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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 1053-2019: Soil and sediment -- Determination of 8 amide pesticides -- Gas chromatography mass spectrometry Status: Valid
Basic dataStandard ID: HJ 1053-2019 (HJ1053-2019)Description (Translated English): Soil and sediment -- Determination of 8 amide pesticides -- Gas chromatography mass spectrometry Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z18 Classification of International Standard: 13.080 Word Count Estimation: 20,224 Date of Issue: 2019 Date of Implementation: 2020-04-24 Issuing agency(ies): Ministry of Ecology and Environment HJ 1053-2019: Soil and sediment -- Determination of 8 amide pesticides -- Gas chromatography mass spectrometry---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 eight amide pesticides Gas chromatography-mass spectrometry) National Environmental Protection Standard of the People's Republic of China Determination of 8 amide pesticides in soil and sediment Gas chromatography-mass spectrometry Soil and sediment-Determination of 8 amide pesticides -Gas chromatography mass spectrometry 2019-10-24 released 2020-04-24 Implementation release ContentsForeword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Methodology ... 1 4 Reagents and materials ... 1 5 Instruments and equipment ... 3 6 Sample ... 3 7 Analysis steps ... 5 8 Results calculation and representation ... 7 9 Precision and accuracy ... 8 10 Quality Assurance and Quality Control ... 9 11 Waste disposal ... 10 Appendix A (Normative Appendix) Method detection limit and determination lower limit ... 11 Appendix B (informative) Mass spectrometry reference conditions ... 12 Appendix C (Informative) Precision and accuracy of methods ... 13ForewordIn order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination method of amide pesticides in soil and sediment, and formulate this standard. This standard specifies gas chromatography-mass spectrometry for the determination of eight amide pesticides in soil and sediment. Appendix A of this standard is a normative appendix, and appendixes B and C are informative appendices. 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. Verification units of this standard. Zhejiang Environmental Monitoring Center, Chongqing Ecological Environment Monitoring Center, Hainan Environmental Monitoring Center Xinzhan Station, Wuhan Environmental Monitoring Center, Huangshi Environmental Monitoring Station and Tai'an Environmental Protection 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 8 amide pesticides in soil and sediments by gas chromatography-mass spectrometry Warning. The organic solvents and standard materials used in the experiment are toxic and hazardous substances. Solution preparation and sample preparation The process should be carried out 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 gas chromatography-mass spectrometry for the determination of eight amide pesticides in soil and sediment. This standard applies to acetochlor, isopropachlor, alachlor, diazepam, methachlor, fenitrothion, Determination of Butachlor and Pretilachlor 8 Amides When the sample volume is 10 g and the constant volume is 1.0 ml, the detection limit of the method is as follows. 0.01 ～ 0.02 mg/kg, the lower limit of measurement is 0.04 ～ 0.08 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 Marine Monitoring Code 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 911 Soil and sediment organic matter extraction ultrasonic extraction method HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 166 Technical Specifications for Soil Environmental Monitoring3 Method principleUsing acetone-n-hexane as an extractant, extract the soil by Soxhlet extraction, pressurized fluid extraction or ultrasonic extraction Or the amide pesticides in the sediment are purified by solid phase extraction, concentrated and fixed to volume, then separated by gas chromatography and detected by mass spectrometry. Under warranty Retention time, fragment ion mass-to-charge ratio and abundance ratio were qualitative and quantified by internal standard method.4 Reagents and materialsUnless otherwise specified, analytical reagents that meet national standards are used. Experimental water is freshly prepared ultrapure water Or distilled water. 4.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml. 4.2 Hydrochloric acid solution. 1 5. Measure 5 ml of hydrochloric acid (4.1), slowly add to 25 ml of water, and mix well. 4.3 Copper particles (Cu). Purity ≥99.5%. Activate with hydrochloric acid solution (4.2) before use to remove surface oxides. Wash away the residual acid with distilled water, and then use propylene Ketone cleaning, and finally drying under a stream of nitrogen, gives the copper particles a shiny surface. Handle before each use. 4.4 Acetone (C3H6O). pesticide residue level. 