HJ 544-2016_English: PDF (HJ544-2016)
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Stationary source emission. Determination of sulfuric acid mist. Ion chromatography
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HJ 544-2016
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Standards related to: HJ 544-2016
| Standard ID | HJ 544-2016 (HJ544-2016) | | Description (Translated English) | Stationary source emission. Determination of sulfuric acid mist. Ion chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Word Count Estimation | 12,140 | | Date of Issue | 2016-03-29 | | Date of Implementation | 2016-05-01 | | Older Standard (superseded by this standard) | HJ 544-2009 | | Quoted Standard | GB/T 16157; HJ/T 55; HJ/T 373; HJ/T 397 | | Drafting Organization | Beijing Environmental Protection Monitoring Center | | Administrative Organization | Ministry of Environmental Protection | | Regulation (derived from) | Ministry of Environmental Protection Announcement No | HJ 544-2016
Stationary source emission. Determination of sulfuric acid mist
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 544-2009
Determination of sulfuric acid mist in fixed source waste gas
Ion chromatography
Stationary source emission-Determination of sulfuric acid
Mist-ion chromatography
2016-03-29 released
2016-05-01 implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application 1
2 normative reference document 1
3 Terms and Definitions
Principle of Method 1
5 interference and elimination
6 reagents and materials
7 instruments and equipment
8 samples
9 Analysis Step 5
Calculation and representation of results
11 Precision and Accuracy 7
12 Quality assurance and quality control
13 Waste treatment 9
14 Precautions 9
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,
Protection of human health, regulate the fixed source of waste gas in the determination of sulfuric acid mist, the development of this standard.
This standard specifies the determination of sulfuric acid mist in fixed sources of waste gas by ion chromatography.
This standard is the "fixed pollution source of sulfuric acid mist determination of ion chromatography (provisional)" (HJ 544-2009) 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, methodological principles, interference and elimination, reagents and materials, instruments and equipment, sample collection,
Sample transport and preservation, sample preparation and analysis steps;
- increased terminology and definition, precision and accuracy;
- complements quality assurance and quality control.
From the date of implementation of this standard, the original standard "fixed pollution source sulfur sulfur fog determination of ion chromatography (provisional)" (HJ
544-2009).
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. Beijing Physical and Chemical Analysis and Testing Center, Peking University Environmental Engineering Laboratory, Jiangsu Province Environmental Monitoring
Test center, Beijing Haidian District Environmental Protection Bureau monitoring station, Beijing Fangshan District Environmental Protection Monitoring Station, Beijing Environmental Protection
Monitoring center.
The environmental protection department of this standard approved on March 29,.2016.
This standard has been implemented since May 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of sulfuric acid mist from fixed sources - Ion chromatography
1 Scope of application
This standard specifies the determination of sulfuric acid mist in fixed sources of waste gas by ion chromatography.
This standard is applicable to the determination of sulfuric acid mist in the exhaust gas of fixed pollution source.
Determination of tissue emissions, when the sampling volume of 0.40 m3 (standard state), constant volume of 100 ml, the sample
When the product is 25 μl, the detection limit is 0.2 mg/m3 and the determination limit is 0.80 mg/m3. Determination of unorganized emissions, when mining
The volume of the sample was 3.0 m3 (standard state), the volume of volume was 50.0 ml, and the detection limit was 0.005
Mg/m3, the determination of the lower limit of 0.020 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
HJ/T 373 fixed pollution source monitoring quality assurance and quality control technical specifications (Trial)
Technical specification for HJ/T 397 fixed source exhaust gas monitoring
3 terms and definitions
The following terms and definitions apply to this standard.
Sulfuric acid mist
The sulfuric acid mist measured in this standard includes small sulfuric acid droplets, sulfur trioxide and soluble sulfate in particulate matter.
4 principle of the method
With a glass fiber filter cartridge (or quartz fiber filter cartridge) in series 50 ml of absorption liquid absorption bottle, collecting tissue emissions
Sulfuric acid mist samples in the air; samples of sulfuric acid mist from unorganized exhaust gas collected from quartz fiber filter. The collected samples were preached
After treatment, the sulfate was separated and determined by ion chromatograph, and quantified according to the retention time, peak area or peak height.
