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HJ 1184-2021 English PDF

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HJ 1184-2021: (Soil and sediments Determination of 6 phthalate compounds by gas chromatography-mass spectrometry)
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Basic data

Standard ID HJ 1184-2021 (HJ1184-2021)
Description (Translated English) (Soil and sediments Determination of 6 phthalate compounds by gas chromatography-mass spectrometry)
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Word Count Estimation 19,168
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1184-2021: (Soil and sediments Determination of 6 phthalate compounds by gas chromatography-mass spectrometry)


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(Soil and sediments Determination of 6 phthalate compounds by gas chromatography-mass spectrometry) National Ecological Environment Standard of the People's Republic of China Soil and Sediment 6 Phthalates Determination of Compounds by Gas Chromatography-Mass Spectrometry Soil and sediment-Determination of 6 Phthalate Esters (PAEs) -Gas chromatography mass spectrometry This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment. Published on 2021-06-03 2021-09-15 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Terms and Definitions...1 4 Principles of the method...1 5 Interference and cancellation...2 6 Reagents and materials...2 7 Instruments and equipment...3 8 Samples...3 9 Analysis steps...4 10 Result calculation and representation...6 11 Accuracy...8 12 Quality Assurance and Quality Control...9 13 Waste Disposal...9 14 Notes...9 Appendix A (normative appendix) detection limit and lower limit of determination of the method...10 Appendix B (informative appendix) Determination reference parameters of the target... 11 Appendix C (informative) Accuracy of the method...12 Determination of Six Phthalates in Soil and Sediments gas chromatography-mass spectrometry Warning. The organic solvents and standard substances used in the experiment are toxic and harmful substances. The standard solution preparation and sample pretreatment process should be Carry out the operation in a fume hood; wear protective equipment as required to avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies the gas chromatography-mass spectrometry method for the determination of six phthalates in soil and sediment. This standard applies to dimethyl phthalate (DMP), diethyl phthalate (DEP), phthalate in soil and sediments Di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), bis(2-ethylhexyl) phthalate (DEHP) and phthalate Determination of 6 kinds of phthalate compounds such as di-n-octyl dicarboxylate (DNOP). Other phthalates are verified can also be determined by this method. When the sampling volume is 10.0 g, the extraction volume is 20.0 ml, and the injection volume is 1.0 µl, this standard method for the determination of phthalates The detection limit is 0.02 mg/kg～0.05 mg/kg, and the lower limit of determination is 0.08 mg/kg～0.20 mg/kg. See Appendix A for details.

2 Normative references

This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. GB 17378.3 Marine Monitoring Specification Part 3.Sample Collection, Storage and Transportation GB 17378.5 Marine Monitoring Specification Part 5.Sediment Analysis HJ/T 166 Technical Specification for Soil Environment Monitoring HJ 494 Water Quality Sampling Technical Guide HJ 613 Gravimetric Method for Determination of Soil Dry Matter and Moisture HJ 834 Determination of Semivolatile Organic Compounds in Soil and Sediments by Gas Chromatography-Mass Spectrometry

3 Terms and Definitions

The following terms and definitions apply to this standard. 3.1 Phthalates phthalate esters Also known as phthalate esters (PAEs), it is a general term for ester compounds formed by phthalic acid, generally referring to phthalates. Esters of dicarboxylic acid and alcohols of 4 to 15 carbons.

4 Principles of the method

Phthalates in soil and sediment were extracted with ethyl acetate, separated by gas chromatography and detected by mass spectrometry. According to reservation Time, mass-to-charge ratio of fragment ions and their abundance were qualitative, and internal standard method was used for quantification.

5 Interference and cancellation

5.1 In the process of sample collection and preservation, use metal sampling utensils, brown ground-mouth jars with stoppers, and wrap them in aluminum foil (6.17). Wrap to eliminate distractions. 5.2 When weighing the sample, remove the sample on the surface of the bottle mouth to eliminate interference. 5.3 During the injection process, the injection septum of the gas chromatograph will cause positive interference to the measurement results, which cannot be eliminated by the interference of the instrument itself. Note. Try to choose septa with good quality and low blank. 5.4 The bottle gasket of the sample bottle (7.4) will interfere with the measurement results, which can be avoided by placing a layer of aluminum foil (6.17) between the sample bottle and the bottle cap. method to eliminate interference.