4.5 n-hexane (C6H14). pesticide residue grade. 4.6 Dichloromethane (CH2Cl2). pesticide residue level. 4.7 Methanol (CH3OH). chromatographically pure. 4.8 Acetone-n-hexane mixed solvent. 1 1. Acetone (4.4) and n-hexane (4.5) were mixed in a 1. 1 volume ratio. 4.18 Diatomaceous earth. 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. 4.19 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. 4.20 Solid-phase extraction column. Commercially available Flory silica, silica gel, amino, or other equivalent solid-phase extraction columns, 1 000 mg/6 ml or larger capacity specifications. 4.21 Glass wool or glass fiber membrane. Dip with dichloromethane (4.6) before use. After it has completely evaporated, place it in a ground glass bottle and keep it sealed. 4.22 Soxhlet extraction sleeve. glass fiber or natural fiber material sleeve. Glass fiber sleeves are placed in a muffle furnace at 450 ° C for 4 hours before use. Natural fiber material sleeves should be used and sampled before use. The product was extracted with the same solvent and washed. 4.23 Nitrogen. purity ≥99.99%. 4.24 Helium. Purity ≥99.999%.5 Instruments and equipment5.1 Gas chromatograph-mass spectrometer. Capillary column and split/splitless inlet, programmable temperature, mass spectrometer with electron bomb Shock ionization (EI) source. 5.2 Chromatographic column. the stationary phase is 35% phenyl-methyl polysiloxane, the column length is 30 m, the inner diameter is 0.25 mm, and the film thickness is 0.25 μm Fused silica capillary columns can also be used with other similar performance columns to meet analytical requirements. 5.3 Extraction device. Soxhlet extraction device, pressurized fluid extraction device or ultrasonic extraction device. 5.4 Concentration device. Rotary evaporator, nitrogen blower or other equipment with equivalent performance. 5.5 Solid phase extraction device. 5.6 Freeze dryer. 5.7 Brown glass bottle. 5.8 Analytical balance. Sensitivity is 0.01 g and 0.1 mg. 5.9 General laboratory instruments and equipment.6 samples6.1 Sample collection and storage Collect soil samples in accordance with the relevant regulations of HJ/T 166, in accordance with GB 17378.3, GB 17378.5, HJ 494, HJ 495 And HJ/T 91 relevant regulations to collect sediment samples. After the samples are collected, they should be stored in brown glass bottles (5.7). During transportation, they should be refrigerated, sealed, and protected Keep it light and ship it back to the laboratory for analysis as soon as possible. If it cannot be analyzed in a timely manner, it should be refrigerated, sealed and protected from light below 4 ° C. If The analysis of enemy pupae should be completed within 24 h. If the enemy pupae are not analyzed, the extraction can be completed within 10 d. Extract at 4 ° C Keep refrigerated, sealed and protected from light for 20 days. 6.2 Preparation of samples Place the sample in a polytetrafluoroethylene or stainless steel plate, remove foreign matter such as sticks, leaves, stones, etc. press Perform sample reduction as required by HJ/T 166. Can be freeze-dried or desiccant dehydration two drying methods dehydration drying. Freeze-drying method. Take an appropriate amount of the sample after mixing and put it into a freeze-dryer (5.6) to dry and dehydrate for at least 12 h. dry The subsequent samples need to be ground and mixed. Weigh a 10 g (accurate to 0.01 g) sample for extraction. Desiccant method. Weigh a fresh sample of 10 g (accurate to 0.01 g), add an appropriate amount of anhydrous sodium sulfate (4.17), Mix well into quicksand, transfer all to extraction container for use. If using pressurized fluid extraction, use diatomaceous earth (4.18) Instead of anhydrous sodium sulfate (4.17) dehydration. 6.3 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. 