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HJ 868-2017 English PDF

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HJ 868-2017: Ambient air. Determination of phthalate esters. High performance liquid chromatography
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HJ 868-2017329 Add to Cart 3 days Ambient air. Determination of phthalate esters. High performance liquid chromatography Valid

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Basic data

Standard ID: HJ 868-2017 (HJ868-2017)
Description (Translated English): Ambient air. Determination of phthalate esters. High performance liquid chromatography
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z15
Classification of International Standard: 13.040.20
Word Count Estimation: 14,117
Date of Issue: 2017-11-28
Date of Implementation: 2018-01-01
Quoted Standard: HJ 691
Regulation (derived from): Ministry of Environmental Protection Announcement 2017 No. 59
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies high performance liquid chromatography for the determination of phthalate ester compounds in ambient air. This standard applies to dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate, butyl phthalate in the gas phase and particulates in ambient air. Determination of esters, di(2-ethylhexyl) phthalate and di-n-octyl phthalate. If verified, this standard also applies to the determination of other phthalate ester compounds. When the sample volume is 144 m^(3) (standard state) and the volume is 1.0 ml, the detection limit of the method is 0.002 ��g to 0.006 ��g/m^(3) The lower limit of determination is 0.008 to 0.024 ��g/m3. . See Appendix A for details.

HJ 868-2017: Ambient air. Determination of phthalate esters. High performance liquid chromatography


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(Ambient air - Determination of phthalates - High performance liquid chromatography) People's Republic of China national environmental protection standards Ambient air - Determination of phthalates High performance liquid chromatography Ambient air-Determination of phthalate esters -High performance liquid 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 9 Calculation and Expression of Results ... 7 10 Precision and accuracy ... 7 11 Quality Assurance and Quality Control ... 8 12 Waste Treatment ... 8 13 Notes ... 8 Appendix A (Normative) Detection limit and lower limit of the method ...9 Appendix B (informative) method of precision and accuracy ... 10

Foreword

In order to implement the Law of the People's Republic of China on Environmental Protection and the Law of the People's Republic of China on Prevention and Control of Atmospheric Pollution, protect the environment and protect people Health, standardize the determination of phthalates in ambient air, the development of this standard. This standard specifies the determination of high-performance liquid chromatography of phthalates esters in the air. This standard Appendix A normative appendix, Appendix B is an informative annex. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Shenyang Environmental Monitoring Center Station. This standard verification unit. Liaoning Province Environmental Monitoring Experimental Center, Dalian City Environmental Monitoring Center, Anshan City Environmental Monitoring Center Station, Fushun City Environmental Monitoring Center Station, Shenyang City Center for Disease Control and Prevention and Shenyang Environmental Protection Bureau Tiexi Branch Environmental Monitoring Station. This standard MEP approved on November 28,.2017. This standard since January 1,.2018 come into operation. This standard is interpreted by the MEP.

1 Ambient air phthalates Determination of high performance liquid 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 high-performance liquid chromatography of phthalates esters in the air. This standard applies to the ambient air in the gas phase and particulate matter dimethyl phthalate, diethyl phthalate, phthalic acid two different Butyl, dibutyl phthalate, butyl benzyl phthalate, di (2-ethylhexyl) phthalate and di-n-octyl phthalate A total of 7 phthalates Determination. If verified, this standard also applies to the determination of other phthalate compounds. When the sampling volume is 144 m3 (standard state) and the volume of concentrated volume is 1.0 ml, the detection limit of this method is 0.002 μg/m3 ~ 0.006 μg/m3, and the lower limit of determination is 0.008 μg/m3 ~ 0.024 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. HJ 691 Environmental airborne semi-volatile organic compounds sampling techniques

