HJ 549-2016 (HJ549-2016) & related versions
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Ambient air and stationary source emissions. Determination of hydrogen chloride. Ion chromatography
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Ambient air and waste gas. Determination of hydrogen chloride. Ion chromatography
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HJ 549-2016: PDF in English
HJ 549-2016
Ambient air and stationary source emissions -Determination of Hydrogen Chloride-Ion Chromatography
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 549-2009
Determination of ambient air and waste hydrogen chloride
Ion chromatography
Ambient air and stationary source emissions -Determination of Hydrogen
Chloride-Ion Chromatography
2016-05-13 release
2016-08-01 implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Terms and definitions 1
4 Principle of the method
5 interference and elimination
6 reagents and materials 1
7 instruments and equipment 2
8 Sample 3
9 Analysis steps
10 results are calculated and expressed
11 Precision and Accuracy
Quality assurance and quality control
13 Waste treatment .7
14 Precautions .8
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,
The protection of human health, regulate the ambient air and waste gas in the determination of hydrogen chloride, the development of this standard.
This standard specifies the determination of ambient air and hydrogen chloride in waste gas by ion chromatography.
This standard is the "ambient air and waste hydrogen chloride determination of ion chromatography (provisional)" (HJ 549-2009) repair
Set.
This standard was first published in.2009, the original standard drafting unit for the Beijing Environmental Protection Monitoring Center. This time for the first time
The main contents of the amendments and amendments are as follows.
- revised method limits, reagents and materials, instruments and equipment, sample collection, analysis steps, results calculations
With the express clause.
- complements the principle of the method, quality assurance and quality control part of the content.
- Added warnings, terms and definitions, interference and elimination, precision and accuracy, and cautionary terms.
From the date of implementation of this standard, the original standard "Determination of ambient air and waste hydrogen chloride ion chromatography (provisional)" (HJ
549-2009).
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.
The standard verification unit. Jiangsu Province Environmental Monitoring Center, Peking University Environmental Engineering Laboratory, Beijing physical and chemical analysis
Center, Beijing Environmental Protection Monitoring Center, Beijing Haidian District Environmental Protection Bureau Monitoring Station and Beijing Fangshan District Environmental Protection
Monitoring station.
The environmental protection department of this standard approved on May 13,.2016.
This standard has been implemented since August 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Ambient air and waste gas - Determination of hydrogen chloride - Ion chromatographic method
WARNING. Hydrogen chloride is harmful to the human body. When sampling, wear protective equipment in a sampling environment to avoid inhalation or contact with skin
And eyes.
1 Scope of application
This standard specifies the determination of ambient air and hydrogen chloride in waste gas by ion chromatography.
This standard applies to the determination of hydrogen chloride in ambient air and waste gas.
For ambient air, when the sampling volume is 60 L (standard state) and the volume of volume is 10.0 ml, the detection limit is
0.02 mg/m3, the determination of the lower limit of 0.080 mg/m3.
For the fixed source of waste gas, when the sampling volume of 10 L (standard state), the volume of volume is 50.0 ml, the method check
Limit of 0.2 mg/m3, the determination of the lower limit of 0.80 mg/m3.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Determination of particulate matter and sampling method of gaseous pollutants in exhaust gas of fixed pollution sources GB/T 16157
Technical Guidelines for Unorganized Emissions Monitoring of Air Pollutants
Technical specification for manual monitoring of ambient air quality
HJ 664 ambient air quality monitoring point layout technical specifications (Trial)
3 terms and definitions
The following terms and definitions apply to this standard.
Hydrogen chloride hydrogen chloride
Hydrogen chloride as defined in this standard refers to hydrogen chloride gas in the form of gaseous or mist droplets.
4 principle of the method
Water or alkaline absorption solution, respectively, to absorb ambient air or fixed sources of waste gas in the hydrogen chloride, the formation of chloride ions
The sample was injected into an ion chromatograph for separation and determination. Detection by conductivity detector, according to retention time qualitative, peak area or peak height
Quantitative.
