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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 1052-2019: Soil and sediment -- Determination of 11 triazine pesticides -- High performance liquid chromatography Status: Valid
Basic dataStandard ID: HJ 1052-2019 (HJ1052-2019)Description (Translated English): Soil and sediment -- Determination of 11 triazine pesticides -- High performance liquid chromatography Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z18 Classification of International Standard: 13.080 Word Count Estimation: 20,271 Date of Issue: 2019 Date of Implementation: 2020-04-24 Issuing agency(ies): Ministry of Ecology and Environment HJ 1052-2019: Soil and sediment -- Determination of 11 triazine pesticides -- 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. (Soils and sediments Determination of 11 triazine pesticides High performance liquid chromatography) National Environmental Protection Standard of the People's Republic of China Determination of 11 triazine pesticides in soil and sediment HPLC Soil and sediment-Determination of 11 triazine pesticides -High performance liquid chromatography 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment ContentsForeword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Methodology ... 1 4 Interference and cancellation ... 1 5 Reagents and materials ... 2 6 Instruments and equipment ... 2 7 Sample ... 3 8 Analysis steps ... 4 9 Calculation and Representation of Results ... 6 10 Precision and accuracy ... 7 11 Quality Assurance and Quality Control ... 7 12 Waste disposal ... 8 Appendix A (Normative Appendix) Method detection limits and determination limits ... 9 Appendix B (Informative) Precision and accuracy of methods ... 10ForewordIn order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination of triazine pesticides in soil and sediment, and formulate this standard. This standard specifies HPLC for the determination of 11 triazine pesticides in soil and sediment. Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Hubei Provincial Environmental Monitoring Center Station. This standard is verified by. Zhejiang Environmental Monitoring Center, Chongqing Ecological Environment Monitoring Center, Shaanxi Environmental Monitoring Center Xinzhan Station, Hainan Provincial Environmental Monitoring Center Station, Wuhan Environmental Monitoring Center and Huangshi Environmental Monitoring Station. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Determination of 11 triazine pesticides in soil and sediments by high performance liquid chromatography Warning. The organic solvents and standard materials used in the experiment are toxic and harmful substances. The solution preparation and sample preparation have been processed. Procedures should be performed in a fume hood, and protective equipment should be worn in accordance with regulations to avoid inhalation and contact with skin and clothing.1 ScopeThis standard specifies HPLC for the determination of 11 triazine pesticides in soil and sediment. This standard applies to simazine, atrazine, xicaojing, atrazine, zhongdingtong, extinguishant, Determination of eleven triazine pesticides of fenfenjing, fenfenjin, terbutin, prometryn and dicambarine. When the sample volume is 10 g, the constant volume is 1.0 ml, and the injection volume is 10 μl, the method of 11 kinds of triazine pesticides is checked. The output limit is 0.02 ~ 0.08 mg/kg, and the lower limit of determination is 0.08 ~ 0.32 mg/kg. See Appendix A for details.2 Normative referencesThis standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. GB 17378.3 Marine Monitoring Code Part 3. Sample Collection, Storage and Transportation GB 17378.5 Code for Marine Monitoring Part 5. Sediment Analysis HJ 494 Water Quality Sampling Technical Guide HJ 495 Water Quality Sampling Scheme Design Technical Regulations HJ 613 Soil dry matter and moisture determination by gravimetric method HJ 783 Soil and sediment organic matter extraction Pressurized fluid extraction method HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 166 Technical Specifications for Soil Environmental Monitoring3 Method principleExtraction of triazine from soil or sediment with Soxhlet extraction or pressurized fluid extraction with acetone-dichloromethane as extraction agent Pesticides, the extraction solution is purified by solid phase extraction, concentrated, and fixed volume, then separated by high performance liquid chromatography, detected by UV detector, and Qualitative retention time and external standard method.4 Interference and cancellationOrganic compounds such as polycyclic aromatic hydrocarbons, phthalates and phenols may interfere with the determination and can be separated by chromatography Or solid phase extraction purification.5 Reagents and materialsUnless otherwise specified, analytical reagents that meet national standards are used. Experimental water is freshly prepared ultrapure water Or distilled water. 