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HJ 867-2017 English PDF

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HJ 867-2017: Ambient air. Determination of phthalate esters. Gas chromatography/mass spectrometry
Status: Valid
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HJ 867-2017399 Add to Cart 4 days Ambient air. Determination of phthalate esters. Gas chromatography/mass spectrometry Valid

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Basic data

Standard ID: HJ 867-2017 (HJ867-2017)
Description (Translated English): Ambient air. Determination of phthalate esters. Gas chromatography/mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z15
Classification of International Standard: 13.040.20
Word Count Estimation: 17,120
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 gas chromatography-mass spectrometry 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 sampling volume is 144m^(3) (under standard conditions), the volume of concentrated constant volume is 1.0 ml. The full scan method is used. The detection limit of the method is 0.003 to 0.004 ��g/m3, and the lower limit of determination is 0.012 to 0.016 ��g/m. ^(3). See Appendix A for details.

HJ 867-2017: Ambient air. Determination of phthalate esters. Gas chromatography/mass spectrometry


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(Ambient air - Determination of phthalates - Gas chromatography - mass spectrometry) People's Republic of China national environmental protection standards Ambient air - Determination of phthalates Gas chromatography - mass spectrometry Ambient air - Determination of phthalate esters -Gas chromatography/mass spectrometry 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 ...8 10 Precision and accuracy ... 9 11 Quality Assurance and Quality Control ... 9 12 Waste Treatment ... 10 13 Notes ... 10 Appendix A (normative) method of detection limit and lower limit ... 11 Appendix B (Informative) Qualitative and quantitative ionization of target compounds, internal standards and substitutes ... 12 Appendix C (informative) method of precision and accuracy ... 13

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 phthalates in ambient air by gas chromatography - mass spectrometry. Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices. 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 - Determination of phthalates - Gas chromatography - mass spectrometry 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 phthalates in ambient air by gas chromatography - mass spectrometry. 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 the method is 0.003 μg/m 3 to 0.004 μg/m 3, and the lower limit of determination is 0.012 μg/m 3 to 0.016 μg/m 3. 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 ether-n-hexane mixed solution, the extract was concentrated, purified, and analyzed by gas chromatography-mass spectrometry Instrument separation test. According to the retention time and characteristic ion abundance ratio qualitative, internal standard method.

4 Interference and elimination

4.1 Disturbances with the same retention time At the onset of an interference, the qualifier ions can be detected by mass spectrometry to distinguish them. 4.2 Purification using magnesium silicate column can remove or reduce interference, see 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 Anhydrous sodium sulfate (Na2SO4) Bake in a muffle furnace at 450 ℃ for 4 h before use, cool, and store in sealed glass jar. 25.6 decafluorotriphenylphosphine (DFTPP). ρ = 50 μg/ml, can be purchased directly from the certified public standard solution, or with a high concentration of standard solution with system. 5.7 ether - n-hexane mixed solution. 1 9, Pro use now. 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 diphenyl phthalate (5.11) about 0.1 g, accurate to 0.1 mg, in 50 ml volumetric flask, dissolved in a small amount of acetone, With n-hexane (5.2) constant volume, mix well. 4 ℃ the following sealed. Can also be purchased directly from the market certified standard solution. 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 with n-hexane (5.2) and mix well. 4 ℃ below the dense Save sealed. 5.14 Internal standard stock solution. ρ = 4000 μg/ml. Direct purchase of a certified public standard solution, with 苊-D10, Philippines-D10, 䓛 -D12, reference standard solution certificate. 5.15 Internal standard solution. ρ = 1000 μg/ml. The internal standard stock solution (5.14) was diluted to 1000 μg/ml with dichloromethane (5.1). 4 ℃ below the sealed dark save. 5.16 Diisobutyl phthalate Reference material. purity 98% or more. 5.17 Diisobutyl phthalate stock solution. ρ =.2000 μg/ml. Weigh 0.1 g of diisobutyl phthalate standard (5.16), accurate to 0.1 mg in a 50 ml volumetric flask with n-hexane (5.2) Dissolve and set the volume, mix well. 4 ℃ the following sealed. Can also be purchased directly from the market certified standard solution. 5.18 6 phthalates standard stock solution. ρ =.2000 μg/ml. Direct purchase of a certified commercial standard solution, including dimethyl phthalate, diethyl phthalate, dibutyl phthalate, o Butyl phthalate, di-2-ethylhexyl phthalate and di-n-octyl phthalate in n-hexane. 4 ℃ below the preservation, or reference standard solution certificate preservation. 5.19 8 phthalates standard solution. ρ = 80.0 μg/ml. Remove phthalate standard stock solution (5.17), (5.18) and replacement stock solution (5.12) each 1.00 ml, in 25 ml capacity Volume flask with n-hexane (5.2) constant volume, mix well. 4 ℃ the following sealed. 5.20 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, capped 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. 5.21 Magnesium silicate SPE. 1000 mg/6 ml. According to the content of impurities can also choose the appropriate capacity of commercial solid phase extraction column. 5.22 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. 3 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. 5.23 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. 5.24 Polyurethane Foam (PUF). polyether type, with a density of 22 mg/cm3 to 25 mg/cm3, cut for growth of 25 mm and 50 mm, straight Cylindrical diameter of 45 mm to 65 mm (length, diameter as determined by the specifications of the glass sampling cartridge). Wash with experimental water before use, drained, rinsed three times with acetone (5.4) and placed in a Soxhlet extractor (6.4), followed by C Ketone (5.4), diethyl ether - n-hexane mixed solution (5.7) refluxed 16 h, during the replacement of 2 to 3 times the fresh ether - hexane mixed solution Liquid (5.7). Room temperature vacuum drying 2 h ~ 3 h (also available nitrogen (5.25) dry). Wrap with aluminum foil and seal in a suitable container save. 5.25 Nitrogen. Purity ≥99.999%. 5.26 Helium. Purity ≥99.999%. 5.27 glass wool. before use dichloromethane (5.1) reflux extraction 2 h ~ 4 h, dried and sealed.