5 interference and elimination
Granular chloride has interference with the measurement, sampling can be used PTFE filter or quartz filter to remove its interference. Chlorine gas
Interference with the determination of the use of acid absorption liquid in series alkaline absorption liquid sampling, respectively, to absorb hydrogen chloride and chlorine can remove its interference.
6 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The test water is a resistivity ≥18 ΜΩ · cm
Of fresh deionized water.
6.1 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml.
6.2 sodium hydroxide (NaOH). excellent grade pure.
6.3 Potassium hydroxide (KOH). excellent grade pure.
6.4 potassium chloride (KCl). excellent grade pure. Before use, should be 105 ℃ ± 5 ℃ bake 2 h, placed in a dryer to cool to room temperature, prepare
use.
6.5 alkaline absorption solution. c (NaOH) = 30 mmol/L or c (KOH) = 30 mmol/L.
Weigh 1.20 g of sodium hydroxide (6.2), dissolve in water and set to 1000 ml of polyethylene vials, mix; or weigh 1.68 g
Potassium hydroxide (6.3), dissolved in water and fixed to 1000 ml of polyethylene bottles, and mix well. Pro is now available.
6.6 Rinse stock solution. according to the instrument model and column instructions for the use of conditions for preparation. In 0 ℃ ~ 4 ℃ cold, sealed
Can be saved for 3 months.
6.7 Eluent. Dilute the eluent (6.6) to obtain eluent.
Note 1. If the instrument model has automatic on-line generation of eluent function, can be automatically generated.
Note 2. The eluent should be degassed before use to avoid bubbling into the ion chromatographic system.
6.8 Chloride stock solution. ρ (Cl -) = 1000 mg/L.
Accurately weighed 0.5257 g potassium chloride (6.4), dissolved in water and volume to 250 ml volumetric flask, mix. Transferred to polyethylene
The bottle is refrigerated at 4 ° C and the seal can be stored for 6 months. You can also purchase commercially available standard solutions.
6.9 Chloride standard solution, ρ (Cl -) = 100 mg/L.
Remove 10.00 ml of chloride stock solution (6.8), diluted with water volume to 100 ml volumetric flask, mix, with the current allocation.
6.10 sulfuric acid absorption solution, c (H2SO4) = 0.05 mol/L.
Remove 2.7 ml of sulfuric acid (6.1), slowly add the appropriate amount of water, after cooling diluted volume to 1000 ml volumetric flask, mix.
Cold storage at 4 ℃ can be stored for 3 months.
6.11 sodium hydroxide solution, c (NaOH) = 0.1 mol/L.
Weigh 4.0 g sodium hydroxide (6.2), dissolve in water, cool, set to 1000 ml volumetric flask. Into the polyethylene bottle,
Cold storage at 4 ℃ can be stored for 3 months.
7 instruments and equipment
7.1 Air Sampler. Sampling Flow 0 L/min ~ 1 L/min.
7.2 Flue gas sampler. sampling flow rate 0 L/min ~ 1 L/min, sampling tube for the hard glass or fluorine resin material, should have the heating
And insulation function.
7.3 Smoke sampler. sampling flow 5 L/min ~ 50 L/min, sampling tube for the hard glass or fluorine resin material, should be equipped with
Heat and insulation functions.
7.4 polytetrafluoroethylene filter or quartz filter. particle size greater than 0.3 μm particles of the retention efficiency of not less than 99.9%.
7.5 filter folder. Teflon material, size and filter (7.4) match.
7.6 Connecting tube. Teflon hose or silicone rubber tube with PTFE film.
7.7 Cooling device. ice water bath.
7.8 Impact absorption bottle. 25 ml, 75 ml.
7.9 Ion Chromatograph. An analysis system consisting of an ion chromatographic host, operating software and required accessories. Equipped with anions
From the column (polydiorylene benzene/ethyl vinyl benzene, with alkanol quaternary ammonium functional groups, hydrophilic, high-capacity column) and the
Ion protection column, detector and other testing equipment, suitable for the detection of chloride ions.