5 interference and elimination
Organic pollutants can pollute the column and interfere with the determination of samples can be removed using C18 solid phase extraction column.
6 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water for the resistivity ≥ 18
MΩ • cm deionized water.
6.1 Methanol. ρ (CH3OH) = 0.79 g/ml.
6.2 sodium hydroxide (NaOH). excellent grade pure.
6.3 Potassium hydroxide (KOH). excellent grade pure.
6.4 Potassium Sulfate (K2SO4). Reference reagent.
Weigh 5.0 g of potassium sulfate in a porcelain crucible, placed in an oven at 105 ° C for 2 h, cooled to room temperature and placed in a dryer
Save, spare.
6.5 Absorbent 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 bottle, mix; or weigh 1.68
G potassium hydroxide (6.3), dissolved in water and volume to 1000 ml of polyethylene bottles, mix, with the current allocation.
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
Save 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 Potassium sulphate stock solution. ρ (SO42 -) = 1000 mg/L.
Accurately weigh 1.8140 g potassium sulfate (6.4), dissolved in water and volume to 1000 ml volumetric flask, shake. At 0 ° C to 4 ° C
Refrigerated, sealed for 3 months. You can also purchase commercially available standard solutions.
6.9 Standard Specification for Potassium Sulfate. ρ (SO42 -) = 100 mg/L.
Remove 10.00 ml of potassium sulfate stock solution (6.8), diluted with water volume to 100 ml volumetric flask, shake. Potassium Sulfate Standard
Use liquid at 0 ℃ ~ 4 ℃ cold, sealed can be stored for 1 month.
6.10 C18 solid phase extraction column..200 mg/3 ml.
C18 solid phase extraction column must be activated before use. With the syringe were measured 10 ml of methanol (6.1) and 15 ml experimental use
Water, followed by light through the column, the column placed about 30 min, you can start using.
6.11 glass fiber filter or quartz fiber filter cartridge.
The filter particles have a barrier efficiency of not less than 99.9% for particles with particle size greater than 3 μm. Such as glass fiber filter blank value is higher than the detection
Limit, with the experimental water repeatedly dip filter cartridge, the filter into the experimental water with a large beaker, with paraffin seal film or surface dish
Cover the beaker, place it in an ultrasonic cleaner for 10 min, then measure the conductivity of the soaked water. The conductivity should be less than 3.0
MS/m, otherwise repeat the above steps. Will be washed on the filter cartridge on the filter holder, placed in a dry box at room temperature to dry and dry
After the filter box into the spare. Quartz fiber cartridge without pre-treatment.
6.12 quartz fiber filter. diameter 90 mm.
6.13 Water microporous membrane. pore size 0.45 μm.
6.14 Water Microporous Membrane Filter. Aperture 0.45 μm.
6.15 Disposable syringes. 10 ml.
6.16 Polyethylene tube. used to seal the impact absorption bottle.
6.17 filter box. Teflon (PTFE) or polystyrene (PS) material.
6.18 Carrier gas. high purity nitrogen, purity ≥99.99%.
7 instruments and equipment
7.1 dust sampler. 5 L/min ~ 50 L/min, smoke gun with heating and insulation function.
7.2 Flow Particle Sampler. Flow rate 80 L/min ~ 130 L/min, error ≤ 2%.
7.3 Impact absorption bottle. 75 ml.
7.4 Ion Chromatograph. An analytical system consisting of an ion chromatograph, operating software, and required accessories. Equipped with anionic separation
Column (polydiorylenebenzene/ethyl vinyl benzene, with quaternary ammonium functional groups, hydrophilic, high-capacity columns) and anionic
Sub-protection column, detector and other testing equipment for the detection of sulfate.