3 method principle

Phthalates in ambient air are collected on glass (or quartz) fiber filters using a medium- or high-flow sampler. Polyurethane foam (PUF) and XAD-2 resin, extracted with a mixture of ether and n-hexane, the extract was concentrated, purified, with a UV detector HPLC separation test, according to the retention time of qualitative, 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, analytical grade analytical reagents used in accordance with national standards were used. Experimental water is freshly prepared ultrapure water. 5.1 Dichloromethane (CH2Cl2). Chromatographic purity. 5.2 n-Hexane (C6H14). Chromatographic purity. 5.3 ether (C4H10O). Chromatography. 5.4 Acetone (C3H6O). Chromatography pure. 5.5 Acetonitrile (CH3CN). Chromatographic purity. 5.6 Anhydrous sodium sulfate (Na2SO4) Bake in a muffle furnace at 450 ℃ for 4 h before use, cool, and store in sealed glass jar. 25.7 ether - n-hexane mixed solution. 1 9, Pro use now with. 5.8 ether - n-hexane mixed solution. 2 8, Pro use now. 5.9 acetone - n-hexane mixed solution. 1 9, Pro use now. 5.10 methylene chloride - n-hexane mixed solution. 2 8, Pro use now. 5.11 diphenyl phthalate (C20H14O4). purity of 98% or more. Alternatives may also be used. 5.12 Substitute stock solution. ρ =.2000 μg/ml. Weigh about 0.1 g of diphenyl phthalate (5.11), accurate to 0.1 mg, dissolved in acetonitrile (5.5) in a 50 ml volumetric flask And set the volume, shake well. 4 ℃ the following sealed. Can be purchased directly from the market certified standard solution, reference standard solution certificate for preservation. 5.13 Alternative solution. ρ = 80.0 μg/ml. Pipette 1.00 ml of stock solution (5.12) into a 25 ml volumetric flask, dilute to volume with acetonitrile (5.5) and mix well. 4 ℃ below the dense Save sealed. 5.14 Diisobutyl phthalate Standard substance. purity 98% or more. 5.15 Diisobutyl phthalate standard stock solution. ρ =.2000 μg/ml. Weigh about 0.1 g of diisobutyl phthalate (5.14), accurate to 0.1 mg in a 50 ml volumetric flask, dissolve it in acetonitrile (5.5) Solution and set the volume, shake well. Can be purchased directly from the market certified standard solution. 4 ℃ the following sealed. 5.16 6 phthalates standard stock solution. ρ =.2000 μg/ml. Buy a commercially available standard solution of acetonitrile or methanol as a solvent, including dimethyl phthalate, diethyl phthalate, Dibutyl phthalate, butyl benzyl phthalate, di-2-ethylhexyl phthalate and di-n-octyl phthalate. 4 ° C The following seal preservation, or reference standard solution certificate to save. 5.17 8 phthalates standard solution. ρ = 80.0 μg/ml. Pipette 1.00 ml stock solution (5.12) and 1.00 ml phthalate standard stock solution (5.15), (5.16) in 25 ml Volumetric flask, with acetonitrile (5.5) constant volume, mix well. 4 ℃ the following sealed. 5.18 Magnesium silicate. 150 μm to 250 μm (100 mesh to 60 mesh). Before use, weigh 100 g ± 10 g into an evaporating dish at 140 ° C Heated 16 h, while hot transferred to 500 ml grinding mouth reagent bottle, cooled to room temperature, add 3.0 ml ± 0.1 ml experimental water, sealed, Shake well for 10 min and let stand for 2 h. 5.19 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 solid phase extraction column. 5.20 glass (or quartz) fiber filter. According to the sampling head to select the appropriate size of the filter. The retention of the membrane on 0.3 μm standard particles The rate of not less than 99%, air flow velocity of 0.45 m/s, leaflets filter resistance of not more than 3.5 kPa. Before use in a muffle furnace at 400 ℃ heating 5 h or more, cooled, wrapped with aluminum foil, stored in a filter box, to avoid direct connection with the plastic Touch, to ensure that the filter before sampling and sampling is not stained, and in the flat before the sample is not folded state. 5.21 XAD-2 resin (styrene-divinylbenzene polymer). 250 μm to 840 μm (60 mesh to 20 mesh). Before extraction with dichloromethane (5.1) reflux 16 h, the replacement of dichloromethane (5.1) to continue reflux extraction 16 h, then ether - N-hexane mixed solution (5.7) refluxed 16 h, vacuum dried at room temperature 2 h ~ 3 h. Keep in a clean glass bottle. 5.22 Polyurethane Foam (PUF). polyether type, with a density of 22 mg/cm3 to 25 mg/cm3, cut and grown 25 mm and 50 mm in diameter 3 is a cylinder of 45 mm to 65 mm (length, diameter is determined by the specifications of the glass sampling cartridge). Before use, wash with experimental water, drain water, rinse three times with acetone (5.4), place into Soxhlet extractor (6.4), wash with acetone (5.4). The mixture of diethyl ether and n-hexane (5.7) was refluxed for 16 h, and the mixture was replaced with fresh ether-n-hexane solution (5.7) Reflux extraction. Room temperature vacuum drying 2 h ~ 3 h (also available nitrogen (5.23) dry). Keep it in a suitable container with aluminum foil and seal it. 5.23 Nitrogen. Purity ≥99.999%. 5.24 glass wool. Before use with dichloromethane (5.1) reflux extraction 2 h ~ 4 h, dried and sealed.