6 Reagents and Materials

Unless otherwise specified, analytical reagents that meet national standards were used in the analysis. The experimental water was freshly prepared distilled water with clean glass Glass container. 6.1 Dichloromethane (CH2Cl2). pesticide residue grade. 6.2 Acetone (CH3COCH3). pesticide residue grade. 6.3 Ethyl acetate (CH3COOC2H5). pesticide residue grade. 6.4 Phthalates mixed standard stock solution. ρ = 1 000 mg/L. Commercially available certified standard solutions can be purchased directly, stored in the refrigerator below 4°C, protected from light, or stored with reference to the standard solution certificate. use should be returned to room temperature and shaken. 6.5 Phthalate mixed standard intermediate solution. ρ = 100 mg/L. Pipette 1.00 ml of phthalate mixed standard stock solution (6.4) into a 10 ml brown volumetric flask, dilute with ethyl acetate (6.3) and make up to volume to the marking line, shake well, transfer to a compact bottle (7.10), refrigerate below 4°C, and store in the dark. 6.6 Phthalate mixed standard solution. ρ = 20.0 mg/L. Pipette 2.00 ml of phthalate mixed standard intermediate solution (6.5) into a 10 ml brown volumetric flask, dilute with ethyl acetate (6.3) and make up to volume to the marking line, shake well, transfer to a compact bottle (7.10), refrigerate below 4°C, store in the dark, and store for no more than 7 days. 6.7 Substitute stock solution. ρ = 5 000 mg/L. Benzyl benzoate (BBZ) was chosen as an alternative. Commercially available certified standard solutions can be directly purchased, refrigerated below 4°C, and stored in the dark. Or refer to the standard solution certificate for preservation. Return to room temperature and shake well before use. 6.8 Substitute intermediate solution. ρ = 100 mg/L. Pipette.200 μl of substitute stock solution (6.7) into a 10 ml brown volumetric flask, dilute with ethyl acetate (6.3) and make up to the mark, shake Homogenize, transfer to a compact bottle (7.10), refrigerate below 4°C, and store in the dark. 6.9 Substitute liquid. ρ = 20.0 mg/L. Pipette 2.00 ml of substitute intermediate solution (6.8) into a 10 ml brown volumetric flask, dilute with ethyl acetate (6.3) and dilute to the mark, shake Homogenize, transfer to a compact bottle (7.10), refrigerate below 4°C, and store in the dark. Return to room temperature and shake well before use. 6.10 Internal standard stock solution. ρ =100 mg/L. Diamyl phthalate-d4 (DPP-d4) and bis(2-ethylhexyl) phthalate-d4 (DEHP-d4) were selected as internal standards. Commercially available certified standard solutions can be purchased directly, stored in the refrigerator below 4°C, protected from light, or stored with reference to the standard solution certificate. should be used Return to room temperature and shake. 6.11 Internal standard solution. ρ = 20.0 mg/L. Pipette 2.00 ml of internal standard stock solution (6.10) into a 10 ml brown volumetric flask, dilute with ethyl acetate (6.3) and dilute to the mark, shake Homogenize, transfer to a compact bottle (7.10), refrigerate below 4°C, and store in the dark. Return to room temperature and shake well before use. 6.12 Decafluorotriphenylphosphine (DFTPP). ρ=50.0 mg/L. Commercially available certified standard solutions can be purchased directly. Other concentrations were diluted to 50.0 mg/L with ethyl acetate (6.3) and mixed. 6.13 Anhydrous sodium sulfate (Na2SO4). 150 μm ~ 250 μm (100 mesh ~ 60 mesh), excellent grade. Burn in a muffle furnace at 400 °C for 6 h, and after a little cooling, place it in a desiccator with a stopper and a ground-mouth jar for later use. 6.14 Quartz glass wool. Burn in a muffle furnace at 400 °C for 6 h, and store in a ground jar with a stopper after cooling. 6.15 Alumina (Al2O3). neutral, with a particle size of 50 μm to.200 μm (about 300 mesh to 70 mesh). Burn in a muffle furnace at 400 °C for 6 h, and store in a sealed flask or desiccator after being slightly cooled, and the storage time should not exceed 5 d. 6.16 Quartz sand. the particle size is 150 μm～830 μm (100 meshes～20 meshes). Burn in a muffle furnace at 400°C for 6 h, cool slightly and place in a desiccator with a stopper and a ground-mouth jar for later use. Check before use to confirm that there is no interference. 6.17 Aluminum foil. After burning at 400 ℃ for 2 h. 6.18 High-purity nitrogen. purity ≥99.999%. 6.19 High-purity helium. purity ≥99.999%.