7.5 Analysis of the balance. the amount of 0.1 mg.
7.6 Sampling cooling device. ice bath.
7.7 Ultrasonic cleaner. ultrasonic frequency range of 40 KHz ~ 100 KHz, ultrasonic power range of 100 W ~ 600 W.
7.8 electric stove or electric plate.
7.9 Glass funnel. diameter 60 mm.
7.10 with a stopper mouth vial. 250 ml.
7.11 Screw-type wide-mouth polyethylene sealing tube. 50 ml.
7.12 Water-based suction filter.
7.13 with a colorimetric tube. 50 ml, 100 ml.
7.14 General laboratory equipment and equipment.
8 samples
8.1 Sample collection
8.1.1 Organized emissions
The emission and sampling of the exhaust emissions shall be in accordance with the relevant provisions in GB/T 16157. The exhaust gas sampling device is shown in Fig.
Figure 1 Schematic diagram of the organization of exhaust gas sampling devices
Insert the filter cartridge (6.11) into the filter holder of the sampler head and connect the two inlaid 50 ml absorbant
(6.5) impact absorption bottle, collecting sulfur trioxide gas and penetrate the filter tube of small droplets, and then with the empty bottles and dryers
connection. The connection pipe should be as short as possible and check the system for air tightness and reliability. Attach the sampler with the filter cartridge into the exhaust cylinder
Of the sampling point isotope sampling, sampling process, the gun heating temperature is not lower than the flue gas temperature. Select according to the sulfuric acid mist concentration appropriate
Of the sampling time, for 1 hour sampling, or within 1 hour at equal intervals to collect three to four samples, while measuring the temperature
Degree, pressure and other parameters. After sampling, carefully remove the filter into the capped wide-mouth polyethylene sealed tube, with a small amount of experiment
Rinse the mouth of the nozzle and elbow with water, wash the liquid into the sealed tube, cover the stopper, the first, two impact absorption bottle
Polyethylene tube (6.16) sealed to be tested.
8.1.2 Organized emissions Full program blank
Each sample should be collected with at least two sets of full program blank samples. Will be the same batch of filter cartridge and the absorption of the absorption of the bottle
To the sampling site, not connected with the sampler, after sampling to bring back to the laboratory to be tested.
Note 3. Sample collection and blank test shall be carried out using the same batch filter cartridge.
8.1.3 Unorganized emissions
The unorganized emissions shall be in accordance with the relevant provisions of HJ/T 55. With medium flow with quartz fiber filter (6.12)
The particle sampler samples the sample at a flow rate of 100 L/min, sampled continuously for 1 hour, or at equal intervals in 1 hour
Set the average of 3 to 4 samples, such as low concentration may be appropriate to extend the sampling time. The filter should be folded into the sample after collecting the sample
Clean paper bag or filter box (6.17).
8.1.4 Unorganized emissions Full program blank
Each sample should be collected with at least two full-program blank samples. Will be with the batch filter to the sampling site, not with the sampler
Connection, after sampling to bring back to the laboratory to be tested.
Note 4. Sample collection and blank experiments shall be carried out using the same batch filter.
8.2 Sample transport and storage
Collect the sample and the whole program blank should be 0 ℃ ~ 4 ℃ cold storage, sealed, within 24 hours to complete the sample preparation. If
Can not be measured in time, the prepared samples should be 0 ℃ ~ 4 ℃ cold, sealed can be stored for 30 days.
8.3 Sample preparation
8.3.1 Ultrasonic extraction
8.3.1.1 Organized emissions
The samples (lotions and cartridges) in the sealed tubes of the collected exhaust gas (8.1.1) are sampled and the first absorption bottle
Of the absorption liquid all into the 100 ml with a colorimetric tube, with the amount of experimental water washing screw cap-type wide-mouth polyethylene sealing tube and red
Hit the absorption of the inner wall of the bottle, the washing liquid into a plug colorimetric tube, constant volume to the line (need to immerse the cartridge). Put the plug color tube into the super
In the acoustic cleaner, the glass fiber cartridge was sonicated for 45 minutes and the quartz fiber cartridge was ultrasound for 60 minutes. Cool to mix and leach
The liquid was filtered through a 0.45 μm water microporous membrane filter (6.14) to a clean container. The second collection of samples in the whole bottle
Into the other 100 ml with a colorimetric tube, with the right amount of experimental water wash the bottom of the impact absorption bottle, washing liquid and into the
The chenille color tube is scheduled to be measured.
