HJ 538-2009_English: PDF (HJ538-2009)
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Stationary source emission. Determination of lead. Flame atomic absorption spectrometry
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HJ 538-2009
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Standards related to: HJ 538-2009
| Standard ID | HJ 538-2009 (HJ538-2009) | | Description (Translated English) | Stationary source emission. Determination of lead. Flame atomic absorption spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Word Count Estimation | 8,880 | | 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 lead by flame atomic absorption spectrophotometry. This standard applies to stationary source emissions Determination of lead. | HJ 538-2009
Stationary source emission.Determination of lead.Flame atomic absorption spectrometry
National Environmental Protection Standard of the People's Republic
Determination of lead in fixed pollution source
Flame atomic absorption spectrophotometry (provisional)
Stationary source emission-Determination of lead
-Flame atomic absorption spectrometry
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.
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);
6. Determination of mercury in fixed pollution sources - Cold atomic absorption spectrophotometry (provisional) (HJ 543-2009);
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 and elimination.1
5 Reagents and materials.1
6 instruments and equipment.2
7 samples. 2
8 Analysis steps..2
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 the health monitoring and monitoring methods for the determination of lead in waste gas from fixed sources.
This standard specifies the flame atomic absorption spectrophotometric method for the determination of lead in exhaust gas 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 lead in fixed pollution source
Flame atomic absorption spectrophotometry (provisional)
1 Scope of application
This standard specifies the flame atomic absorption spectrophotometric method for the determination of lead in exhaust gas from stationary sources.
This standard applies to the determination of lead in fixed source pollution.
The detection limit of the method is 5 μg/50 ml sample solution. When the sampling volume is 400 L, the detection limit is 0.013 mg/m3, and the lower limit of determination is
0.052 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
The exhaust gas sample is collected by a quartz fiber filter cartridge, digested to prepare a sample solution, and the lead solution in the sample solution is determined by an atomic absorption spectrophotometer.
concentration.
4 interference and elimination
Fe3, A13, Be3, Cr3, Cd2, Cu2, Zn2, Co2, Hg2, Sn2, Mn2, Mg2, Ag over 100 times lead
The plasma does not interfere with the measurement and SiO32− is slightly disturbed. Na, K, and Ca2 are slightly sensitized. When the concentration is high, the dilution method can be used.
Eliminate interference.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis; experimental water, GB/T 6682, grade 2.
5.1 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.2 Perchloric acid. ρ (HClO4) = 1.67 g/ml, excellent grade pure.
5.3 Hydrogen peroxide. w (H2O2) = 30%, excellent grade pure.
5.4 Nitric acid solution. φ (HNO3) = 1%.
Formulated with nitric acid (5.1).
5.5 Nitric acid solution. 1 1.
Formulated with nitric acid (5.1).
5.6 Lead standard stock solution. ρ (Pb) = 1.00 mg/ml.
Weigh 0.500 0 g of metal lead (99.99%) in a 100 ml beaker and dissolve it with 15 ml of (1 1) nitric acid solution (5.5). After cooling,
Transfer to a 500 ml volumetric flask and dilute to the mark with water.
Commercially available certified standard solutions can also be used as lead standard stock solutions.
5.7 Lead standard use solution. ρ (Pb) = 100 μg/ml.
The lead standard stock solution (5.6) was diluted with 1% HNO3 (5.4) to a standard stock solution containing 100 μg lead per ml.
5.8 Acetylene. The purity is not less than 99.6%.
6 Instruments and equipment
Unless otherwise stated, Class A glassware in accordance with national standards was used for the analysis.
6.1 Smoke sampler. The flow range is 5~50 L/min.
6.2 Quartz fiber filter cartridge.
Note. If the filter cartridge blank value is high, it can be soaked with hot (1 1) nitric acid solution (5.5) for about 3 h before use (can not be boiled, so as not to damage the filter cartridge). From acid
After taking out, soak it in water for 10 min, remove it with water and wash it to near neutrality. After drying, it can be used.