5.1 Acetone (C3H6O). pesticide residue level. 5.2 Dichloromethane (CH2Cl2). pesticide residue level. 5.3 n-hexane (C6H14). pesticide residue level. 5.4 Acetonitrile (C2H3N). Liquid chromatography grade. 5.5 Acetone-dichloromethane mixed solvent. 1 1. Mix with acetone (5.1) and dichloromethane (5.2) at a volume ratio of 1. 1. 5.6 Acetone-n-hexane mixed solvent. 19. Mix with acetone (5.1) and n-hexane (5.3) in a volume ratio of 1. 9. 5.7 Triazine pesticide standard stock solution. ρ = 1 000 mg/L. You can directly purchase a commercially available certified standard solution, store it in accordance with the requirements of the standard solution certificate, and return to room temperature during use And shake well. 5.8 Triazine pesticide standard solution. ρ = 10.0 ~ 100 mg/L. Dilute the standard stock solution (5.7) with acetonitrile (5.4) to prepare a standard use solution with a concentration of 10.0 ~ 100 mg/L. Protect from light and refrigerate below 4 ℃ for 60 days. 5.9 Anhydrous sodium sulfate (Na2SO4). Bake in a muffle furnace at 450 ° C for 4 hours before use. After cooling, place it in a ground glass bottle and seal it. Store in a desiccator. 5.10 Diatomaceous earth. particle size 150 ~ 250 μm (100 ~ 60 mesh). Bake in a muffle furnace at 450 ° C for 4 hours before use. After cooling, place it in a ground glass bottle and seal it. Store in a desiccator. 5.11 Quartz sand. The particle size is 150 ~ 250 μm (100 ~ 60 mesh). Bake in a muffle furnace at 450 ° C for 4 hours before use. After cooling, place it in a ground glass bottle and seal it. Store in a desiccator. 5.12 Solid-phase extraction column. Commercially available magnesium silicate, silica gel, amino, or other equivalent solid-phase extraction columns with a capacity of 1 000 mg/6 ml or greater. 5.13 Glass wool or glass fiber membrane. Immerse in acetone-dichloromethane mixed solvent (5.5) before use. After the solvent evaporates to dryness, place it in a milled glass bottle. Sealed. 5.14 Soxhlet extraction sleeve. Glass fiber or natural fiber material sleeve. The glass fiber sleeve is baked in a muffle furnace at 450 ° C for 4 hours before use, and then sealed in a ground glass bottle after cooling; The natural fiber material sleeve is immersed in a mixed solvent of acetone-dichloromethane (5.5) before use. Sealed glass jars. 5.15 Nitrogen. Purity ≥99.99%.6 Instruments and equipment6.1 HPLC. with gradient elution function, temperature control of the column oven, equipped with UV detector or diode array Column detector. 6.2 Chromatographic column. The packing is octadecylsilane bonded silica gel, the particle size is 5 μm, the column length is 250 mm, and the color of the inner diameter is 4.6 mm. Column or other equivalent column. 6.3 Extraction device. Soxhlet extraction device or pressurized fluid extraction instrument. 6.4 Concentration device. Rotary evaporator, nitrogen blower or other equivalent concentration equipment. 6.5 Solid phase extraction device. 6.6 Freeze dryer. 6.7 Brown glass bottle. 250 ml. 6.8 Instruments and equipment commonly used in general laboratories.7 samples7.1 Sample collection and storage Collect and preserve soil samples in accordance with the relevant regulations of HJ/T 166; in accordance with GB 17378.3, GB 17378.5, The relevant regulations of HJ 494, HJ 495 and HJ/T 91 are used to collect and preserve sediment samples. The sample should be stored in a clean brown glass bottle (6.7), protected from light, sealed and refrigerated during transportation. If not Can be analyzed, soil samples should be stored below 4 ° C, protected from light, and stored for 5 d (of which simazine, xicaojing, Atrazine, Zhongdingtong, Fenjin, and herbicide have a net storage time of 15 d); sediment samples should be frozen, sealed, and protected from light For 8 days. The sample extraction solution (7.4.1) should be refrigerated, sealed, and protected from light at a temperature below 4 ° C. The storage time is 60 d. 7.2 Sample preparation Place the sample in a stainless steel tray or Teflon tray, remove foreign matter such as sticks, leaves, stones, etc., mix well and follow HJ/T 166 requires sample shrinkage, which can be dehydrated by freeze drying or desiccant. Freeze-drying method. Take an appropriate amount of the mixed sample and put it into a freeze-dryer (6.6) to dry and dehydrate. Dried sample Need to grind and mix. Weigh a 10 g (accurate to 0.01 g) sample for extraction. Desiccant method. Weigh 10 g (accurate to 0.01 g) fresh sample, add Soxhlet extraction method with an appropriate amount of anhydrous sodium sulfate (5.9), A proper amount of diatomaceous earth (5.10) is added to the pressurized fluid extraction method, ground into a quicksand shape, and all transferred to an extraction device for extraction. 