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HJ 647-2013 English PDF

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HJ 647-2013: Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons. High performance liquid chromatography
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 647-2013	English	499	Add to Cart	4 days [Need to translate]	Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons. High performance liquid chromatography	Valid	HJ 647-2013

PDF similar to HJ 647-2013

Standard similar to HJ 647-2013

HJ 644 HJ/T 400 GB/T 16157 HJ 646 HJ 645

Basic data

Standard ID	HJ 647-2013 (HJ647-2013)
Description (Translated English)	Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons. High performance liquid chromatography
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z11
Classification of International Standard	13.040.20
Word Count Estimation	19,194
Quoted Standard	GB/T 16157; HJ/T 48; HJ/T 55; HJ/T 93; HJ/T 365
Regulation (derived from)	Department of Environmental Protection Notice No. 33 of 2013
Issuing agency(ies)	Ministry of Ecology and Environment
Summary	This standard specifies: Determination of ambient air and exhaust sixteen PAHs high performance liquid chromatography. This standard applies to: the ambient air, stationary source emission and fugitive emissions from the gas and particulate matter in the

HJ 647-2013: Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons. High performance liquid chromatography

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Ambient air and stationary source emissions.Determination of gas and particle-phase polycyclic aromatic hydrocarbons.High performance liquid chromatography Ambient air and exhaust gas in gaseous and particulate matter Determination of polycyclic aromatic hydrocarbons by high performance liquid chromatography Ambient air and stationary source emissions - Determination of gas and Particle-phase polycyclic aromatic hydrocarbons - High performance Liquid chromatography Published on.2013-06-03 2013-09-01 Implementation Ministry of Environmental Protection released National Environmental Protection Standard of the People's Republic

Content

Foreword I 1 Scope 1 2 Normative references 1 3 Terms and Definitions 1 4 Principle of the method 2 5 interference and elimination 2 6 Reagents and materials 2 7 Instruments and equipment 4 8 sample 6 9 Analysis step 8 1 0 result calculation 9 11 Accuracy and precision 1 0 1 2 Quality Control and Quality Assurance 11 13 Waste treatment 12 Appendix A (Normative) The detection limit and lower limit of the method 13 Appendix B (informative) The wavelength corresponding to the detection of polycyclic aromatic hydrocarbons by ultraviolet and fluorescence detectors 15 Appendix C (informative) Precision and accuracy of the method 17 Appendix D (informative) Polycyclic aromatic hydrocarbons physical constant 18

Foreword

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 This standard is formulated to ensure human health and to regulate the determination of polycyclic aromatic hydrocarbons in ambient air and exhaust gases. This standard specifies high performance liquid chromatography for the determination of sixteen polycyclic aromatic hydrocarbons in ambient air and exhaust gases. This standard is the first release. Appendix A of this standard is a normative appendix, and Appendix B, Appendix C and Appendix D are informative appendices. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard was drafted. Shenyang Environmental Monitoring Center Station, Environmental Standards Institute of the Ministry of Environmental Protection. This standard is verified by. Jiangsu Environmental Monitoring Center, Liaoning Provincial Environmental Monitoring Experimental Center, and Dalian Environmental Monitoring Heart, Anshan Environmental Monitoring Center Station and Liaoning Provincial Academy of Environmental Sciences. This standard was approved by the Ministry of Environmental Protection on June 3,.2013. This standard has been implemented since September 1,.2013. This standard is explained by the Ministry of Environmental Protection. Determination of polycyclic aromatic hydrocarbons in gaseous and particulate gases from ambient air and exhaust gases High performance liquid chromatography Warning. The solvents and reagents used in this method are all toxic and have potential hazards to health. Avoid direct contact with these chemicals. Sample preparation should be carried out in a fume hood, reagents used and samples after analysis Need to be recycled and safely disposed of.