7.10 Acetate microporous membrane. 0.45 μm.
7.11 disposable syringes. 10 ml.
7.12 General laboratory equipment and equipment commonly used.
8 samples
8.1 Absorption bottle preparation
Pre-wash the impact absorption bottle with water (7.8) to wash the liquid conductivity less than 1.0 μS/cm, placed in a clean environment to dry
spare. Before sampling, add the absorbent (water or 6.5) and seal and store with a connecting tube (7.6).
8.2 Sample collection
8.2.1 Ambient air samples
Ambient air distribution and sampling shall comply with the relevant provisions of HJ 664 and HJ/T 194. At the time of sampling, the filter (7.4) is set
In the membrane clamp (7.5), the two series of 10 ml of water as the absorption solution of 25 ml impact absorption bottle (7.8), and air
The sampler (7.1) is connected. At a sampling flow rate of 0.5 L/min ~ 1.0 L/min, collected at least 45 min, before and after sampling flow
Poor ≤ 5%.
8.2.2 Unorganized Emissions Samples
The distribution and sampling of unorganized emission samples shall comply with the relevant provisions of HJ/T 55. At the time of sampling, the filter (7.4) was placed in a filter
Membrane holder (7.5), in series with two loaded 10 ml of water as the absorbent solution of 25 ml impact absorption bottle (7.8), with air sampling
(7.1) connection. Sampling at a flow rate of 0.5 L/min to 1.0 L/min, sampling for 1 hour or 1 hour
Interval to collect the average of 3 to 4 samples, such as low concentration may be appropriate to extend the sampling time, before and after sampling flow deviation should be
≤ 5%.
8.2.3 Fixed sources of waste gas samples
Fixed source of waste gas distribution and sampling should be consistent with the relevant provisions of GB/T 16157, sampling device shown in Figure 1. Series two
(7.5) 75 ml impact absorption bottle (7.8), according to the gaseous pollutant collection method, with 0.5
L/min ~ 1.0 L/min flow, continuous 1 hour sampling, or in 1 hour at equal intervals to collect three to four samples,
The flow deviation before and after sampling should be ≤5%. In the sampling process, should keep the sampling tube insulation jacket temperature of 120 ℃, to avoid water
Steamed before the absorption of the bottle. If the exhaust gas contains particulate chloride, it should be placed in the absorption bottle (7.8) before the filter into the filter (7.4)
Of the filter clip (7.5).
Figure 1 Schematic diagram of hydrogen chloride sampling in waste gas from fixed sources
Note 3. When the concentration of hydrogen chloride in the exhaust gas of the fixed source is higher than 100 mg/m3, the concentration of the absorption liquid may be increased appropriately, but the test should be diluted to
And the concentration of eluent.
Note 4. When the fixed source of waste gas containing chlorine, the four series of four absorption bottles, the first two for each 50 ml of sulfuric acid absorption solution (6.10) 75
Ml impact absorption bottle (7.8), the latter two for each 50 ml of alkaline absorption solution (6.5) 75 ml impact absorption bottle (7.8), before and after the two groups of suction
The collection of hydrogen chloride gas and chlorine, respectively, to avoid chlorine interference.
Note 5. High concentration SO42- will interfere with the column, after use should be promptly cleaned.
Note 6. When the humidity in the exhaust gas of the fixed source is large and the hydrogen chloride is absorbed and is mainly in the form of hydrochloric acid mist, the sampling device is shown in Fig. This time cloth
Points and sampling should be consistent with GB/T 16157 on the relevant provisions of the collection of particulate matter. After the soot sampler connected to the heating device (including the diversion valve and filter
Film jacket), and in series with two 50 ml of alkaline absorption solution (6.5) 75 ml impact absorption bottle (7.8), according to the particle sampling method
Hydrochloric acid fog. Sampling process to keep the dust sampling tube and heating device temperature at 120 ℃, in order to avoid water vapor in the absorption bottle before the condensation. Through the diverter valve,
The hydrogen chloride gas sampling flow control in the 0.5 L/min ~ 1.0 L/min, for 1 hour sampling, or within 1 hour at equal intervals to collect three ~
4 samples. When the fixed source of waste gas containing chlorine interference, the absorption bottle in series according to note 4 operation.