8.3.1.2 Organized emissions Full program blank
(8.1.2) in the same manner as in the case of the Organ Exhaust Emissions Ultrasonic Extraction (8.3.1.1)
Preparation of tissue emissions of the whole program blank sample.
8.3.1.3 Organized emissions laboratory blank
The same procedure was used for the same batch of filter cartridges and two impact absorbers in accordance with the Ultrasonic Extraction of Organized Emissions (8.3.1.1)
Preparation of tissue discharge laboratory blank samples.
8.3.1.4 Unorganized emissions
(11.3.3) Sampling the unseasoned exhaust gas (8.1.3) into the 50 ml screw cap type polyethylene sealing tube,
Into the 50 ml of experimental water (need to immerse the filter), screw tight cap, into the ultrasonic cleaner, ultrasonic 60 minutes, cooling and mixing.
The leachate was filtered through a 0.45 μm water microporous membrane filter (6.14) into a clean container.
8.3.1.5 Unorganized emissions Full program blank
(8.1.4) The same procedure as in the case of unintended emission of exhaust gas extraction (8.3.1.4)
Preparation of unorganized emissions of the whole program blank sample.
8.3.1.6 Unorganized emissions laboratory blank
The same procedure was used to prepare the non-tissue emission test in the same batch as the unselected exhaust gas extraction method (8.3.1.4)
Room blank sample.
8.3.2 Heating leaching method
8.3.2.1 Organized emissions
The samples (lotions and cartridges) in the sealed tubes of the collected exhaust gas (8.1.1) are sampled and the first absorption bottle
Of the absorbent liquid all into the 250 ml plug with a mouth-shaped flask, with the right amount of experimental water washing screw-type wide-mouth polyethylene sealing tube
And the impact of the absorption of the inner wall of the bottle, the washing liquid into the conical flask, add about 100 ml of experimental water immersion filter,
Glass funnel, heated in the electric furnace or hot plate near boiling, about 30 minutes after the removal, after cooling the leaching solution by 0.45 μm water system
Microporous membrane (6.13) filter to 100 ml volumetric flask, with the right amount of experimental water washing cone and sample residue 3 times to 4 times,
Wash the liquid by the microporous membrane (6.13) filter into the volumetric flask, fixed capacity to be measured. The samples in the second absorption bottle are all moved into the other
A 100 ml with a colorimetric tube, with the experimental water wash the bottom of the impact absorption bottle, the washing liquid into the color tube
Measurement.
8.3.2.2 Organized emissions Full program blank
(11.2.2) The same procedure as in the case of the exhaust emissions of the exhausted exhaust gas (8.3.2.1)
Organized emissions of the whole program blank sample.
8.3.2.3 Organized emissions laboratory blank
The same batch of filter cartridges and two impact absorption bottles in accordance with the organization of exhaust gas heating leaching method (8.3.2.1) the same steps
Organized tissue laboratory blank sample.
8.3.2.4 Unorganized emissions
The unselected exhaust gas (8.1.3) was sampled into a 250 ml stoppered conical flask and about 100 ml
Experimental water immersion filter, bottle on a glass funnel, in the electric furnace or electric heating plate near boiling, about 30 minutes after the removal,
After cooling, the leachate was filtered through a 0.45 μm water microporous membrane (6.13) into a 50 ml volumetric flask and washed with an appropriate amount of water
Polyester flask and sample residue 3 times to 4 times, the washing liquid through the water microporous membrane (6.13) filter into the volumetric flask,
Measurement.
8.3.2.5 Unorganized emissions Full program blank
(8.1.4) in accordance with the Unorganized Emissions Exhaust Gas Heating Leaching Method (8.3.2.4) Synchro
Preparation of unorganized emissions of the whole program blank sample.