1 Scope of application

This standard specifies high performance liquid chromatography for the determination of sixteen polycyclic aromatic hydrocarbons in ambient air and exhaust gases. This standard is applicable to more than 16 kinds of gas and particulate matter in ambient air, fixed source exhaust and unorganized exhaust air. Determination of cyclic aromatic hydrocarbons. Sixteen polycyclic aromatic hydrocarbons (PAHs) include. naphthalene, terpenes, anthracene, anthracene, phenanthrene, anthracene, fluoranthene, anthracene, Benzo[a]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene,benzo[a]pyrene,indole[1,2,3-c,d]indole, dibenzo[ a,h]蒽, Benzo[g,h,i]苝. This standard is also applicable to the determination of other polycyclic aromatic hydrocarbons. When the ambient air is collected at 100L/min for 24h, the detection limit of the method is 0.04-0.26ng/m3, and the lower limit of determination is 0.16-1.04ng/m3; when collecting 1m3 of fixed source exhaust gas, the detection limit of the method is 0.01-0.04μg/m3, and the lower limit of determination is 0.04-0.16 μg/m3. See Appendix A for details.

2 Normative references

The contents of this standard refer to the terms in the following documents. 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 48 soot sampler technical conditions HJ/T 55 Technical Guidelines for the Monitoring of Unorganized Emissions of Air Pollutants HJ/T 93 PM10 sampler technical requirements and testing methods HJ/T 365 Hazardous Waste Incineration (including Medical Waste) Disposal Facilities Dioxin Emission Monitoring Technical Specifications

3 Terms and definitions

The following terms and definitions apply to this standard. 3.1 Full program blank whole program blank Bring the sealed sample cylinder and glass fiber filter/cylinder to the sampling site, and expose it to the sampling site without sampling. Oversampling, sampled and shipped back to the laboratory, processed and measured in the same operating steps as the sample, used for inspection Whether the sample is collected and analyzed is contaminated. 3.2 Shipping Blank Trip Blank The sealed sample cylinder and the glass fiber filter/cylinder are brought to the sampling site, and the sample is not opened during sampling, and the sample is sampled after sampling. Returned to the laboratory, processed and measured in the same operating steps as the sample, used to check whether the sample transport process is contaminated dye. 3.3 Surrogate standards Refers to a substance that is not contained in the sample but has similar physicochemical properties to the analyte. Usually added before sample extraction or sampling In, the recovery rate can be used to evaluate the effect of the sample preparation or sampling process on the analytical results. 3.4 sampling efficiency Refers to the ability of the sampler to capture and retain polycyclic aromatic hydrocarbons. Add a certain amount of polycyclic aromatic hydrocarbons to the sampling filter, press and sample Air was drawn under the same operating conditions to determine the retention capacity of the sample medium for polycyclic aromatic hydrocarbons. 3.5 dynamic sampling efficiency Add a certain amount of polycyclic aromatic hydrocarbons to the surface of the sampling adsorption column, pump air according to the same operating conditions as the sample, and measure the sampling medium. The ability to retain polycyclic aromatic hydrocarbons.

4 Principle of the method

Polycyclic aromatic hydrocarbons in gas phase and particulate matter are collected in sampling cylinder and glass (or quartz) fiber membrane/tube, sampling cylinder And filter/cartridge with 10/90 (v/v) ether/n-hexane mixed solvent extraction, the extract is concentrated, silica gel column or Flory After purification by a silica column or the like, it is separated and detected by a high performance liquid chromatograph with a fluorescent/ultraviolet detector.

5 interference and elimination

Heating, ozone, nitrogen oxides, and ultraviolet light during sample collection, storage, and processing can cause degradation of polycyclic aromatic hydrocarbons. Need to be sealed, low temperature, and protected from light.

