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HJ 869-2017 English PDF

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HJ 869-2017: Stationary source emission. Determination of phthalate esters. Gas chromatography
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HJ 869-2017English349 Add to Cart 3 days [Need to translate] Stationary source emission. Determination of phthalate esters. Gas chromatography Valid HJ 869-2017

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HJ 870   GB/T 15516   GB/T 14675   HJ 868   HJ 867   

Basic data

Standard ID HJ 869-2017 (HJ869-2017)
Description (Translated English) Stationary source emission. Determination of phthalate esters. Gas chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z15
Classification of International Standard 13.040.40
Word Count Estimation 15,126
Date of Issue 2017-11-28
Date of Implementation 2018-01-01
Quoted Standard GB/T 16157; HJ/T 48; HJ/T 373; HJ/T 397
Regulation (derived from) Ministry of Environmental Protection Announcement 2017 No. 59
Issuing agency(ies) Ministry of Ecology and Environment
Summary The current standard specifies the gas chromatographic method for the determination of phthalate ester compounds in exhaust emissions from fixed sources of pollution. This standard applies to dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, and phthalic acid two (2) (Ethylhexyl) ester and di-n-octyl phthalate - Determination of six phthalates. If verified, this standard also applies to the determination of other phthalate esters. When the sampling volume is 1m^(3) (dry sample volume in the standard state), the detection limit of the method is 0.4 ~ 0.8��g/m ^ (3) The lower limit of determination is 1.6 ~ 3.2��g/m ^ (3). See Appendix A for details.

HJ 869-2017: Stationary source emission. Determination of phthalate esters. Gas chromatography


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(Stationary sources - Determination of phthalates esters - Gas chromatography) People's Republic of China national environmental protection standards Stationary sources - Determination of phthalates Gas chromatography Stationary source emission-Determination of phthalate esters -Gas chromatography 2017-11-28 Posted 2018-01-01 implementation Ministry of Environmental Protection released i directory Preface ... ii 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 ... 3 7 samples ... 4 8 Analysis step ... 6 This standard is interpreted by the MEP. Stationary sources - Determination of phthalates - Gas chromatography Warning. The solvents and reagents used in this method have some toxicity. The sample preparation process should be carried out in a fume hood and worn as required Protective equipment to avoid contact with skin and clothing.

1 scope of application

This standard specifies the determination of fixed sources of emissions of organized emissions of phthalates ester gas chromatography. This standard applies to fixed sources of emissions of organized emissions of dimethyl phthalate, diethyl phthalate, phthalate two Butyl phthalate, butyl benzyl phthalate, di-2-ethylhexyl phthalate and di-n-octyl phthalate were measured. If verified, this standard also applies to the determination of other phthalates. The detection limit of the method is 0.4 μg/m3 ~ 0.8 μg/m3 when the sampling volume is 1 m3 (dry sampling volume in the standard state) The limit is 1.6 μg/m3 ~ 3.2 μg/m3. See Appendix A for details.

2 Normative references

This standard references the following documents in the terms. For undated references, the effective version applies to this standard. Determination of Particulate Matter and Gaseous Pollutants in Exhaust of Fixed Pollution Sources GB/T 16157 HJ/T 48 dust sampler technical conditions HJ/T 373 fixed pollution source monitoring quality assurance and quality control technical specifications (Trial) HJ/T 397 fixed source exhaust gas monitoring technical specifications

3 method principle

Constant-speed sampling mode, so that fixed sources of exhaust through the heated sampling tube, cooling device and the resin column, particulate and gas phase Of the phthalates were collected on glass (or quartz) fiber filters (or cartridges) and XAD-2 resin, respectively, while the condensate was collected. The filter (or cartridge) and XAD-2 resin were extracted with ether-n-hexane mixed solution, the condensate was extracted with n-hexane, the extract was concentrated, the net After purification, with hydrogen flame ionization detector gas chromatography detection, according to retention time qualitative, internal standard method or external standard method.

4 Interference and elimination

Purification using a magnesium silicate column removes or reduces interference as detailed in 7.3.3.