Figure 2 Schematic diagram of a hydrochloric acid mist sampling device for fixed sources of waste gas
8.2.4 Full program blank
Each sample should be collected with at least two sets of full program blank samples. Will be equipped with the same batch of absorption liquid absorption of the bottle to the sampling is now
Field, not connected with the sampler, after sampling to bring back to the laboratory to be tested.
8.3 Sample transport and preservation
After the sample collection, the absorbent bottle was sealed with a connecting tube (7.6), stored at 4 ℃ or below, and analyzed and finished within 48 h.
If the analysis can not be timely, the sample should be transferred to the polyethylene bottle, frozen at 4 ℃ can be stored for 7 d.
8.4 Preparation of sample
8.4.1 Ambient air and unorganized emissions samples
The sample solution in the two absorption bottles (8.2.1 or 8.2.2) was transferred to two 10 ml plugs
Color tube, with a small amount of water to absorb the absorption of the inner wall of the bottle, lotion into the colorimetric tube, diluted volume to 10 ml mark, shake.
8.4.2 Fixed sources of waste gas samples
A sample solution of two 75 ml impact absorbers (8.2.3 of the absorbed solution) was transferred to two 50 ml
With a plug color tube, with a small amount of water to absorb the absorption of the inner wall of the bottle, lotion into the colorimetric tube, diluted volume to 50 ml mark, shake.
Note 7. After collecting the exhaust gas from the fixed source containing chlorine gas, the acid absorption solution in the first two impact absorbing bottles (Note 4)
Absorption liquid) were transferred into two 50 ml with a colorimetric tube, with a small amount of water to absorb the absorption of the inner wall of the bottle, lotion into the colorimetric tube, diluted volume to the mark,
Shake well To avoid the interference of acidic absorption solution, remove the sample solution of 10.0 ml of the above-mentioned plug colorimetric tube, and place it in the other two 50 ml
Plug the color tube, and were added 5.00 ml sodium hydroxide solution (6.11), diluted with water volume to the mark, shake.
8.4.3 Lab blank
In the laboratory, take the same batch, with the same volume of absorbent solution in accordance with 8.4.1 or 8.4.2 the same steps to prepare
Laboratory blank samples.
8.4.4 Full program blank
The whole program blank sample solution (8.2.4) was prepared in the same procedure as in 8.4.1 or 8.4.2.
8.5 Preparation of the sample
The treated sample (8.4) was extracted with a disposable syringe (7.11), and a microporous membrane (7.10) was inserted at the front end of the syringe,
Push the sample thoroughly and discard the initial 3 ml sample and collect the remaining eluent.
9 Analysis steps
9.1 Chromatographic reference conditions
Optimize measurement conditions or parameters according to the instrument manual. Reference conditions. eluent for 30 mmol/L potassium hydroxide dissolved
Liquid at a flow rate of 1.00 ml/min and an injection volume of 100 μl. The column temperature is 30 ° C ± 0.5 ° C. Suppressor current is 75 mA.
9.2 Standard curve drawing
Respectively, remove 0.00 ml, 0.50 ml, 1.00 ml, 5.00 ml, 10.00 ml chloride standard solution (6.9) placed in a group
50 ml volumetric flask, the water volume to the mark, shake. The standard series of chloride ion concentration (in Cl-dollars) were 0.00 mg/L,
1.00 mg/L, 2.00 mg/L, 10.0 mg/L and 20.0 mg/L. From the low concentration to the high concentration, the injection volume was 100
Μl, get different concentrations of chloride ion chromatogram. The chloride ion concentration (in Cl-, mg/L) is the abscissa, peak height or peak
Area is the ordinate, draw the standard curve. The chromatogram containing chloride ions is shown in Fig.