7.3 Determination of moisture When the extracted sample is weighed, another sample is weighed for moisture determination. Determination of soil dry matter content according to HJ According to the requirements of 613, the determination of sediment moisture content shall be carried out according to the requirements of GB 17378.5. 7.4 Preparation of test specimens 7.4.1 Extraction A mixed solvent of acetone-dichloromethane (5.5) was used as an extractant, and extraction was performed by Soxhlet extraction or pressurized fluid extraction. Soxhlet extraction method. Carefully transfer all samples (7.2) into the Soxhlet extraction sleeve (5.14), and place the sleeve in the Soxhlet extraction Add.200 ml of acetone-dichloromethane mixed solvent (5.5) to the bottom tube of the extractor reflux tube for reflux extraction for 24 h. The degree of control is 3 to 4 times/h, and the extract is collected. Pressurized fluid extraction method. Fill the sample (7.2) according to HJ 783, and collect the extract after static extraction for 3 times. Extract Take reference conditions. carrier gas pressure 0.8 MPa, heating temperature 100 ° C, extraction pressure 1.034 × 107 Pa (1500 psi), pre-addition Thermal equilibrium was 5 min, static extraction was 5 min, solvent was rinsed at 60% of the cell volume, and nitrogen was purged for 60 s. Note. If validated, other equivalent extraction methods can be used. 7.4.2 Filtration and dewatering Place a layer of glass wool or glass fiber filter (5.13) in the glass funnel and add an appropriate amount of anhydrous sodium sulfate (5.9). The liquid was filtered into a concentration container. Wash the extraction container with 2 ~ 3 ml of acetone-dichloromethane mixed solvent (5.5) and rinse the leak. Bucket and collect them together in a concentrating container. 7.4.3 Concentration Concentrate the extract (7.4.2) to about 0.5 ml, add about 5 ml of n-hexane (5.3) and concentrate to about 1 ml. The agent was completely converted to n-hexane and was to be purified. 7.4.4 Purification Fix the solid-phase extraction column (5.12) on the solid-phase extraction device (6.5). 5 ml of acetone (5.1) followed by 10 ml Hexane (5.3) activates the extraction column and keeps the head wet. Approximately 1 ml of the extract (7.4.3) after the solvent has dried Transfer to the column, start to collect the effluent, wash the concentration container 3 times with 3 ml n-hexane (5.3), and transfer all the washing liquid into the column Then, the mixture was eluted with 10 ml of an acetone-n-hexane mixed solvent (5.6), and the entire eluate was collected. 7.4.5 Constant volume The purified eluate (7.4.4) is concentrated to about 0.5 ml, about 3 ml of acetonitrile (5.4) is added, and then concentrated to about 0.5 ml, The solvent was completely converted to acetonitrile, and the volume was adjusted to 1.0 ml with acetonitrile (5.4) to be tested. 7.5 Preparation of blank sample Use quartz sand (5.11) instead of the actual sample, and follow the same steps as the sample preparation (7.4) to prepare a blank sample.8 Analysis steps8.1 Instrument Reference Conditions Mobile phase. A is water, B is acetonitrile (5.4), the gradient elution reference procedure is shown in Table 1; flow rate. 1.0 ml/min; column temperature. 30 ℃; injection volume. 10 μl; detection wavelength. 222 nm, auxiliary qualitative wavelength. 231 nm. Table 1 Reference procedure for gradient elution Time (min) Mobile phase A (%) Mobile phase B (%) Continued Time (min) Mobile phase A (%) Mobile phase B (%) 8.2 Establishment of standard curve Take a certain amount of triazine pesticide standard solution (5.8), dilute with acetonitrile (5.4), and prepare at least 5 concentration points Quasi-series, the target compound mass concentration is 1.00 mg/L, 10.0 mg/L, 25.0 mg/L, 50.0 mg/L, 100 mg/L, Store in a brown vial for testing. According to the instrument reference conditions (8.1), the sample is analyzed from low concentration to high concentration in turn. Use the concentration of the target compound in the standard solution as the abscissa and the corresponding peak area (peak height) as the ordinate to establish the standard curve. 8.3 Standard sample chromatogram Figure 1 is a reference chromatogram of 11 triazine pesticides. 1-Ximazine; 2-Xinqutong; 3-Xicaojing; 4-Atrazine; 5-Zhongdingtong; 7- fendijing; 8- fendijin; 9- tedinjin; 10- fencajing; 11- dicamba Figure 1 Reference chromatograms of standard samples of 11 triazine pesticides (ρ = 5.00 mg/L) 8.4 Sample determination Test the sample (7.4) according to the same instrument conditions as the standard curve (8.2). If the target compound in the sample is concentrated The degree is beyond the range of the standard curve, and the sample needs to be re-extracted. After the appropriate amount of extraction solution is dispensed, follow steps 7.4.2 to 7.4.5 after re-processing. Determination. 