HJ 549-2009_English: PDF (HJ549-2009)
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Ambient air and waste gas. Determination of hydrogen chloride. Ion chromatography
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HJ 549-2009
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| HJ 549-2016 | English | 279 |
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Ambient air and stationary source emissions. Determination of hydrogen chloride. Ion chromatography
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HJ 549-2016
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Newer version: HJ 549-2016 Standards related to: HJ 549-2016
| Standard ID | HJ 549-2009 (HJ549-2009) | | Description (Translated English) | Ambient air and waste gas. Determination of hydrogen chloride. Ion chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 9,926 | | Date of Issue | 2009-12-30 | | Date of Implementation | 2010-04-01 | | Quoted Standard | GB/T 16157; HJ/T 194; 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 ambient air and emissions of hydrogen chloride ion chromatography. This standard applies to HCl in ambient air and exhaust gas measurement. | HJ 549-2009
Ambient air and waste gas.Determination of hydrogen chloride.Ion chromatography
National Environmental Protection Standard of the People's Republic
Determination of ambient air and exhaust gas hydrogen chloride
Ion chromatography (interim)
Ambient air and waste gas-Determination of hydrogen chloride
-Ion chromatography
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);
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);
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 Reagents and materials.1
5 instruments and equipment. 2
6 samples. 2
7 Analysis steps..3
8 result calculation..3
9 Quality Assurance and Quality Control 4
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 established for the health monitoring and regulation of hydrogen chloride in air and exhaust gases.
This standard specifies ion chromatography for the determination of hydrogen chloride in air and exhaust gases.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. 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 ambient air and exhaust gas hydrogen chloride
Ion chromatography (interim)
1 Scope of application
This standard specifies ion chromatography for the determination of hydrogen chloride in ambient air and exhaust gases.
This standard applies to the determination of hydrogen chloride in ambient air and exhaust gases.
For organized exhaust emissions, the detection limit of this method is 1 μg/50 ml. When the sampling volume is 10 L, the detection limit is 0.5 mg/m3.
The lower limit of determination is 2 mg/m3.
For ambient air, the detection limit of this method is 0.2 μg/10 ml. When the sampling volume is 60 L, the detection limit is 0.003 mg/m3.
The lower limit is 0.012 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 194 Technical Specifications for Manual Air Quality Monitoring
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 hydrogen chloride gas is absorbed by the alkaline absorption liquid to form a chloride. Inject the sample into the ion chromatograph to separate the chloride ions, depending on the retention time
Qualitative, quantitative response.
4 reagents and materials
Analytically pure reagents in accordance with national standards, deionized water, GB/T 6682, grade 2, were used for analysis unless otherwise stated.
4.1 Absorbent. potassium hydroxide-sodium carbonate solution, c(KOH)=0.089 mol/L, c(Na2CO3)=0.12 mol/L.
Weigh 5.0 g of potassium hydroxide and 12.72 g of anhydrous sodium carbonate, dissolve in water, and dilute to 1 000 ml. Also according to the instrument model and chromatography
The column is configured using conditions.
4.2 Eluent. It is prepared from 1 part of absorption liquid and 49 parts of water.
4.3 Potassium chloride standard stock solution. ρ (Cl−)=1 000 μg/ml.
Weigh 2.103 g of potassium chloride (reference reagent, dried at 110 °C for 2 h), dissolve and transfer to a 1 000 ml volumetric flask, use eluent (4.2)
Dilute to the mark and shake well. It can also be configured using a certified standard solution. Potassium chloride stock solution can be stored at 0~4 °C for 3 months.
4.4 Potassium chloride standard use solution I. ρ (Cl−) = 100 μg/ml.
Pipette 10.00 ml of potassium chloride standard stock solution (4.3), place in a 100 ml volumetric flask, and dilute to the mark with eluent (4.2).
Shake well and use it now.
4.5 Potassium chloride standard use solution II. ρ (Cl−) = 10 μg/ml.
Pipette 10.00 ml of potassium chloride standard stock solution (4.3), place in a 1 000 ml volumetric flask, and dilute to the mark with eluent (4.2).
Shake well and use it now.
The above reagents are stored in plastic bottles.
4.6 0.45 μm acetate fiber microporous membrane.
4.7 0.3 μm acetate fiber microporous membrane.
5 Instruments and equipment
Unless otherwise stated, the analysis uses a Class A glass gauge that complies with national standards.
5.1 Porous glass plate absorption tube. 10 ml.
5.2 Large bubble absorption tube. 10 ml.
5.3 Flue gas sampler. flow range, 0 ~ 1 L/min.
5.4 Air sampler. flow range, 0 ~ 1 L/min.
5.5 Sampling tube. It is made of hard glass or fluororesin, with appropriate size of pipe material, and should be insulated with heat that can be heated above 120 °C.
Jacket.
5.6 Teflon filter holder. The size matches the filter (4.7).
5.7 Connecting pipe. Use Teflon hose or silicone rubber tube lined with PTFE film.
5.8 Ion Chromatograph. Contains a conductivity detector and an anion column.
5.9 Vacuum filtration unit.
5.10 Teflon or polyethylene plastic bottles.
5.11 with colorimetric tube. 10 ml, 50 ml.
6 samples
6.1 Sample Collection
6.1.1 Organized emissions
Sampling shall be carried out in accordance with the relevant provisions of GB/T 16157. Two porous cells each containing 5.0 ml of absorbing solution (4.1) in series on the sampling device
The plate absorption tube was sampled at a flow rate of 0.5 L/min for 15 to 30 minutes. During the gas production process, keep the temperature of the sampling tube insulation jacket at 120 °C.