6 reagents and materials

Analytical purification reagents and distilled water in accordance with national standards were used for analysis unless otherwise stated. 6.1 Acetonitrile (CH3CN). Pure by liquid chromatography. 6.2 Methanol (CH3OH). Pure by liquid chromatography. 6.3 Dichloromethane (CH2Cl2). Chromatographically pure. 6.4 n-Hexane (C6H14). Chromatographically pure. 6.5 Ether (C2H5O C2H5). Chromatographically pure. 6.6 Acetone (CH3 CO CH3). Chromatographically pure. 6.7 anhydrous sodium sulfate (Na2SO4). baked in a muffle furnace at 450 ° C for 2 h, cooled, stored in a ground glass bottle Sealed. 6.8 standard solution 6.8.1 Standard stock solution of polycyclic aromatic hydrocarbons. ρ=200μg/ml. Direct purchase of commercially available certified standard solutions, including naphthalene, terpenes, anthracene, anthracene, phenanthrene, anthracene, fluoranthene, anthracene, benzo[a] Bismuth, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]indole,indole[1,2,3-c,d]芘, dibenzo[a,h]蒽, Benzo[g,h,i] Hey. 6.8.2 Polycyclic aromatic hydrocarbon standard use solution. ρ = 20.0 μg/ml. Take 1.0ml of polycyclic aromatic hydrocarbon standard stock solution (6.8.1) in a 10ml volumetric flask and dilute to the mark with acetonitrile (6.1). Mix well. 6.9 Standard stock solution of decafluorobiphenyl. ρ=1000μg/ml. Alternatives, other analogs may also be employed. Commercially available certified standard solutions can be purchased directly or formulated with standard materials. 6.10 Standard use solution of decafluorobiphenyl. ρ=40.0μg/ml. Measure 1.0 ml of the decafluorobiphenyl standard stock solution (6.9) in a 25 ml volumetric flask, dilute to the mark with acetonitrile, and mix. Note 1. All standard solutions (6.8, 6.9, 6.10) are transferred to screw glass bottles with Teflon liner, and protected from light below 4 °C. refrigeration. 6.11 Sample extract. (1 9) (V/V) ether/n-hexane mixed solution. 6.12 Eluent 6.12.1 Column Eluent. 2 3 (V/V) dichloromethane/n-hexane mixed solution. 6.12.2 Solid phase column eluent. 1 1 (V/V) dichloromethane/n-hexane mixed solution. 6.13 particulate matter sampling material 6.13.1 Ultra-fine glass (or quartz) fiber filter. Select other sizes of filter according to the sampling flow rate. Filter pair 0.3μm The retention efficiency of the standard particles is not less than 99%, and the resistance of the single filter is not more than 3.5 KPa at a gas flow rate of 0.45 m/s. At this air flow rate, the air purified by the high efficiency filter is extracted for 5 hours, and the weight loss per square centimeter is not more than 0.012 mg. Make Preserved in the filter cartridge before use, to ensure that the filter is not stained before and after sampling, and is flat without being folded before sampling. state. 