6.4 Preparation of test specimens 6.4.1 Extraction The extraction method may be Soxhlet extraction, pressurized fluid extraction or ultrasonic extraction. Soxhlet extraction method. Transfer all prepared soil or sediment samples (6.2) into the Soxhlet extraction sleeve (4.22), Add 10.0 μl of replacement standard solution (4.14), carefully place in the Soxhlet extractor return tube, and add.200 ml to the bottom bottle The acetone-n-hexane mixed solvent (4.8) was extracted for 15-18 hours, and the reflux rate was controlled at 4-6 times per hour, and the extract was collected. Pressurized fluid extraction method. Fill the prepared soil or sediment sample (6.2) into the extraction cell of the pressurized fluid extractor After adding 10.0 μl of the standard solution of substitute (4.14), extract it on the machine and collect the extract. Extraction according to the following reference conditions Take. Extraction solvent is acetone-n-hexane mixed solvent (4.8); extraction temperature is 80 ℃; heating time is 5 min; Extraction time is 5 min; extraction pressure is 1.034 × 107 Pa (1500 psi); solvent eluent volume is 60% cell volume; Ring extraction 3 times; nitrogen (4.23) was purged for 60 s after extraction. Or set and optimize extraction conditions according to HJ 783. Ultrasonic extraction method. Transfer all prepared soil or sediment samples (6.2) into a glass beaker and add 10.0 μl Alternative standard solution (4.14), ultrasonic extraction conditions can be set and optimized according to HJ 911. Note. If validated, other equivalent extraction methods can be used. 6.4.2 Concentration and replacement of solvents Transfer the extraction solution (6.4.1) to a concentration container, and concentrate the extraction solution to about 2 ml with a concentration device (5.4). Add 5 ml of n-hexane (4.5) and continue to concentrate to about 2 ml. Repeat this step 1 or 2 times. If significant water is present in the extract Points need to be dehydrated. Place a layer of glass wool or glass fiber filter membrane (4.21) on the glass funnel and add an appropriate amount of anhydrous sulfuric acid Sodium (4.17), the extract was filtered into a concentration vessel. Rinse the funnel twice with 10 ml n-hexane (4.5) and collect the extract. Take the solution and concentrate it to about 1 ml with a concentration device (5.4). 6.4.3 Purification 6.4.3.1 Desulfurization If the sample contains elemental sulfur, the extraction solution must be desulfurized using copper pellets (4.3). Add suitable solution to the extract (6.4.2) Measure the copper granules (4.3), shake gently and let it stand. Use a dropper to aspirate the extract and transfer it to a concentration container. Use 1 ～ 2 ml The extraction bottle was washed twice with n-hexane (4.5), and the washing solution was transferred to a concentration container. Use of concentration device (5.4) Concentrated to about 1 ml. 6.4.3.2 Purification by solid phase extraction column Fix the solid phase extraction column (4.20) on the solid phase extraction device (5.5). 5 ml of acetone (4.4) followed by 10 ml Hexane (4.5) activates the extraction column and keeps the head wet. Before the solvent is allowed to dry, transfer approximately 1 ml of the concentrated extract Into the column, begin to collect the effluent, wash the concentration container 3 times with 3 ml n-hexane (4.5), and transfer all the washing liquid into the column Then, elution was performed with 10 ml of an acetone-n-hexane mixed solvent (4.9), and the entire eluate was collected. 6.4.4 Concentrated volume The eluate (6.4.3.2) was concentrated to about 2 ml with a concentration device (5.4), and 5 ml of n-hexane (4.5) was added to continue the concentration Reduce to about 0.5 ml, add 20.0 μl of internal standard use solution (4.16), and bring the volume to 1.0 ml for measurement. 6.5 Preparation of blank sample Use quartz sand (4.19) instead of the actual sample, and follow the same steps as the sample preparation (6.4) to prepare a blank sample.7 Analysis steps7.1 Instrument Reference Analysis Conditions 7.1.1 Gas chromatography reference conditions Inlet temperature. 270 ° C; injection mode. splitless injection; injection volume. 1.0 μl; column flow rate. 1.0 ml/min; Oven temperature. 80 ° C (hold for 1 min), rise to 190 ° C at 30 ° C/min, and then rise to 220 ° C at 5 ° C/min (hold 3 min), and then raised to 280 ° C (hold for 2 min) at 20 ° C/min. 7.1.2 Mass spectrometry conditions Ion source temperature. 230 ° C; transmission line temperature. 280 ° C; electron impact ionization (EI) mode, ionization energy 70 eV. Data acquisition method. Select ion scan. Quantitative and qualitative ionic mass-to-charge ratios of amide pesticides were obtained based on full scan standards Take the determined mass spectrum, see Appendix B. 7.2 Instrument performance check Before the analysis of the sample, it should be tuned and checked according to the calibration compounds and procedures specified in the instrument manual. If it does not meet the requirements, You need to optimize the mass spectrometer parameters or clean the ion source. 