5 Reagents and materials

Unless otherwise specified, the analysis of analytical reagents are used in line with national standards of analytical chemistry, experimental water is freshly prepared pure water. 25.1 Dichloromethane (CH2Cl2). Chromatographic purity. 5.2 n-Hexane (C6H14). Chromatographic purity. 5.3 ether (C4H10O). Chromatography. 5.4 Acetone (C3H6O). Chromatography pure. 5.5 Anhydrous sodium sulfate (Na2SO4). Bake in a muffle furnace at 450 ° C for 4 h before use, cool, and seal in a milled glass jar. 5.6 ether - n-hexane mixed solution. 1 9, Pro use now with. 5.7 ether - n-hexane mixed solution. 2 8, Pro use now. 5.8 acetone - n-hexane mixed solution. 1 9, Pro use now. 5.9 Dichloromethane - n-hexane mixed solution. 2 8, Pro use now. 5.10 diphenyl phthalate (C20H14O4). purity of 98% or more. Alternatives may also be used. 5.11 Substitute stock solution. ρ =.2000 μg/ml. Weigh diphenyl phthalate (5.10) 0.1 g (accurate to 0.1 mg), in a 50 ml volumetric flask, add a little acetone (5.4) Dissolve and dilute to volume with n-hexane (5.2) and mix well. 4 ℃ the following sealed. 5.12 Alternative use solution. ρ = 80.0 μg/ml. Pipette 1.00 ml of stock solution (5.11) into a 25 ml volumetric flask, dilute with n-hexane (5.2) and mix well. 4 ℃ below the dense Save sealed. 5.13 Benzyl benzoate (C14H12O2). purity of 98% or more. Internal standard, can also use other analogues. 5.14 Internal standard solution. ρ =.2000 μg/ml. Weigh benzyl benzoate (5.13) 0.1 g (accurate to 0.1 mg), in a 50 ml volumetric flask, add a small amount of methylene chloride (5.1) dissolved Solution and n-hexane (5.2) constant volume, mix well. 4 ℃ the following sealed. 5.15 phthalate standard stock solution. ρ =.2000 μg/ml. Direct purchase of a certified commercial standard solution, including dimethyl phthalate, diethyl phthalate, dibutyl phthalate, o Butyl benzyl phthalate, di (2-ethylhexyl) phthalate and di-n-octyl phthalate, the solvent is n-hexane, the following 4 ℃ dense Seal preservation, or reference standard solution certificate preservation. 5.16 phthalate mixed standard solution. ρ = 80.0 μg/ml. Remove phthalate standard stock solution (5.15) and replacement stock solution (5.11) 1.00 ml in 25 ml volumetric flask with n-hexane (5.2) constant volume, mix well. 4 ℃ the following sealed. 5.17 Magnesium silicate. 150 μm to 250 μm (100 mesh to 60 mesh). Before use, weighed 100 g ± 10 g into the evaporating dish, heated at 140 ℃ for 16 h, while hot transfer to 500 ml grinding mouth reagent bottle, Capped, cooled to room temperature, add 3.0 ml ± 0.1 ml experimental water, sealed, shake thoroughly mixed 10 min, allowed to stand for 2 h before use. 5.18 Magnesium silicate solid phase extraction column. 1000 mg/6 ml, but also according to the content of impurities to select the appropriate volume of commercial magnesium silicate SPE column. 5.19 glass (or quartz) fiber filter (or no filter cartridges). The retention efficiency of 0.3 μm standard particles of not less than 99%. Before use in a muffle furnace at 500 ℃ heating 6 h or more, cooling, to avoid direct contact with the plastic, sealed, guaranteed before use 3 creases. 5.20 XAD-2 resin (styrene-divinylbenzene polymer). 250 μm to 840 μm (60 mesh to 20 mesh). Before using, refluxing with dichloromethane (5.1) for 16 h, replacing dichloromethane and refluxing for 16 h and then ether-n-hexane The combined solution (5.6) refluxed for 16 h, vacuum dried at room temperature for 2 h ~ 3 h, sealed in a glass bottle. 5.21 Nitrogen. Purity ≥99.999%. 5.22 glass wool. Before use with dichloromethane (5.1) reflux extraction 2 h ~ 4 h, dried and sealed. 5.23 Color Silica. 1180 μm ~ 3350 μm (16 mesh ~ 6 mesh).