8.3.2.6 Unorganized emissions laboratory blank
The same procedure was used to prepare the non-tissue emissions test in the same batch as the unseasoned exhaust gas heating leaching method (8.3.2.4)
Room blank sample.
9 Analysis steps
9.1 Chromatographic reference conditions
Optimize measurement conditions or parameters according to the instrument manual. Reference conditions. eluent for 20 mmol/L potassium hydroxide dissolved
Liquid flow rate of 1.00 ml/min, suppressor current of 75 mA, detector temperature of 30 ° C, column temperature of room temperature (not less than 18
℃), the injection volume can be selected according to the level of sample concentration 25 μl ~ 100 μl.
9.2 Standard curve drawing
Respectively, accurate removal of 0.00 ml, 1.00 ml, 2.00 ml, 5.00 ml, 10.00 ml, 20.00 ml potassium sulfate standard use of liquid
(6.9) placed in a set of 100 ml volumetric flask, with the experimental water volume and mix. Prepared at concentrations of 0 mg/L, 1.00, respectively
Mg/L, 2.00 mg/L, 5.00 mg/L, 10.0 mg/L, 20.0 mg/L. Determination by ion chromatograph,
To keep the time for the abscissa, the instrument response value for the vertical axis, draw the standard curve. The ion chromatogram is shown in Fig.
Figure 2 Sulfate ion chromatogram
9.3 Determination of samples
The sample (8.3) was injected with the same chromatographic conditions (9.1) and analytical procedure (9.2) as the standard curve for drawing
The concentration of sulfate was determined by chromatograph, and the time was qualitative and the instrument response was quantified.
Note 5. Samples with organic interference should be removed by C18 solid phase extraction column (6.10). Take the sample with a disposable syringe (6.15)
The front end of the syringe was fitted with a C18 solid phase extraction column (6.10), the sample was gently pushed and the initial 3 ml test solution was discarded and the remaining column eluate was collected.
Note 6. If the concentration of the target compound to be measured exceeds the standard curve, the sample and the laboratory blank should be diluted with the same multiple and measured and recorded
Interpretation factor (DF).
9.4 Full program blank determination
The whole program blank sample (8.3) was subjected to the same chromatographic conditions (9.1) and analytical procedure (9.2) as the standard curve for drawing,
Determination of Sulfate Concentration in Hollow Samples by Ion Chromatography.
9.5 Laboratory blank determination
The laboratory blank sample (8.3) was subjected to the same chromatographic conditions (9.1) and analytical procedure (9.2) as the standard curve for drawing,
Determination of Sulfate Concentration in Laboratory Blank Specimen by Ion Chromatography.
10 results are calculated and expressed
10.1 The concentration of sulfuric acid in the exhaust gas from the organized emissions shall be calculated as follows
06.96
08.98) (021 ××× - = DF
Nd
Tρρρρ
(1)
0.00 1.25 2.50 3.75 5.00 6.25 7.50 9.00
-5.0
0.0
5.0
10.0
15.0
20.0
25.0
30.0
35.0
Μs
Min
1 - fluoride ion; 2 - chloride ion; 3 - sulfate ion; 4 - nitrate ion
Where. ρ - concentration of sulfuric acid mist in the exhaust gas of the organized exhaust gas, mg/m3;
1 ρ - Determination of sulfate (SO42-) concentration in the filter cartridge and the first absorption bottle sample, μg/ml;
2 ρ - Determination of sulfate (SO42-) concentration in the second absorption bottle sample, μg/ml;
0 ρ - the average concentration of sulfate (SO42-) in the laboratory blank sample, μg/ml;
TV - volume of sample to be tested, ml;
NdV - the sampling volume of dry flue gas in the standard state (101.325 kPa, 273 K), L;
DF - dilution of sample;
98.08 - molar mass of H2SO4, g/mol;
96.06 - molar mass of SO42-, g/mol.
10.2 Unorganized emissions The sulfuric acid mist concentr......
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