7 Instruments and equipment

7.1 Gas chromatograph-mass spectrometer. with capillary split/splitless injection port, with constant flow or constant pressure function; the column oven can be temperature-programmed; Electron Impact (EI) ionization source. 7.2 Chromatographic column. quartz capillary column, 30 m (column length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness), the stationary phase is 5% phenyl -95% methyl polysiloxane, or other equivalent capillary column. 7.3 Extraction device. horizontal oscillator or other equipment of equivalent performance. 7.4 Injection bottle. glass material, with polytetrafluoroethylene (PTFE) coated septa, 2.0 ml. 7.5 Glass post. PTFE stopper with stainless steel cone or Luer interface. 7.6 Vacuum freeze dryer. the no-load vacuum degree is below 13 Pa. 7.7 Centrifuge tube. glass material, 50 ml. 7.8 Conical flask. with stopper and ground mouth, 250 ml. 7.9 Glass tube. ground stopper, graduated, 25 ml. 7.10 Compact bottle. brown glass bottle, 10 ml. 7.11 Centrifuge. adjustable speed. 7.12 Common laboratory instruments and equipment.

8 samples

8.1 Sample Collection and Storage Soil samples were collected and stored in accordance with the relevant requirements of HJ/T 166, water sediment samples were collected in accordance with the relevant requirements of HJ 494, and marine sediment samples were collected in accordance with the relevant requirements of HJ/T 166. Ocean sediment samples were collected in accordance with the relevant requirements of GB 17378.3.Samples should be stored in clean brown stoppered ground-mouth jars, during transportation Should be protected from light, sealed and refrigerated below 4 ℃. If it cannot be analyzed in time, it should be refrigerated below 4°C, protected from light and sealed, and the storage time should not exceed 6 d. 8.2 Preparation of samples Place the sample in a clean enamel or stainless steel dish covered with aluminum foil (6.17), remove foreign matter (stones, leaves, etc.) from the sample, Mix the sample. According to the requirements of HJ/T 166, the sample reduction is carried out. It can be dehydrated and dried by desiccant method or freeze-drying method. Method 1.Desiccant method. Weigh 10 g (accurate to 0.01 g) fresh sample, add an appropriate amount of anhydrous sodium sulfate (6.13), grind and homogenize In the form of quicksand, transfer all to a conical flask (7.8) for later use. Method 2.Freeze drying method. Weigh an appropriate amount of sample and put it into a vacuum freeze dryer (7.6) for drying and dehydration. dried sample The product is directly ground and sieved. Then weigh 10 g (accurate to 0.01 g) of the sample and transfer it all to a conical flask for use. 8.3 Determination of moisture According to HJ 613, the dry matter content of soil samples was measured; according to GB 17378.5, the moisture content of sediment samples was measured. 8.4 Preparation of test specimens 8.4.1 Extraction Transfer all the samples (8.2) to the Erlenmeyer flask (7.8), add 100 µl to.200 µl of the substitute solution (6.9), and then add 20.0 ml ethyl acetate (6.3), left for 30 min. Set the oscillation frequency of the horizontal oscillator to 150 r/min, the amplitude to 20 mm, and the extraction for 20 min. After the extraction is completed, transfer all the solution to the centrifuge tube (7.7), move the centrifuge tube to the centrifuge (7.11), set the speed to 2 000 r/min, and centrifuge 3 min. Pipette 1.0 ml of the supernatant into the sample vial (7.4), use a syringe to transfer 5.0 µl of the internal standard solution (6.11) into the sample vial, After mixing, it will be tested. If purification is required, take all the extract and wait for purification. Note 1.The extraction method can also choose other equivalent extraction methods other than horizontal oscillation extraction. Note 2.The storage time of the extract should not exceed 7 days. 8.4.2 Purification 8.4.2.1 Alumina cartridge preparation Fill the bottom of the glass column (7.5) with glass wool (6.14), add 1 g of alumina (6.15), and tap the glass column wall to oxidize Aluminum fills evenly. Add 5 ml of dichloromethane (6.1) to activate, then add 5 ml of ethyl acetate (6.3) to rinse, and dry with nitrogen (6.18) After 2 min, close the stopcock, wrap the top and bottom of the alumina cartridge with aluminum foil (6.17), and store it in a stainless steel container for later use. 8.4.2.2 Alumina cartridge cleanup Pass all the extraction solution (8.4.1) through the alumina cartridge, and collect the purification solution in the glass tube (7.9), after mixing, transfer 1.0 ml to In the sample bottle (7.4), use a syringe to pipette 5.0 µl of the internal standard solution (6.11) into the sample bottle, mix well, and wait for the test. Note. If the sample matrix is complex and there are many interferences, the extraction solution (8.4.1) should be purified with an alumina cartridge. Other methods verified to meet the requirements may also be used. 8.5 Preparation of blank samples Substitute quartz sand (6.16) for the actual sample and prepare a blank sample following the same procedure as in the preparation of the sample (8.4).