8.5 Blank test The blank sample (7.5) was measured under the same conditions as the sample measurement (8.4).9 Calculation and representation of results9.1 Qualitative analysis Characterize by the retention time of the target compound, if necessary, standard sample addition method, absorption ratio at different wavelengths, Scanning UV spectra and other methods are helpful for characterization. 9.2 Result calculation The mass concentration of triazine pesticides in the soil sample is calculated according to formula (1). Vwm VVρ dmi 0ii i ×× ×× = (1) In the formula. wi--mass concentration of the target compound i in the sample, mg/kg; ρi--mass concentration of target compound i in the sample obtained from the standard curve, mg/L; Vi--constant volume of sample, ml; mi--sample size, g; wdm--the dry matter content of the sample,%; V0--total volume of extraction solution, ml; V--Volume of extraction solution used in analysis, ml. The mass concentration of triazine pesticides in the sediment sample is calculated according to formula (2). Vwm VVρ OH2j 0jj × -1 × ×× ) ( (2) In the formula. wj--mass concentration of target compound j in the sample, mg/kg; ρj--mass concentration of target compound j in the sample obtained from the standard curve, mg/L; Vj--constant volume of sample, ml; mj--sample size, g; wH2O--Moisture content of the sample,%; V0--total volume of extraction solution, ml; V--Volume of extraction solution used in analysis, ml. 9.3 Representation of results The number of digits after the decimal point in the measurement result is the same as the detection limit of the method. A maximum of 3 significant digits are retained. 10 Precision and accuracy 10.1 Precision Six laboratories performed spiked samples of quartz sand at levels of 0.50 mg/kg, 2.00 mg/kg and 8.00 mg/kg. Repeat determinations. The relative standard deviations in the laboratory are 1.5% -17%, 7.3% -17%, 2.2% -4.9%; Relative standard deviations were 2.4% to 9.7%, 10% to 14%, 4.3% to 5.8%; repeatability limits were 0.03 to 0.13, respectively. mg/kg, 0.40 ~ 0.63 mg/kg, 0.47 ~ 0.70 mg/kg; the reproducibility limits are 0.05 ~ 0.17 mg/kg, 0.40 ~ 0.63, respectively mg/kg, 0.49 ~ 0.95 mg/kg. Six laboratories add standards for sand, loam and clay at 0.50 mg/kg, 2.00 mg/kg and 8.00 mg/kg The product was tested in 6 replicates. Relative standard deviations in the laboratory are 1.9% ~ 15%, 8.7% ~ 21%, 1.7% ~ 16%; The relative standard deviations among laboratories were 2.9% ~ 9.0%, 13% ~ 19%, 5.0% ~ 6.9%, respectively; the limits of repeatability were 0.03 ~ 0.11 mg/kg, 0.53 ~ 0.73 mg/kg, 0.69 ~ 1.1 mg/kg; the reproducibility limits are 0.07 ~ 0.18 mg/kg, 0.53 ~ 0.73 mg/kg, 0.71 ~ 1.2 mg/kg. Six laboratories spike lake and river sediments at 2.00 mg/kg and 8.00 mg/kg The product was tested in 6 replicates. The relative standard deviations in the laboratory are 4.1% -17% and 4.4% -11%, respectively. Relative standard deviations were 9.9% to 13% and 5.7% to 8.5%; repeatability limits were 0.38 to 0.55 mg/kg and 0.94 ~ 1.4 mg/kg; reproducibility limits range from 0.41 ~ 0.55 mg/kg and 0.94 ~ 1.4 mg/kg. 10.2 Accuracy Six laboratories performed spiked samples of quartz sand at levels of 0.50 mg/kg, 2.00 mg/kg and 8.00 mg/kg. Repeat determinations. The average spike recovery rates are. 70% ~ 81%, 64% ~ 78%, 74% ~ 80%; The final values are. 70% ± 6% ~ 81% ± 12%, 64% ± 4% ~ 78% ± 6%, 74% ± 4% ~ 80% ± 4%. Six laboratories add standards for sand, loam and clay at 0.50 mg/kg, 2.00 mg/kg and 8.00 mg/kg The product was tested in 6 replicates. The average recovery rates for standard addition are. 71% ~ 81%, 62% ~ 72%, 62% ~ 82%; The final standard recovery values are. 71% ± 6% ~ 81% ± 12%, 62% ± 4% ~ 72% ± 2%, 62% ± 6% ~ 82% ± 4%. Six laboratories spike lake and river sediments at 2.00 mg/kg and 8.00 mg/kg The product was tested in 6 replicates. Spike recovery averages are 63% ~ 74% and 66% ~ 72% respectively; The values were 63% ± 8% ~ 74% ± 6% and 66% ± 2% ~ 72% ± 6%, respectively. See Appendix B for statistics on precision and accuracy results. 11 Quality Assurance and Quality Control 11.1 Blank test Each batch of samples (not more than 20) should analyze at least 2 laboratory blank samples, and the determination value of the target compound must not be Above method detection limit. Otherwise, check reagent blanks, instrument systems, and pre-treatment procedures. 11.2 Calibration The correlation coefficient of the standard curve should be ≥0.995. Each batch of samples (not more than 20) needs to be calibrated once with the middle concentration point of the standard curve. 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