6 instruments and equipment

6.1 Gas Chromatograph. with Split/Splitless Inlet, Temperature Programmable, and Flame Ionization Detector. 6.2 Column. Quartz capillary column, 30 m (length) × 0.25 mm (ID) × 0.25 μm (film thickness) with 5% phenyl 95% dimethylpolysiloxane, 35% phenyl 65% dimethylpolysiloxane or 14% cyanopropylphenyl 86% dimethylpolysiloxane or the like Columns. 6.3 Sampling equipment. including combination sampling tube, filter (or cartridge) holder, cooling device, resin column and condensate receiving bottle, flowmeter Quantity and control devices and sampling pump and other parts, shown in Figure 1. Determination of fixed sources of exhaust particulate matter phthalates, should be used in line with HJ/T 48 Soot sampler. 6.3.1 Combination sampling tube. including sampling tube, S-type pitot tube and thermal resistance (or thermocouple). Sampling tube with heating device, heating temperature Degree of 105 ℃ ~ 125 ℃. If the exhaust temperature exceeds 500 ° C, use a sampling tube with a cooling jacket. Sampling tube outer tube material is stainless Steel, the inner tube material is borosilicate glass, quartz glass or titanium alloy metal, the inner surface is smooth. 6.3.2 Filter (or filter cartridge) Bracket. Made of Teflon, stainless steel or titanium alloy, with heating device, heating temperature is 105 ℃ ~ 125 ° C. 6.3.3 Cooling Device, Resin Column and Condensate Receiving Bottle. The cooling device includes a condenser (with a cooling water circulation pump or an electronic cooling device) And cooling water tank. Condenser for condensation into the XAD-2 resin column of high temperature gas, the condenser material is glass or quartz and other non-adsorption of organic matter The cooling water circulation pump can provide ice water to flow through the condenser and the resin column water jacket to keep the temperature below 30 ° C before the gas enters the resin column. The cooling water is ice water or provided by the refrigerator; the impact bottle volume in the cooling water tank is 500 ml, the impact bottles a and b are equipped with 100 ml water and the impact bottle c For the buffer bottle; resin column diameter of 30 mm ~ 50 mm, length of 70 mm ~.200 mm, can be filled with XAD-2 resin (5.20) 10 g ~ 40 g; condensate receiver bottle is 1 L brown glass bottle. 6.3.4 Flow measurement and control device. S-type pitot tube capable of monitoring dynamic pressure and static pressure in real time, capable of indicating and controlling the sampling flow rate Of the device, with real-time monitoring and display of temperature sensors, flowmeter at the same time monitor and display the flow, pre-temperature, pre-pressure and other parameters. Flowmeters have a built-in flowmeter with automatic temperature and pressure correction, and the flowmeter should be calibrated before sampling. 6.3.5 Sampling pump. The suction capacity should be able to overcome the exhaust pipe negative pressure and sampling system resistance, when the sampling system load resistance of 20 kPa, the flow The amount should not be less than 30 L/min. Soxhlet extractor. 500 ml. Other performance extraction devices may also be used. 6.5 Glass Column. 350 mm long, 20 mm id, glass column with Teflon piston on the bottom. 6.6 Concentration device. Rotary evaporator, nitrogen purifier or other performance-equivalent equipment. 46.7 Solid phase extraction device. 6.8 General laboratory equipment commonly used. 1-Exhaust gas cylinder; 2-Thermocouple or RTD; 3-S pitot tube; 4-Sampling pipe; 5-Filter (or cartridge) holder; 6-Condenser; Resin column 8 condensate receiving bottle 9 circulation pump 10 flow sensor 11 flow regulating device 12 sampling pump 13 micro-processing system System 14 mini printer or interface 15 display 16 micro pressure sensor 17 pressure sensor 18 temperature sensor Figure 1 sampling device schematic