To avoid condensation of water vapor before the absorption tube. If the effluent contains chloride particulate matter, install the filter before the absorption bottle (4.7)
Filter clamp.
6.1.2 Air
Sampling is performed as HJ/T 194. The sampler should be air tight and flow calibrated prior to use. Install the microporous membrane (4.7) in the filter
Inside the membrane holder, two large bubble absorption tubes each containing 10 ml of absorption/eluent (4.2) are connected in series, using an air sampler at 1 L/min.
Flow rate, gas production for 60 min.
6.2 Sample storage
After the sample was collected, it was sealed with a Teflon tube, stored at 0-4 ° C, and analyzed within 48 h.
6.3 Sample preparation
6.3.1 Organized emission samples
After sampling, inject the sample (6.1.1) in the two absorption tubes into a 50 ml plug colorimetric tube, dilute to the mark with water, shake
uniform. Pipette 10.00 ml of the above sample solution, place it in two other 50 ml plug colorimetric tubes, dilute with water to the mark, and shake well.
6.3.2 Organized emission blank samples
Handle the blank sample of the whole procedure with 6.3.1.
6.3.3 Air sample
Move the sample (6.1.2) from the two absorption tubes into two 10 ml plug colorimetric tubes and wash them with a small amount of eluent (4.2).
After the inner wall of the tube is closed, the eluent is transferred into the colorimetric tube, diluted to a 10 ml mark, and shaken.
6.3.4 Air blank sample
The full procedure blank sample processing steps are the same as 6.3.3.
7 Analysis steps
7.1 Chromatographic conditions
Instrument conditions can be selected by referring to the instructions. The conditions and parameters listed below are for reference only.
Flow rate. 1.00 ml/min; injection volume. 100 μl.
Column temperature. room temperature (not less than 18 ° C ± 0.5 ° C).
7.2 Drawing of standard curve
7.2.1 Take 6 50 ml volumetric flasks and prepare standard series I according to Table 1.
Table 1 Potassium Chloride Standard Series I
Pipe number 0 1 2 3 4 5
KCl standard use liquid I (4.4)/ml 0 0.50 1.00 5.00 10.0 25.0
Eluent/ml 50.00 49.5 49.0 45.0 40.0 25.0
Cl− mass concentration/(μg/ml) 0 1.00 2.00 10.0 20.0 50.0
After mixing the tubes, the ion chromatograph was injected to measure the response and retention time of the instrument. With the instrument response value versus Cl− mass concentration (μg/ml),
Draw a standard curve I, which is suitable for stationary source exhaust gas samples.
7.2.2 Take 6 10 ml volumetric flasks and prepare standard series II according to Table 2.
Table 2 Potassium Chloride Standard Series II
Pipe number 0 1 2 3 4 5
KCl standard use liquid II (4.5)/ml 0 0.10 0.25 0.50 1.00 2.00
Eluent/ml 10.0 9.90 9.75 9.50 9.00 8.00
Cl− mass concentration/(μg/ml) 0 0.10 0.25 0.50 1.00 2.00
After mixing the tubes, the ion chromatograph was injected to measure the response and retention time of the instrument. With the instrument response value versus Cl− mass concentration (μg/ml),
Draw a standard curve II that is suitable for air samples.
7.3 Determination of samples
The sample (6.3) was filtered with a 0.45 μm acetate fiber microporous membrane (4.6) to obtain a sample, which was stored in polytetrafluoroethylene or polyethylene.
In a plastic bottle. The same procedure blank sample is processed in the same way. The sample is injected into the ion chromatograph during the measurement, under the same conditions as the standard curve is drawn.
Determine the Cl− content.
8 Calculation of results
8.1 The mass concentration of hydrogen chloride in the fixed source of waste gas is calculated according to formula (1).
Nd
( 2 ) 50 36.46 (HCl)
10.0 35.45
ρ ρ ρρ − ×= × × (1)
Where. (HCl)ρ - mass concentration of HCl in the fixed source exhaust gas, mg/m3;
Ρ1, ρ2--Cl− mass concentration in the first and second tube samples, μg/ml;
ρ0--Cl− mass concentration in blank sample, μg/ml;
V1--sample volume after dilution, ml;
Vnd - the sampling volume of dry gas in the standard state (101.325 kPa, 273 K), L;
36.46-- molar mass of HCl, g/mol;
The molar mass of 35.45--Cl−, g/mol.
8.2 The mass concentration of hydrogen chloride in the air is calculated according to formula (2).
Nd
( 2 ) 10.0 36.46 (HCl)
35.45V
ρ ρ ρρ − ×= × (2)
Where. (HCl)ρ - mass concentration of HCl in air, mg/m3;
Ρ1, ρ2--Cl− mass concentration in the first and second tube samples, μg/ml;
ρ0--Cl− mass concentration in blank sample, μg/ml;
Vnd - the sampling volume of dry gas in the standard state (101.325 kPa, 273 K), L.
9 Quality Assurance and Quality Control
9.1 Quality control and quality assurance are carried out in accordance with HJ/T 373.
9.2 For organized exhaust emissions, the concentration of the absorbent is 50 times the concentration of the eluent, so the sample solution must be diluted 50 times before the measurement, so that
The concentration is close to the elution liquid phase, and when the concentration difference is large, the measurement error is large.
9.3 When the concentration of hydrogen chloride in the exhaust gas is low, the concentration of the absorption liquid can be set lower, and the measurement is diluted to be close to the concentration of the eluent.
9.4 The sensitivity of this method is high, and the absorption tube, connecting tube and each utensil should be carefully washed; pay attention to prevent chlorine in tap water and air dust during operation.
Interference with the compound.
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