6 instruments and equipment

6.1 Gas Chromatography - Mass Spectrometer. The gas chromatograph has a split/splitless inlet with programmed temperature capability; the mass spectrometer uses an electron bombardment Ionization source. 6.2 Column. Quartz capillary column, 30 m (length) × 0.25 mm (ID) × 0.25 μm (film thickness) with 5% phenyl 95% Dimethylpolysiloxane, or other equivalent low-loss chromatography 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 cylinder are PUF (5.24) with a minimum thickness of 50 mm and 25 mm with a minimum of 10 g of XAD-2 resin (5.23) with the bottom supported by stainless steel mesh. 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 After the sample was collected, it was refrigerated below 4 ℃ and extracted within 7 days. The sample extract is stored below 4 ° C and stored in 40 days 5 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 into the bottom bottle. Add a little anhydrous sodium sulfate (5.5) To sodium sulfate particles can be free-flowing, dehydration drying 30min. 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 replaced by 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 (5.27), 2 cm of anhydrous sodium sulfate (5.5) and n-hexane (5.2) The agent is wet-filled with 10 g of magnesium silicate (5.20), expelled the air bubble, and the upper portion is added with 1 cm-2 cm of anhydrous sodium sulfate (5.5). Use 40 ml of n-hexane The 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 1.0 ml or less according to 7.3.2, fixed to 1.0 ml, and 10.0 μl of internal standard solution (5.15) was transferred to the sample Bottle to be analyzed. 7.3.3.2 Magnesium silicate solid phase extraction column Take solid-phase extraction column (5.21), followed by 10 ml of acetone - n-hexane mixed solution (5.9), 10 ml of n-hexane (5.2) 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 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 solid-phase extraction column, the effluent discarded. Elute with 10 ml of acetone-n-hexane mixed solution (5.9) and receive the eluate. The eluent was concentrated to 1.0 ml or less according to 7.3.2, fixed to 1.0 ml, and 10.0 μl of internal standard solution (5.15) was transferred to the sample Bottle to be analyzed. 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). 7.4.2 Laboratory blank 6 same batch of glass sampling cartridges and filters in accordance with the same sample preparation steps (7.3) Preparation of laboratory samples blank.

8 Analysis steps

8.1 Instrument reference conditions 8.1.1 GC reference conditions Inlet temperature. 250 ℃; Injection mode. split injection, split ratio 10.1; injection volume. 1.0 μl; column temperature. 45 ℃ for 2 min, Raise temperature to 320 ° C at 10 ° C/min for 5.5 min; Carrier gas. Helium (5.26), Flow rate. 1.0 ml/min. 8.1.2 Reference conditions for mass spectrometry Transmission line temperature. 280 ℃; Ion source temperature. 250 ℃; Ion source electron energy. 70 eV; Mass range. 35 amu ~ 500 amu; Scan mode. full scan; solvent delay time. 10 min; electron multiplier voltage. consistent with the tuning voltage; the remaining parameters with reference to the instrument Use manual to set. 8.2 Instrument Performance Check Before calibration, inject 1.0 μl of DFTPP solution (5.6), and the key ion abundance of DFTPP obtained by GC-MS system should satisfy the table 1 requirements; otherwise some parameters of the mass spectrometer need to be adjusted or cleaned of the ion source. Table 1 DFTPP key ion abundance criteria Mass ion m/z abundance standard mass ion m/z abundance standard 51 Base peak 30% ~ 60%.199 Base peak 5% ~ 9% 68 2% of less than 69 peaks 275% of the base peak 10% to 30% 70 Less than 69 2% of peak 365 365% of base peak 1% 40% to 60% of Base Peaks 441 are present and less than 443 Peaks 197 Less than 1% of base peak 442 Greater than 40% of base peak 198 base peak with an abundance of 100% 443 442 17% ~ 23% 8.3 Calibration 8.3.1 Determination of standard series Pipette a certain amount of standard solution (5.19), diluted with n-hexane (5.2) to prepare a concentration 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. Add 10.0 μl of internal standard solution to every 1.0 ml of standard solution (5.15). According to the instrument reference conditions (8.1) for analysis, to obtain different concentrations of standard solution of the mass spectrum, record the target compound, internal standard And retention times of substitutes and quantitation of ion peak area. The total ion current of phthalate compounds is shown in Fig.2. Dimethyl phthalate; 2-苊 -D10 (internal standard); 3-diethyl phthalate; 4-phenanthrene-D10 (internal standard) Dibutyl phthalate; butyl benzyl phthalate; 8- 䓛 -D12 (internal standard); bis (2- Ethylhexyl) phthalate; 10-diphenyl phthalate (alternative); 11-di-n-octyl phthalate. Figure 2 Phthalate compounds total ion current diagram 8.3.2 Calculation of the average relative response factor According to the formula (1) and formula (2), the relative response factor and the average relative response factor of the target ions with different concentrations were calculated, And cal......
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