7 samples

7.1 sample collection 7.1.1 Sampling preparation Data collection before sampling and on-site investigation to confirm the sampling site in line with the basic requirements of sampling. Sampling tube, filter (or cartridge) bracket, Condenser and condensate receiving bottles, etc. followed by acetone, n-hexane rinse, sealed and brought to the scene. 7.1.2 Sampling steps According to HJ/T 397 requirements sampling location selection, set up sampling holes to determine the location and number of sampling points. The sampling tube into the exhaust tube, Determination of exhaust parameters, select the appropriate sampling nozzle. Install the sampling nozzle, according to Figure 1 connected to the sampling device, in accordance with GB/T 16157 sampling system tightness inspection. Set the sampling time for each sampling point, insert the sampling tube into the exhaust tube, and seal the sampling hole so that the sampling nozzle and the pitot tube are in full pressure Airflow, located at the first sampling point. Open the sampling tube, filter (or cartridge) heating function and circulating pump refrigeration function, to reach the desired temperature, Start the sampling pump and start sampling. The first sampling end, move to the second sampling point to continue, the order of sampling at each point. Sampling process should be guaranteed Hold constant speed sampling. Sampling end, take out the sampling tube, remove the filter, dust inward, wrapped with aluminum foil; filter cartridge removed, the cartridge mouth folded inward, with aluminum 5 foil wrapped into the sample box vertically. The XAD-2 resin column sealed at both ends, placed in a special container for storage; condensate transfer to brown glass Bottle save. Record exhaust parameters (temperature, dynamic pressure, static pressure, etc.), the cumulative sampling time and the cumulative standard dry sampling volume. Note. If it is not suitable for constant-speed tracking sampling due to unstable flow rate or eddy current at the sampling point, the constant flow rate is 20 L/min ~ 30 L/min Sampling 7.2 Sample preservation After the sample is collected, it should be sealed and refrigerated below 4 ℃, and extracted within 7 days. The sample extract should be stored at below 4 ℃ and stored within 40 days Analysis of ingredients. 7.3 Sample Preparation 7.3.1 Sample Extraction The filter (or cartridge), the resin column XAD-2 resin was transferred to the extraction cup cannula, with a certain amount of ether - n-hexane mixed solution (5.6) The resin column is eluted and the eluent is transferred to the extractor bottoms. The surface of the resin is covered with glass wool (5.22), and 250 μl of the alternative use solution is added (5.12), add the appropriate amount of ether - hexane mixed solution (5.6), reflux extraction more than 16 h, hourly refluxed not less than 4 times. extract After cooling down to room temperature, remove the bottom bottle, clean the extractor and the interface, and transfer the cleaning liquid to the bottom bottle together. The extract was added to anhydrous sulfuric acid Sodium (5.5) to sodium sulfate particles are free-flowing and are allowed to settle for 30 minutes to dry. The condensate from the fixed source exhaust gas is transferred to a separatory funnel, and the condensate preservative bottle is rinsed with n-hexane and transferred to a separatory funnel, Per liter of condensate was added 50 ml of n-hexane (5.2) the proportion of extraction 2 to 3 times, the extract was dehydrated with the filter (or cartridge) and XAD-2 The resin extracts are combined. Note 1. As long as the quality control requirements of this standard can be achieved, other sample extraction methods may also be adopted. Note 2. If the XAD-2 resin contains moisture, rinse with acetone and transfer to the extraction cup. If the moisture content is high, transfer the extract to a separatory funnel and add The experimental water, shaking 3 min, standing stratification, the organic phase was added anhydrous sodium sulfate (5.5) dehydration and drying. 7.3.2 Sample concentration The sample extract was transferred to a concentration device, concentrated to about 1 ml below 45 ℃, to be purified. 7.3.3 Sample Purification 7.3.3.1 Magnesium silicate column The bottom of the glass column (6.5) is stuffed with glass wool (5.22), 2 cm of anhydrous sodium sulfate (5.5) is added and n-hexane (5.2) is dissolved Agent wet fill 10 g magnesium silicate (5.17), discharge bubbles, the upper part by adding 1 cm ~ 2 cm anhydrous sodium sulfate. Pre-pour with 40 ml of n-hexane Wash the column, control the flow rate 2 ml/min, keep the liquid level slightly higher than the column bed, transfer the concentrated liquid (7.3.2) to the column and wash with 1 ml The sample bottle was washed twice with n-hexane and transferred to a chromatographic column. The column was eluted with 40 ml of n-hexane and the eluate discarded. The column was eluted with.200 ml diethyl ether-n-hexane mixed solution (5.7) at an elution rate of 2 ml/min to 5 ml/min to receive the eluate. Eluate (7.3.2) concentrated to 1 ml or less, with n-hexane to 1.0 ml. If using internal standard quantification, add 10.0 μl internal standard Use liquid (5.14) and transfer to vial for analysis. 7.3.3.2 Magnesium silicate solid phase extraction column Take solid-phase extraction column (5.18), followed by 10 ml of acetone - n-hexane mixed solution (5.8), 10 ml of n-hexane (5.2) 6-phase extraction column, discard the effluent. Keep the liquid level just above the bed and transfer the extract concentrate (7.3.2) to the column and wash with 1 ml n-hexane (5.2) The sample bottle was washed twice and transferred to the column, which was washed with 5 ml n-hexane, 10 ml dichloromethane-n-hexane mixed solution (5.9) Phase extraction column, discard the effluent. Elute with 10 ml of acetone-n-hexane mixed solution (5.8) and receive the eluate. The eluent was concentrated as in (7.3.2), washed with n-hexane (5.2) Set the volume to 1.0 ml. If using internal standard quantification, add 10.0 μl of internal standard solution (5.14) and transfer to vial for analysis. Note. the purification process to keep the liquid level is not less than the bed; each batch of activated magnesium silicate need to be spiked experiment to determine the amount of elution solvent; as long as this standard can be achieved Set the quality control requirements, but also the use of other sample purification methods. 7.4 Preparation of blank samples Take and sample the same batch of XAD-2 resin, filter (or cartridge) and the same volume of water with the test water, according to the sample system Prepare laboratory blank samples with the same procedure (7.3).

