regulations are enforced.
10.2 All glassware should be soaked in 10% nitric acid solution overnight or soaked in (1 1) nitric acid solution for 40 min before use.
Mercury adsorbed on the wall.
10.3 A reagent blank test must be performed before the sample is measured. The blank value should not exceed 0.005 μg mercury.
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