9 Analysis steps

9.1 Instrument Reference Conditions 9.1.1 Gas chromatography reference conditions Inlet temperature. 280℃, splitless; Injection volume. 1.0 μl, carrier gas flow rate. 1.2 ml/min (constant flow); The temperature program of the chromatographic column was as follows. 50 °C for 1 min, then heated to 280 °C at a rate of 15 °C/min, and held for 5 min. IS IS H ORRF (1) x xA Vw A mw ρ × × × × × − (6) In the formula. w -- the content of the target compound in the sample, mg/kg; Ax - the quantitative ion peak area of the target compound in the sample; AIS - the quantitative ion peak area of the internal standard compound in the sample; ρ IS -- the mass concentration of the internal standard compound in the test solution, mg/L; RRF -- the average relative response factor of the target compound in the standard curve series; Vx - the volume of the sample extract, ml; 2HO w -- the moisture content of the sample, %; m -- the weighing amount of the sample, g. 10.4 Result representation The retention of the number of digits after the decimal point of the determination result is consistent with the detection limit of the method, and at most 2 significant figures are retained. 11 Accuracy 11.1 Precision The 6 laboratories carried out 6 repeated tests on the quartz sand samples spiked with concentration of 0.10 mg/kg, 0.50 mg/kg and 0.80 mg/kg respectively. The intra-laboratory relative standard deviations were 2.0%-25%, 1.8%-17%, 1.2%-9.2%; the inter-laboratory relative standard deviations were divided into 7.8%～19%, 7.0%～18%, 4.9%～18%; the repeatability limits are 0.03 mg/kg～0.05 mg/kg, 0.06 mg/kg～ 0.15 mg/kg, 0.08 mg/kg～0.14 mg/kg; the reproducibility limits are 0.04 mg/kg～0.07 mg/kg, 0.13 mg/kg～0.26 mg/kg, 0.13 mg/kg～0.40 mg/kg. The 6 laboratories tested the Hunan laterite and Zibo samples with standard concentrations of 0.10 mg/kg, 0.50 mg/kg, 0.80 mg/kg and 0.10 mg/kg respectively. The soil samples of cinnamon soil, Harbin black soil and Zibo brown soil were tested six times repeatedly, and the relative standard deviations in the laboratory were 2.2%-23%, respectively. 0.90%-9.4%, 1.3%-12%, 2.6%-24%; the relative standard deviations between laboratories were 7.8%-27%, 6.6%-20%, 5.3%～24%, 7.5%～29%; the repeatability limits are 0.03 mg/kg～0.06 mg/kg, 0.07 mg/kg～0.09 mg/kg, 0.10 mg/kg～0.20 mg/kg, 0.03 mg/kg～0.05 mg/kg; the reproducibility limits are 0.06 mg/kg～0.10 mg/kg, 0.14 mg/kg～ 0.34 mg/kg, 0.18 mg/kg to 0.66 mg/kg, 0.04 mg/kg to 0.09 mg/kg. Six laboratories carried out 6 repetitions of sediment samples from Mengshan Reservoir and Xiaofu River with spiked concentrations of 0.50 mg/kg and 0.80 mg/kg, respectively. For repeated determination, the relative standard deviations within the laboratory were 1.0% to 15%, 1.4% to 20%, and the relative standard deviations between the laboratories were 3.6% to 20%. 29%, 6.1%～27%; the repeatability limits are 0.07 mg/kg～0.12 mg/kg, 0.07 mg/kg～0.29 mg/kg; the repeatability limits are respectively 0.13 mg/kg～0.42 mg/kg, 0.30 mg/kg～0.50 mg/kg. See Appendix C for precision data. 11.2 Correctness 6 laboratories measured quartz sand samples spiked with concentration of 0.10 mg/kg, 0.50 mg/kg and 0.80 mg/kg respectively. The standard recoveries ranged from 85.7% to 140%, 66.9% to 124%, and 66.3% to 118%; the final values of the standard addition recoveries were (103±16.0)%～(115±35.0)%, (95.9±28.0)%～(107±27.6)%, (94.7±9.4)%～(103±18.2)%. The 6 laboratories tested the Hunan laterite and Zibo samples with standard concentrations of 0.10 mg/kg, 0.50 mg/kg, 0.80 mg/kg and 0.10 mg/kg respectively. The actual samples of cinnamon soil, Harbin black soil and Zibo brown soil soil were measured, and the recovery rates of standard addition ranged from 66.7% to 132%, 66.4% to 66.4%, respectively. 