8 Analysis steps

8.1 Instrument reference conditions Inlet temperature. 250 ℃; Injection mode. split injection, split ratio 5. 1; injection volume. 1.0 μl; column temperature. 50 ℃ for 1 min, The temperature was raised to 270 ° C at 10 ° C/min for 1 min and the temperature was raised to 300 ° C at 10 ° C/min for 1 min. The carrier gas was nitrogen (5.21) Flow rate. 1.0 ml/min; temperature of hydrogen flame ionization detector (FID). 300 ° C .; hydrogen flow rate. 30 ml/min; air flow rate. 450 ml/min; Makeup gas. 60 ml/min. 8.2 standard curve drawing Pipette a standard amount of phthalate ester standard solution (5.16) and dilute with n-hexane (5.2) to prepare a standard set of at least 5 concentration levels Column, the mass concentration of 2.0 μg/ml, 5.0 μg/ml, 10.0 μg/ml, 20.0 μg/ml and 40.0 μg/ml. If using internal standard method, For each 1.0 ml of standard solution, add 10.0 μl of internal standard solution (5.14) accurately. From low concentration to high concentration gas chromatograph, press the instrument Reference conditions (8.1) were analyzed to obtain the chromatograms of different concentrations of the target compound, record retention time, peak area (or peak height). The concentration of the target compound (or the concentration of the internal standard compound) as the abscissa, corresponding to the target compound peak area or peak height (or And internal standard compound peak area or peak height ratio) for the vertical axis, using the least squares method to draw the standard curve. Phthalates standard chromatogram see Appendix C. 8.3 Determination of the sample Assay the sample according to the same instrument conditions as the standard curve. Record the peak retention time and peak area (or peak height). 8.4 Blank test The blank sample (7.4) was measured according to the same instrument conditions as the sample.