6.13.2 Treatment method of glass (or quartz) fiber filter. wrap the filter with aluminum foil and leave an opening for the muffle furnace Heat at 400 ° C for 5 h, and pay attention to the filter can not have creases. The treated filter membrane is wrapped in aluminum foil and sealed. From each batch The polycyclic aromatic hydrocarbons blank experiment was sampled in the filter. 6.13.3 Ultra-fine glass fiber filter cartridge or quartz filter cartridge. The retention efficiency of 0.5μm standard particles is not less than 99.9%. before use Heated in a muffle furnace at 600 ° C for more than 6 h, cooled, sealed and stored to ensure that the filter cartridge has no creases. 6.14 Adsorption resin. XAD-2 resin, styrene-divinylbenzene polymer. Treatment method of XAD-2 macroporous resin. After refluxing with dichloromethane (6.3) for 16 h before use, replace the dichlorocarb. The alkane was continuously refluxed for 16 h, and then refluxed with a 9 (v/v) diethyl ether/n-hexane mixed solution (6.11) for 16 h, and then placed. The solvent was evaporated in a fume hood (or vacuum dried at 50 ° C for 8 h). Store in a clean wide-mouth glass bottle and store in a sealed container. 6.15 Polyurethane foam (PUF). polyether type, density 22 ~ 25mg/cm3, cutting growth 10mm ~ 20mm The cylindrical shape (diameter is determined according to the specifications of the glass sampling cylinder). PUF treatment method. wash with distilled water before the first use, drain the water, replace the water with acetone (6.6), clear Wash three times, and then extract with acetone for 16h, and then extract the ether/n-hexane mixture of 1 9 and reflux for 16h, and replace with new one. The ether/n-hexane mixed solution was refluxed 2 to 3 times, and refluxed for 16 hours each time. Then take it out and dry the solvent (or blow dry with nitrogen). It can also be dried under vacuum at 50 ° C for 8 h). Wrap it in aluminum foil and store in a suitable container. If necessary, use acetone PUF is returned and the solvent is evaporated. Commercially available pretreated PUFs can be purchased. Pretreatment can also be carried out by other methods such as rapid solvent extraction (ASE), automatic Soxhlet extraction, and the like. Note 2. After purification, use PUF, XAD-2 resin and glass fiber filter (or filter cartridge) blank naphthalene, phenanthrene < 50ng, other polycyclic aromatic Hydrocarbon < 10 ng. 6.16 Silica gel, for chromatography, 100-200 mesh. Before use, it is baked in a shallow dish at 130 ° C for 16 h and cooled in a desiccator. Then, put it in a glass bottle for later use. If necessary, dilute the silica gel with methylene chloride before activation. 6.17 Silica gel column. 1000mg/6.0ml, or a commercial silica gel column of suitable capacity according to the impurity content. 6.18 Florisil column. 1000 mg/6.0 ml, or a commercial Florisil column of suitable capacity based on the impurity content. 6.19 Glass wool. Dip in dichloromethane before use, remove the solvent and store in a sealed form. 6.20 Nitrogen, purity ≥99.999%, for dry concentration of the sample.