7.3 Calibration 7.3.1 Preparation and determination of calibration series Take a certain amount of amide pesticide standard use solution I (4.12) or amide pesticide standard use solution II (4.13) and substitute Substitute standard solution (4.14) into the injection vial, add 20.0 μl of internal standard use solution (4.16), and use acetone-n-hexane The mixed solvent (4.9) was diluted and made up to 1000 μl, so that the mass concentration of amide pesticides and substitutes was 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 25.0 mg/L. Can also be configured based on instrument sensitivity or linear range to cover Standard series of at least 5 concentration points for a sample concentration range. According to the instrument reference conditions (7.1), the sample was analyzed from low concentration to high concentration in order to obtain the target compounds of different concentrations. Mass spectrum, recording the retention time of each target and the peak area or peak height of the quantitative ion mass spectrum peak. Under the instrument reference conditions recommended by this standard, the total ion chromatogram of the target is shown in Figure 1. 1. Acetochlor-d11 (substitute); 2. Acetochlor; 3. Isopronil; 4. Alachlor; 5. Dichlorbin; 6. Metolachlor-d6 (internal standard) ; 7. isopropyl Alachlor; 8. Fenitrothion; 9. Butachlor; 10. Propachlor Figure 1 Total ion chromatogram of amide pesticides 7.3.2 Calculation of average relative response factor The relative response factor (RRFi) of the i-point target in the standard series is calculated according to formula (1). iIS ISi i ρ × A ρ × A = RRF (1) In the formula. RRFi--the relative response factor of the i-th target in the standard series; 𝐴𝑖--response value of the target ion quantitation ion in the standard series; 𝐴𝐼𝑆--response value of quantitative ion of internal standard in standard series; 𝜌𝐼𝑆--content of internal standard in standard series, mg/L; 𝜌𝑖--The content of the target substance at point i in the standard series, mg/L. The average relative response factor of the target is calculated according to formula (2). RRF = RRF 1 = ii (2) Where. 𝑅𝑅𝐹̅̅ ̅̅ ̅̅-the average relative response factor of the target; 𝑅𝑅𝐹𝑖--the relative response factor of the i-th target in the standard series; 𝑛--Standard points. The standard deviation (SD) of RRF is calculated according to formula (3). 1-n ) RRF- (RRF = SD 1 = i i∑ (3) The relative standard deviation (RSD) of RRF is calculated according to formula (4). 100% × RRF SD = RSD (4) The relative standard deviation (RSD) of the relative response factor (RRF) of the standard series target should be ≤20%. 7.3.3 Establishing a calibration curve using the least square method Taking the target concentration as the abscissa, the ratio of the response of the target and the concentration of the internal standard to the response of the internal standard For the ordinate, a calibration curve is established by least squares fitting, and the correlation coefficient of the curve should be ≥0.995. 7.4 Sample determination Test the sample (6.4) under the same instrument conditions as the calibration curve (7.3). If the target concentration in the sample Beyond the range of the calibration curve, the sample needs to be re-extracted. After the appropriate amount of extraction solution is dispensed, the measurement is performed after reprocessing according to step 6.4. 7.5 Blank test The blank sample (6.5) was measured by the same analysis procedure as the sample measurement (7.4).8 Results calculation and representation8.1 Qualitative analysis Through the retention time, the ion mass-to-charge ratio and the abundance ratio of the target in the sample and the target in the standard series Compare and characterize the target. The standard solution should be analyzed multiple times to obtain the average retention time of the target. The standard deviation of ± 3 times is the retention time window. The retention time of the target in the sample should be within its range. Relative abundance of qualifier ions to quantifier ions of the target in the sample and relative abundance of recently obtained standard samples Degree comparison, the relative deviation should be within ± 30%. 8.2 Quantitative analysis 8.2.1 Calculation of the mass concentration xρ of the target in the sample 8.2.1.1 Calculation using average relative response factor When the average relative response factor is used for calibration, the mass concentration xρ of the target in the sample is......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 1053-2019_English be delivered?Answer: Upon your order, we will start to translate HJ 1053-2019_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of HJ 1053-2019_English with my colleagues?Answer: Yes. 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