9 results calculated and expressed

9.1 Qualitative analysis Qualitatively based on retention time, complex matrix samples were identified by gas chromatography-mass spectrometry or using another capillary of different polarity 7 column to aid characterization. 9.2 Quantitative analysis According to the peak area or peak height, the internal standard method or external standard method. 9.3 Results Calculation Calculate the mass concentration () of the target compound in the stationary source exhaust gas according to the formula (1). nd V) (0 (1) Where.  - Concentration of target compound in fixed pollutant exhaust gas, μg/m3; i - mass concentration of the target compound in the sample obtained from the standard curve, μg/ml; 0 - the mass concentration of the target compound in the laboratory blank, whichever is the blank mean, μg/ml; V - sample volume concentrated volume, ml; Vnd - Dry sample volume at standard conditions (101.325 kPa, 273 K), m3. 9.4 results indicated When the concentration of the target compound in the stationary source exhaust gas is greater than or equal to 10.0 μg/m3, the result retains three significant digits; less than 10.0 μg/m3, the result is retained to one decimal place. 10 precision and accuracy 10.1 Precision Six laboratories repeated the determination of six blank spike additions of 4.0 μg, 20.0 μg and 36.0 μg of sample (equivalent to the exhaust gas concentration 4.0 μg/m 3, 20.0 μg/m 3 and 36.0 μg/m 3). The relative standard deviations in the laboratory ranged from 1.4% to 18%, 3.1% to 12% and 4.2% The relative standard deviations (RSDs) were 3.9% ~ 14%, 3.4% ~ 7.8% and 3.5% ~ 6.6% respectively. The repeatability limits were 0.7 μg/m3 ~ 1.3 μg/m3, 2.8 μg/m3 ~ 3.4 μg/m3 and 5.8 μg/m3 ~ 6.5 μg/m3 with reproducibility limits of 0.7 μg/m3 ~ 1.8 μg/m3, 3.4 μg/m3 to 5.3 μg/m3 and 6.2 μg/m3 to 8.4 μg/m3. See Table B.1 for details. 10.2 Accuracy Six laboratories to extract the actual sample concentrate as a unified sample, the determination of six spike recoveries, with a standard addition of 10.0 μg (phase When the exhaust gas concentration is 10.0 μg/m3), the spiked recoveries ranged from 70.2% to 129%. The final spike recoveries were 83.9% 22.2% 112% 23%. See Table B.2 for details. 11 Quality Assurance and Quality Control 11.1 blank Each batch of samples does not exceed 20, with at least two laboratory blank, blank phthalate esters content does not exceed the lower limit of determination. air 8 white parallel double the relative deviation does not exceed 30%. 11.2 Calibration 11.2.1 Initial calibration The correlation coefficient of the standard curve ≥0.995, otherwise, draw the standard curve again. 11.2.2 Continuous calibration At least once every 24 h during the measurement of the sample A standard solution of the midpoint concentration of the curve, the measurement of the target compound and the standard value of The relative error should be within ± 20%, otherwise draw a new standard curve. 11.3 Internal standard Sample internal standard, continuous calibration of the internal standard curve and the midpoint of the internal standard comparison, the retention time does not exceed 10 s, the peak area or peak height Change -50% ~ 100%. 11.4 Recovery of Substitutes After extraction, purification, concentration and analysis process, the control range of the recovery rate of substitute is 60% ~ 150%. 11.5 Sampling Quality Control 11.5.1 Periodically meter, pitot tube, temperature sensor calibration. 11.5.2 The sampling nozzle should be inserted into the exhaust pipe backwards in the direction of the airflow. When sampling, align the airflow direction and the deviation of the angle should be less than 10 °. 11.5.3 Constant-rate sampling rate of tracking requirements of 1.0 ± 0.1; using a fixed flow sampling, the sampling should be repeated after the determination of exhaust flow rate, mining Changes in flow rate before and after the sample should be within ± 20%. 12 Waste treatment The wastes generated by the laboratory shall be stored in categories and centrally stored, entrusted to qualified units for disposal. 13 Precautions 13.1 The experimental process should avoid the use of plastic materials and other interference with the experimental materials and utensils. Glassware before use in chromic acid lotion Soaked in not less than 6 h, followed by water, acetone and n-hexane leaching; glassware placed for a long time before use must use organic solvents Rinse the surface; anhydrous sodium sulfate, filter (or cartridge) to be used after baking at high temperatures; sampling resin before extraction and purification, such as If you can not guarantee the preservation in a clean environment, to avoid prolonged storage in the laboratory. 13.2 If the discharge is intermittent, and the discharge time is greater than or equal to 1 h, or continuous exhaust emissions, sampling time of not less than 1 h; In the case of intermittent exhaust gases with an emission time of less than 1 h, continuous sampling is taken during the emission period. 13.3 sampling device connecting pipe made of PTFE or Viton. Pitot tubes before sampling, sampling system for air tightness check, such as If the system leaks, should be segment...

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