6 instruments and equipment

6.1 High Performance Liquid Chromatography (HPLC). Gradient elution with UV detector at 225 nm and 235 nm. 6.2 Column. ODS-C18 (octadecylsilane-bonded octadecylsilane) column with a size of 4.6 mm × 250 mm and a particle size of 5.0 μm Column or other similar performance of the column. 6.3 Ambient air sampling device. to meet the HJ 691 requirements. 6.3.1 Sampler. with automatic accumulation of sampling volume, automatic conversion standard cumulative sample volume function, and has automatic timing, power off and then Function to automatically compensate for flow changes due to voltage fluctuations and resistance changes. Under normal sampling conditions, large flow sampling workers For the point of flow of 225 L/min, medium flow sampler flow rate of 100 L/min. 6.3.2 Sampling head. the filter holder and the sampling sleeve sleeve of two parts, as shown in Figure 1. Sampling head material selection of stainless steel or PTFE Ene and other non-adsorption of organic materials. Filter clip includes filter ring, filter and filter holder. Sampling tube sleeve for the glass sampling tube inside, Inside and out of the glass sampling cartridge are PUFs (5.22) with a minimum thickness of 50 mm and 25 mm with a minimum of 10 g of XAD-2 resin (5.21), the bottom of the stainless steel mesh support. Glass sampling tube sealed with a silicone rubber seal between the filter holder and the suction pump. Soxhlet extractor. 1000 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. 6.7 solid phase extraction device. 6.8 General laboratory equipment commonly used. 41-airflow inlet; 2-filter holder; 3-sampling cartridge sleeve; 4-gas flow Outlet; 5-filter on the pressure ring; 6-silicone rubber seals; 7-filter; 8-stainless steel mesh; 9-membrane holder; 10-glass sampling cartridge. Figure 1 sampling head schematic

7 samples

7.1 sample collection Sample collection meets HJ 691 requirements. Phthalates in the ambient air exist in the gas phase, particulate matter or both exist at the same time, you must also use glass (or quartz) fiber filter, XAD-2 resin and polyurethane foam collection. Before sampling the membrane filter and glass sampling tube installed in the filter holder and the sampling sleeve, connecting the sampler, adjusting the sampling flow, the beginning sampling. Remove the filter after the sample is finished, the sample dust to the inside of the fold, remove the glass sampling tube, and fold the filter together with aluminum foil wrapped, Put in the original box sealed. Collect the site before the sample collection blank, sealed glass sampling tube and filter membrane to the sampling site, the sampling head is not installed Sampling, and then remove the glass sampling cartridge and filter, sealed with the same sample and sealed, with the sample shipped back to the laboratory. 7.2 Sample preservation 5 After the samples were collected, the samples were refrigerated below 4 ℃ and extracted within 7 days. The sample extract is stored below 4 ° C and stored in 40 days Analysis. 7.3 Sample Preparation 7.3.1 Sample Extraction Put the filter and glass sample tube into a Soxhlet extractor (6.4), add 250 μl of alternative liquid (5.13) to XAD-2 resin, Add 500 ml diethyl ether - n-hexane mixed solution (5.7), reflux extraction 16 h or more, hourly reflux not less than 3 times to 4 times. Extracted Completed, cooled to room temperature, remove the bottom bottle, rinsed the extraction cup interface, the cleaning fluid will be transferred to the end of the bottle. Add a little anhydrous sodium sulfate (5.6) To the sodium sulfate particles can be free-flowing, placed 30 min, dehydrated and dried. Note. As long as the quality control requirements of this standard can be met, other sample extraction methods may also be used. 7.3.2 Sample concentration The sample extract was transferred to a concentration flask, concentrated at below 45 ℃, the solvent was completely converted to n-hexane, concentrated to about 1 ml until Purification. 7.3.3 Sample Purification 7.3.3.1 Magnesium silicate column The bottom of the glass column (6.5) is filled with glass wool (5.24), 2 cm of anhydrous sodium sulfate (5.6) and n-hexane (5.2) The agent was wet-filled with 10 g of magnesium silicate (5.18), the bubbles were bubbled off, and 1 cm to 2 cm of anhydrous sodium sulfate (5.6) was added to the top. Use 40 ml of n-hexane Alkane (5.2) pre-rinsed the column and controlled the flow rate to about 2 ml/min to keep the liquid level slightly higher than the packed bed and transfer the concentrated liquid (7.3.2) To the column, the vial was washed twice with 1 ml of n-hexane and transferred to the column. Rinse the column with 40 ml of n-hexane and discard the flow Liquid. The column was eluted with.200 ml diethyl ether-n-hexane mixed solution (5.8) at an elution rate of 2 ml/min to 5 ml/min to receive the eluate. The eluent was concentrated to about 1 ml by 7.3.2, 2 ml of acetonitrile was added, and the mixture was concentrated to continue the conversion. Finally, the solvent was converted to acetonitrile, Make up to 1.0 ml and transfer to vial for analysis. 7.3.3.2 Magnesium silicate solid phase extraction column Take the solid phase extraction column (5.19), pre-rinse the solid phase with 10 ml of acetone-n-hexane mixed solution (5.9) and 10 ml of n-hexane Extract the column and 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 vial was washed twice and transferred to the column, followed by 5 ml n-hexane (5.2), 10 ml dichloromethane-n-hexane mixed solution (5.10) Rinse the SPE cartridges and discard the effluent. Elute with 10 ml of acetone-n-hexane mixed solution (5.9) and receive the eluate. The eluent was concentrated to about 1 ml by 7.3.2, 2 ml of acetonitrile was added, and the mixture was concentrated to continue the concentration. Finally, the solvent was converted to acetonitrile, Make up to 1.0 ml and transfer to vial for analysis. Note. As long as the quality control requirements of this standard can be met, other sample purification methods, solid phase columns of different specifications and different batch numbers of magnesium silicate may be used for elution The amount of solvent may be different, the need to conduct the conditions before use experiments. 7.4 Preparation of blank samples 7.4.1 Site blank Site blank (7.1) Prepare a site blank sample following the same procedure as for sample preparation (7.3). 67.4.2 Laboratory blank The same batch of glass sampling cartridges and filters according to the same sample preparation steps (7.3) Preparation of laboratory blank samples.