Figure 3 Standard chromatogram containing chloride ion (1-fluoro ion; 2-chloride ion; 3-sulfate ion; 4-nitrate ion)
9.3 Determination of samples
The sample (8.5) was injected into an ion chromatograph according to the same chromatographic conditions (9.1) and (9.2) as the standard curve,
Determination of Cl-content. When the Cl-content in the sample exceeds the standard curve drawing range, the water is diluted with water and then re-determined.
10 results are calculated and expressed
10.1 Ambient air and unorganized emissions
Calculate the concentration of hydrogen chloride in ambient air and unorganized emissions according to equation (1).
()
45.35
45.360.102 021
) (×× - =
NV
Ρρρρ Hydrogen Chloride (1)
Where. (hydrogen chloride ρ - ambient air or unorganized emissions of hydrogen chloride concentration, mg/m3;
1 ρ - Cl-concentration, mg/L for the first sample prepared with a plug colorimetric sample;
2 - the concentration of Cl-concentration, mg/L in the sample prepared from the second stopper;
0 μ - Cl-average concentration of mg/L in two samples prepared from laboratory test specimens;
NV - the sampling volume under the standard state (101.325 kPa, 273 K), L;
36.45 - molar mass of HCl, g/mol;
35.45 - molar mass of Cl-, g/mol.
10.2 Fixed sources of waste gas
Calculate the concentration of hydrogen chloride in the exhaust gas of the fixed source according to formula (2)
()
45.35
45.36502 021
) (×× - =
NdV
Ρρρρ Hydrogen Chloride (2)
Where.) (hydrogen chloride ρ - fixed source of waste gas in the concentration of hydrogen chloride, mg/m3;
1 ρ - Cl-concentration, mg/L for the first sample prepared with a plug colorimetric sample;
2 - the concentration of Cl-concentration, mg/L in the sample prepared from the second stopper;
0 μ - Cl - average concentration of mg/L in two samples prepared from laboratory test specimens;
NdV - the sampling volume of dry flue gas in the standard state (101.325 kPa, 273 K), L;
36.45 - molar mass of HCl, g/mol;
35.45 - molar mass of Cl-, g/mol.
10.3 Results indicated
When the concentration of hydrogen chloride in the ambient air or unorganized emissions is greater than or equal to 0.1 mg/m3, the result retains three
Effective number; less than 0.1 mg/m3, the results remain to the decimal point after 3.
When the concentration of hydrogen chloride in the exhaust gas of the fixed source is greater than or equal to 1.0 mg/m3, the result retains three significant digits;
Less than 1.0 mg/m3, the result is reserved for 2 digits after the decimal point.
11 precision and accuracy
11.1 precision
Six laboratory samples were prepared for 4 different concentrations of chloride (Cl-) uniform standard (1.0 mg/L, 2.0 mg/L,
25.0 mg/L and 50.0 mg/L) were measured in parallel. the relative standard deviations in the laboratory were 0.5% to 4.9%
0.2% ~ 4.1%, 0.2% ~ 3.5% and 0.1% ~ 1.2% respectively. The relative standard deviations were 5.3%, 1.2% and 3.5%
And 1.0%; the repeatability r was 0.006 mg/L, 0.004 mg/L, 0.4 mg/L, 0.3 mg/L, respectively; the reproducibility limit R
0.2 mg/L, 0.1 mg/L, 2.7 mg/L, 1.7 mg/L.
11.2 Accuracy
Six laboratory samples of three different concentrations of chloride (Cl-) uniform standard samples (standard values were 0.494
Mg/L ± 0.029 mg/L, 44.0 mg/L ± 1.0 mg/L and 5.02 mg/L ± 0.24 mg/L)
The relative errors were -3.2% ~ 0.5%, 0.4% ~ 2.5%, 4.0% ~ 2.2%, respectively. The relative error values were
0.2% ± 6.6%, 1.1% ± 1.4%, - 1.2% ± 4.6%.