7 Instruments and equipment

7.1 Liquid Chromatograph (HPLC). with adjustable wavelength UV detector or fluorescence detector and gradient elution. 7.2 Column. C18 column, 4.60mm × 250 mm, reversed-phase column with a particle size of 5.0μm or other similar properties Column. 7.3 Ambient air sampling equipment The sampling device consists of a sampling head, a sampling pump and a flow meter. 7.3.1 Sampling pump. It has automatic accumulative flow, automatic timing, and power-off re-start function. Under normal sampling conditions, large flow rate The sample load can reach more than 225L/min, and the medium flow sampler load can reach more than 100L/min. Able to bring the environment Air is drawn into the glass fiber filter and the adsorbent material behind it (including polyurethane foam XAD-2 resin polyurethane foam) At the beginning, at least 144 m3 of air sample can be collected during 24 hours of continuous sampling. 7.3.2 Sampling head. It consists of two parts. filter cartridge and sorbent sleeve. See Figure 1 for details. The sampling head is equipped with different cutters. Collect TSP, PM10 or PM2.5 particles. 7.3.2.1 Filter cartridges include filter holders, filters and stainless steel screens. The filter holder is made of metal and can A glass (or quartz) fiber filter is attached through a stainless steel mesh support. 7.3.2.2 Adsorbent sleeve The outer cylinder is made of Teflon or stainless steel with a glass sampling cylinder inside. Figure 1 Schematic diagram of the sampling head 7.3.2.3 Glass sampling cylinder. The bottom is supported by stainless steel mesh or 1G glass core panel. The upper and lower layers in the sampling cylinder are at least thick It is a 1cm PUF (6.15) with a XAD-2 macroporous resin (6.14) with a height of about 5 cm. Glass sampling cylinder The seal is fixed between the filter holder and the sampling pump. When sampling, it is loaded into the adsorbent sleeve on the sampling head, and its inlet and filter are solid. The rack connection is connected, and the air outlet is connected to the sampling pump. After sampling, the sampling cylinder can be directly placed in the Soxhlet extractor for reflux extraction. Before sampling, After that, the sampling cylinder is wrapped in aluminum foil paper and placed in the sampling cylinder box to ensure that the glass sampling cylinder and the adsorbent inside it are sampled. After being tarnished. 7.3.3 Flowmeter. The flow rate can be set to not less than 100 L/min. The sampling flow rate is calibrated with a standard flowmeter before sampling. 7.4 Fixed source exhaust sampling equipment Simultaneous collection of polycyclic aromatic hydrocarbons in gas phase and particulates is possible with the recommended instruments in HJ/T 365, which consist of sampling Pipes, filter cartridges, gas phase adsorption units, condensing units, flow meters and control devices are shown in Figure 2. Only the polycyclic aromatic hydrocarbons in the exhaust gas particles of the fixed pollution source can be collected, and the HJ/T 48-compliant soot sampler can be used. 7.4.1 Cartridge (or filter) bracket. The filter cartridge (or filter) bracket is made of borosilicate glass or quartz glass, the size is Matching with the filter cartridge (or filter) should facilitate the pick-and-place of the filter cartridge (or filter), and the interface is well sealed. 7.4.2 Vapor adsorption unit with condensing unit. The condensing unit is used to separate and store the condensed water in the exhaust gas for storage. The volume of the condensate container should be no less than 1L. The gas phase adsorption unit generally has an inner diameter of 30 mm to 50 mm and a length of 70 mm. A glass tube of.200 mm and a capacity of 100 mm to 150 mL can be loaded with an adsorption column of 20 g to 40 g of XAD-2 and PUF. 7.4.3 Flow metering and control devices. devices for indicating and controlling the sampling flow, capable of monitoring dynamic pressure, static pressure, Pre-test temperature, pre-meter pressure, flow rate and other parameters. The flow meter should have an accumulative flow meter that automatically performs temperature and pressure correction. The sample flow should be calibrated using a standard flow meter before sampling. Figure 2 Schematic diagram of exhaust gas polycyclic aromatic hydrocarbon sampling device 1-flue; 2-thermocouple or RTD thermometer; 3-pilot; 4-sampling tube; 5-cartridge (or membrane); 6- with condensing unit Gas phase adsorption unit; 7-micro pressure sensor; 8-pressure sensor; 9-temperature sensor; 10-flow sensor; 11-flow regulating device; 12-sampling pump; 13-microprocessing system; 14-micro printer or interface; 15-display 7.4.4 Sampling pump. The pump's no-load pumping flow should be no less than 6L/min. When the sampling system load resistance is 20kPa, the flow The amount should be no less than 30L/min. 7.5 Soxhlet extractor. 1 or 2 of.2000 ml for purification of adsorbent; several for 500ml or 1000ml, For extracting samples. Other equivalent extraction devices can also be used. 7.6 Constant temperature water bath. The temperature control accuracy is ±5 °C. 7.7 Concentration device. A device with equivalent performance such as a rotary evaporator or a KD concentrator or an organic sample concentrator. 7.8 Solid phase extraction purification device. 7.9 Glass column. glass column with a length of 350 mm and an inner diameter of 20 mm and a PTFE piston at the bottom. 7.10 Microinjectors. 10 μl, 50 μl, 100 μl, 250 μl. 7.11 Hermetic syringe. 500μl, 1000μl. 7.12 Common instruments used in general laboratories.