127%, 71.9%～137%, 60.9%～143%; the final recovery rates of standard addition were (89.7±47.8)%～(106±45.2)%, respectively. (89.0±28.4)%～(97.8±20.2)%, (92.0±27.0)%～(108±27.2)%, (96.4±56.2)%～(110±16.4)%. Six laboratories tested the actual samples of Mengshan Reservoir and Xiaofu River sediments spiked with concentrations of 0.50 mg/kg and 0.80 mg/kg, respectively. The recovery rates of standard additions ranged from 66.2% to 146%, 60.0% to 129%, and the final values of the standard addition recoveries were (96.1±26.2)%～ (109±8.0)%, (79.5±43.4)%～(109±23.8)%. See Appendix C for accuracy data. 12 Quality Assurance and Quality Control 12.1 Blank test Each 20 samples or each batch (less than 20 samples/batch) needs to do 2 blank tests, and the concentration of the target substance in the determination results should not exceed The method determines the lower limit. 12.2 Calibration The standard curve has at least 5 concentration series, and the relative standard deviation RSD of the target compound relative response factor is less than or equal to 20%. During continuous analysis, analyze 1 standard solution at the middle concentration point of the curve every 20 samples or every batch (less than 20 samples/batch), measure The relative error between the determined result and the measured concentration of the initial curve at this point should be within ±20%, otherwise the standard curve needs to be redrawn. 12.3 Parallel samples Analysis of 1 parallel sample every 20 samples or every batch (less than 20 samples/batch), the relative deviation of the results of single parallel sample determination should be between ±30%. 12.4 Matrix spikes One spiked sample was analyzed every 20 samples or each batch (less than 20 samples/batch), and the spiked recovery rate of soil samples ranged from 60% to 140%, and the recoveries of sediment spiked samples ranged from 60% to 150%. 12.5 Spike recoveries for surrogates The laboratory should establish a control chart for the recovery of surrogate spikes, conduct statistics according to the same batch of samples (10-20 samples), and eliminate outliers. Calculate the average recovery rate P and standard deviation PS of the substitute, and the recovery rate of the substitute should be controlled within P ± 2 PS. 13 Waste Disposal The waste generated during the experiment should be collected by classification, and the qualified units should be entrusted for centralized treatment according to law. 14 Notes 14.1 Contact and use of polyethylene products should be avoided throughout the experimental process. 14.2 Before analyzing phthalate compounds by gas chromatography-mass spectrometer, the instrument should be cleaned and maintained or the gas chromatograph should be replaced. Spectrometer injection septa and liners. Carry out a blank test on the performance of gas chromatographic instruments, through the response value and formula of phthalate compounds. Compare the detection limit of the method, judge the performance of the instrument, and ensure that the response value of the phthalate compound is lower than the detection limit of the method, otherwise it is necessary to test the gas GC-MS for maintenance cleaning. Thoroughly wash all glassware used to remove interfering substances, first with tap water, then with chrome Wash with pickling solution, then rinse with tap water and distilled water, set aside.

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