Standard units of hydrogen chloride concentration of 1.04 mg/m3 ~ 1.94 mg/m3 of ambient air samples and hydrogen chloride concentration
The recoveries of spiked samples were 4.82 mg/m3 ~ 28.1 mg/m3, and the recoveries were as follows.
92.5% ~ 104% and 90.0% ~ 109% respectively. The final recoveries were 99.0% ± 4.8% and 98.0% ± 7.7%, respectively.
12 quality assurance and quality control
12.1 Blank experiment
At least two laboratory blanks and two full program blanks were measured for each batch. Laboratory blank determination results should be lower than the method
Detection limit; full program blank determination results should be lower than the lower limit of determination. Otherwise, you should find the cause or re-collect the sample.
12.2 Calibration curve
Each time you start the machine, the standard curve should be drawn and the linear correlation coefficient of the standard curve should be ≥0.999. Each test should be 10 samples
With a standard curve of the middle concentration of the calibration point, the middle of the calibration point of the measured value and the standard solution concentration value of the relative error
Should be ≤ 10%. Otherwise, the standard curve should be redrawn.
12.3 Adsorption efficiency
The adsorption efficiency of the absorption bottle should be ≥80%. That the second absorbent bottle should be collected less than 25% of the first absorbent bottle,
Otherwise it should adjust the flow or sampling time, re-sampling. The adsorption efficiency of the absorption bottle was calculated according to the formula (3).
VV
VK × ×
× = ρρ
(3)
Where. K - absorption efficiency of the absorption bottle,%;
1 - the concentration of Cl-concentration, mg/L in the sample prepared from the first absorption bottle,
2 - the concentration of Cl- in mg/L in the sample prepared by the second absorption bottle.
1V - the volume of the first absorption bottle to absorb the liquid, ml;
2V - the volume of the second absorption bottle absorption liquid, ml.
13 Waste treatment
The waste generated in the experiment shall be collected and collected in a centralized manner, and shall be handled safely or entrusted with qualified units.
14 Precautions
14.1 Absorbent bottles, connecting pipes and containers are used to repeatedly wash the test water and to prevent contamination, the last lotion conductivity should be
Less than 1.0 μS/cm. Operation should prevent the tap water, air dust and the hands of chloride interference.
14.2 Sampler and filter clamp, filter clip and absorption bottle, the connection between the absorption bottle should be as short as possible, and check the system
Air tightness and reliability.
14.3 After each analysis of the sample, use an eluent to clean the instrument line. After the end of the experiment, wash the instrument pump with experimental water
Suppressor, so as not to be subject to eluent corrosion.
14.4 If the instrument analysis accuracy is reduced, check the column efficiency and suppressor working condition, if necessary, to replace
Analyze the accuracy of the data.
......
| Standard ID | HJ 549-2016 (HJ549-2016) | | Description (Translated English) | Ambient air and stationary source emissions. 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 | 12,143 | | Date of Issue | 2016-05-13 | | Date of Implementation | 2016-08-01 | | Older Standard (superseded by this standard) | HJ 549-2009 | | Quoted Standard | GB/T 16157; HJ/T 55; HJ/T 194; HJ 664 | | Drafting Organization | Beijing Environmental Protection Monitoring Center | | Administrative Organization | Ministry of Environmental Protection | | Regulation (derived from) | Ministry of Environmental Protection Announcement No. 39 of 2016 | | Summary | This standard specifies the ion chromatography for the determination of hydrogen chloride in ambient air and exhaust gas. This standard applies to the determination of hydrogen chloride in the ambient air and exhaust gas. For ambient air, when the sample volume is 60 L (standard state) and the volumetric volume is 10.0 ml, the method detection limit is 0.02 mg/m^3 and the lower limit of determination is 0.080 mg/m^3. For the fixed source exhaust gas, when the sampling volume is 10L (standard state), constant volume is 50.0 ml, the method detection limit is 0.2 mg/m^3 and the lower limit of determination is 0.80 mg/m^3. |
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