8 samples

8.1 Sample Collection Polycyclic aromatic hydrocarbons above the five rings are mainly present on the particulate matter and can be collected by a glass (or quartz) fiber filter/filter cartridge; Bicyclic and tricyclic polycyclic aromatic hydrocarbons are mainly present in the gas phase and can pass through glass (or quartz) fiber membranes/filter cartridges. XAD-2 can be used. Resin and polyurethane foam (PUF) collection; tetracyclic polycyclic aromatic hydrocarbons exist at the same time, must use glass (or quartz) fiber Samples were taken from the UF membrane/cylinder, resin and polyurethane foam. 8.1.1 Collection of ambient air samples Before the sampling on site, the flow rate of the sampler should be corrected. Install the filter clamp and the adsorbent sleeve in turn, and connect to the sampling. To adjust the sample flow and start sampling. After sampling, open the filter clip on the sampling head and gently remove the filter with tweezers. The sampling surface is folded in half, and the sampling cylinder is taken out from the adsorbent sleeve, and wrapped with aluminum foil paper together with the folded-fold filter membrane, and placed in the original Sealed in the box. Flow correction after sampling. 8.1.2 Sample collection of fixed source exhaust Install the filter cartridge (6.13.3) and the vapor phase adsorption unit (7.4.2) with the condensing unit, connect the instrument, and sample the tube. Insert the flue from the sampling hole, place the sampling nozzle on the measuring point, face the airflow, start the sampling pump, adjust the suction speed of the sampling nozzle and The airflow velocity at the measuring point is equal (the relative error is controlled within 10%), and the constant velocity sampling flow is adjusted every 60 minutes. If the resistance of the filter cartridge increases until the constant velocity sampling cannot be maintained, replace the new filter cartridge and continue sampling. After reaching the required sample size, Quickly withdraw the sampling tube, stop the sampling pump at the same time, and record parameters such as start and stop time or sample volume. When collecting only the particulate matter in the fixed source exhaust gas, the particulate matter in the exhaust gas of the fixed pollution source is measured and the sample of the gaseous pollutant is sampled. The method (GB/T 16157) is used for sampling. 8.2 Storage of samples. After sample collection, it should be kept away from light below 4 °C, and extracted within 7 days; or stored below -15 °C, and completed within 30 days. take. 8.3 Sample preparation 8.3.1 Extraction. Place the glass fiber filter (or filter cartridge), the glass sampling cylinder filled with resin and PUF into the Soxhlet extractor, in PUF Add 0.1ml of decafluorobiphenyl solution (6.10), add appropriate amount of 1 9 (v/v) ether/n-hexane extract (6.11), per The hourly reflux is not less than 4 times and the speed is extracted for 16 hours. After the reflux is completed, cool to room temperature, remove the bottom bottle, clean the extractor and connect At the mouth, transfer the cleaning solution to the bottom bottle, add anhydrous sodium sulfate (6.7) to the extract to the sodium sulfate particles. Flow, place for 30 min, dehydrate and dry. Transfer the condensate from the fixed source to the separatory funnel, rinse the condensate collection bottle with n-hexane (6.4), and turn Transfer to a separatory funnel, extract with n-hexane or dichloromethane (6.3), and combine the extract with the extract from the bottom bottle. Note 3. Other sample extraction methods may be used as long as the quality control requirements specified in this standard can be met. Automatic Soxhlet extraction using the above mentioned Take liquid (6.11) reflux extraction for 40 cycles; fast solvent extraction reference conditions. temperature 100 ° C, pressure 1500~2000 Psi, static extraction Between 5 min, rinse volume 60% pool volume, nitrogen purge for 60 s, static extraction times 2 times. 8.3.2 Concentration. Transfer the extract to a concentrated bottle and concentrate to 1 ml at 45 ° C or lower with a concentration device (7.7). For purification, add 5-10ml of n-hexane, repeat the concentration process 3 times, completely convert the solvent to n-hexane, and finally concentrate Reduce to 1ml, to be purified. If no purification is required, concentrate to 0.5-1.0ml, add 3ml acetonitrile, and concentrate to less than 1ml. The solvent was completely converted to acetonitrile, and finally the volume was determined to be 1.0 ml to be tested. Prepared samples are stored refrigerated below 4 ° C, 30 The analysis was completed within the day. 8.3.3 Purification 8.3.3.1 Silica gel column purification The glass chromatography column (7.9) was sequentially filled with glass wool, and 10 g of silica gel (6.16) was wet-filled with methylene chloride as a solvent. After filling 1~2cm high anhydrous sodium sulfate. After the column is installed, rinse the column twice with 20-40 ml of dichloromethane to ensure the liquid level. Keep above the surface of sodium sulfate, do not drain, rinse the column with 40 ml of n-hexane, and close the piston. Concentrated Transfer the sample extraction solution to the column, wash the sample bottle with about 3 ml of n-hexane, transfer to the column, and discard. Effluent. The column was eluted with 25 ml of n-hexane and the effluent was discarded. Use 30 ml of dichloromethane/n-hexane eluent (6.12.1) The column was eluted and the effluent was received at a flow rate of 2 to 5 ml/min. Transfer the eluate...

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