6.3 Atomic absorption spectrophotometer.
6.4 Electric heating plate.
7 samples
7.1 Sample collection
Sample collection was performed in accordance with GB/T 16157. When the temperature is below 400 °C, it is sampled at the same speed in the pipeline. When the temperature is higher than 400 ° C, lead
In the presence of gas, the exhaust gas should be led out of the pipeline to lower the temperature to below 400 °C, and sample at a constant flow of 20 L/min for 10 to 30 minutes.
7.2 Preservation of samples
After the sample of the filter cartridge is collected, the seal is folded inward, placed vertically in the original sampling box, and placed in a desiccator for storage.
7.3 Preparation of samples
Cut the filter cartridge into small pieces, place in a 250 ml Erlenmeyer flask, add (1 1) nitric acid solution (5.5) 50 ml and 30% hydrogen peroxide (5.3)
15 ml immersion sample filter cartridge, the bottle mouth was inserted into a small funnel, heated to a slight boiling on the hot plate, and kept slightly boiling for 2 h. Carefully add 30% after cooling
Hydrogen peroxide (5.3) 5 ml, if necessary, add a small amount of water, then heat on a hot plate to a slight boiling, keep boiling for 1 h. Filter after cooling,
The filtrate was filtered into a beaker, and the conical flask and the filter residue were washed three times with water, and the washing liquid was combined with the filtrate. Place the beaker containing the filtrate on the hot plate
On the top, the filtrate is steamed to near dry (the evaporation temperature should not be too high to avoid splashing), then add (1 1) nitric acid solution (5.5) 2 ml, heat to make
The residue was dissolved. After cooling, the solution was transferred to a 50 ml volumetric flask and diluted with water to the mark.
7.4 Preparation of blank samples
Take two blank cartridges of the same batch number, and simultaneously process the sample to prepare a blank sample.
8 Analysis steps
8.1 Atomic absorption spectrophotometer working conditions
Instrument parameters can be selected by referring to the instruction manual. The conditions and parameters listed below are for reference.
Wavelength. 283.3 nm; slit width. 0.8 nm; lamp current. 5 mA; flame type. air-acetylene; gas flow. acetylene
2.1 L/min, air 8.0 L/min; burner height. 10.0 cm.
8.2 Drawing of standard curve
8.2.1 Preparation of standard solutions
Take 7 50 ml volumetric flasks and prepare lead standard series according to Table 1. Dilute to the mark with 1% nitric acid solution (5.4) and shake well.
Table 1 Lead Standard Series
Bottle number 0 1 2 3 4 5 6
Lead standard use solution/ml 0 0.50 1.00 2.00 3.00 4.00 5.00
Lead concentration/(μg/ml) 0.00 1.00 2.00 4.00 6.00 8.00 10.0
8.2.2 Drawing a standard curve
The absorbance of the lead standard series is determined according to the selected instrument operating conditions, and the linear regression equation of the standard curve is calculated.
8.3 Preparation of samples
Take an appropriate amount of the sample solution in a 50 ml volumetric flask and dilute to the mark with a 1% nitric acid solution (5.4). A blank sample was prepared by the same method.
8.4 Determination of sample
The absorbance of the sample and the blank sample was determined by the working conditions of the instrument plotted according to the standard curve.
9 Calculation of results
According to the measured absorbance value, the concentration of lead in the sample and the blank sample was calculated from the linear regression equation, and the solid was calculated by the formula (1).
The concentration of lead in the exhaust gas of the pollution source.
ρ (Pb)= 1 0 t
Nd a
( ) 50 V
VV
ρ ρ− × × (1)
Where. ρ(Pb)--the mass concentration of lead in the fixed source exhaust gas, mg/m3;
Ρ1-- the concentration of lead in the sample solution, μg/ml;
Ρ0--the average value of lead mass concentration in the blank sample, μg/ml;
50--sample solution volume, ml;
Vt--the total volume of the sample solution, ml;
Va--the volume of the sample solution taken during the measurement, ml;
Vnd - the sampling volume of dry gas in the standard state (101.325 kPa, 273 K), L.
10 Quality Assurance and Quality Control
Execute according to the relevant regulations of HJ/T 373.
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