8 Analysis steps

8.1 Instrument reference conditions Column oven temperature. 35 ° C; injection volume. 10 μl; UV detector wavelength. 235 nm and 225 nm. Gradient elution program. Mobile phase A. Acetonitrile; Mobile phase B. Water. Table 1 Gradient elution program Time (min) Mobile phase flow rate (ml/min) A (%) B (%) 0 1.0 35 65 15 1.0 45 55 40 1.0 100 0 50 1.0 35 65 1-dimethyl phthalate; 2-diethyl phthalate; 3-diphenyl phthalate (alternative); 4-butyl phthalate Benzyl phthalate; diisobutyl 5-phthalate; dibutyl phthalate; di-2-ethylhexyl phthalate; Di-n-octyl phthalate. Figure 2 Phthalates standard chromatogram 8.2 standard curve drawing Pipette a standard amount of standard solution (5.17) and dilute with acetonitrile (5.5) to give concentrations of 2.0 μg/ml, 5.0 μg/ml, 10.0 μg/ml, 20.0 μg/ml, 40.0 μg/ml standard series of solutions. From low concentration to high concentration into the high performance liquid chromatography, according to instrument reference conditions (8.1) Analyze the chromatograms of the target compound at different concentrations and record the retention time, peak height or peak area. The target compound mass concentration as abscissa, the corresponding peak height or peak area for the vertical axis, the standard curve. Phthalates standard chromatogram shown in Figure 2. 78.3 Determination of the sample The determination of the sample is performed according to the same instrument conditions as the standard curve, and the peak height or area of the target compound is recorded and retained between. 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 According to the retention time, the absorbance ratio at different wavelengths qualitative, or the use of samples of UV spectrophotometry and standard solution compared to the qualitative UV spectra. 9.2 Quantitative analysis According to the peak height or peak area of the target compound, the external standard method was used for quantification, and the quantitative wavelength was 235 nm. 9.3 Results Calculation Calculate the mass concentration () of the target compound in ambient air according to equation (1). V) (0 (1) Where.  - the mass concentration of the target compound in ambient air, 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; Vs - Sampling volume at standard conditions (101.325 kPa, 273 K), m3. 9.4 results indicated When the concentration of phthalates in ambient air is greater than or equal to 1.00 μg/m3, the result retains three significant figures; for less than 1.00 μg/m3, The result is retained to the third decimal place. 10 precision and accuracy 10.1 Precision Six laboratories respectively added spiked samples of 4.0 μg, 20.0 μg and 36.0 μg to air (equivalent to 0.028 μg/m3 for air samples, 0.139 μg/m3 and 0.250 μg/m3). The relative standard deviations in the laboratory ranged from 1.5% to 14% and from 2.2% to 17% And 1.0% ~ 15% respectively. The relative standard deviations (RSDs) were 3.3% ~ 13%, 3.2% ~ 8.4% and 3.2% ~ 5.8% 0.003 μg/m3 to 0.006 μg/m3, 0.016 μg/m3 to 0.033 μg/m3 and 0.022 μg/m3 to 0.042 μg/m3 respectively; ......
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