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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 961-2018: Soil and sediment - Determination of carbamate pesticides - High performance liquid chromatography-triple quadrupole mass spectrometry Status: Valid
Basic dataStandard ID: HJ 961-2018 (HJ961-2018)Description (Translated English): Soil and sediment - Determination of carbamate pesticides - High performance liquid chromatography-triple quadrupole mass spectrometry Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z18 Word Count Estimation: 17,177 Date of Issue: 2018-07-29 Date of Implementation: 2019-01-01 Regulation (derived from): Ministry of Ecology and Environment Announcement No. 27 of 2018 Issuing agency(ies): Ministry of Ecology and Environment HJ 961-2018: Soil and sediment - Determination of carbamate pesticides - High performance liquid chromatography-triple quadrupole 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. Soil and sediment - Determination of carbamate pesticides - High performance liquid chromatography-triple quadrupole mass spectrometry National Environmental Protection Standard of the People's Republic Soil and sediment carbamate pesticides Determination of high performance liquid chromatography - triple quadrupole Mass spectrometry Soil and sediment-Determination of carbamate pesticides-High Performance liquid chromatography-triple quadrupole mass Spectrometry Published on.2018-07-29 2019-01-01 Implementation Ministry of Ecology and Environment released i directory Foreword.ii 1 Scope 1 2 Normative references 1 3 Principle of the method 1 4 interference and elimination..1 5 reagents and materials..2 6 instruments and equipment..2 7 samples..3 8 Analysis step 4 9 Calculation and representation of results 7 10 Precision and Accuracy.9 11 Quality Assurance and Quality Control 10 12 Waste treatment..10 Appendix A (Normative Appendix) Method Detection Limit and Lower Measurement Limit..11 Appendix B (informative) Method Precision and Accuracy 12 ForewordTo implement the "Environmental Protection Law of the People's Republic of China", protect the ecological environment, protect human health, regulate soil and sink This standard is established for the measurement method of carbamate pesticides in the product. This standard specifies high performance liquid chromatography-triple quadrupole for the determination of 15 carbamate pesticides in soil and sediment. Mass spectrometry. Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix. This standard is the first release. This standard is formulated by the Environmental Monitoring Department and the Science and Technology Standards Department. This standard was drafted. Zhejiang Environmental Monitoring Center. This standard is verified by. Jiangsu Environmental Monitoring Center, Zhejiang Zhoushan Marine Ecological Environment Monitoring Station, Hangzhou Environment Monitoring Center Station, Suzhou Environmental Monitoring Center, Shaoxing Environmental Monitoring Center Station and Jiaxing Environmental Protection Monitoring Station. This standard is approved by the Ministry of Ecology and Environment on July 29,.2018. This standard has been implemented since January 1,.2019. This standard is explained by the Ministry of Ecology and Environment.1 Determination of soil and sediment carbamate pesticidesHigh performance liquid chromatography-triple quadrupole mass spectrometry Warning. The solvents and standard solutions used in the experiment are harmful to human health. The solution preparation and sample preparation process should be Wear in a fume hood; wear protective equipment as required to avoid direct contact with skin and clothing.1 Scope of applicationThis standard specifies high performance liquid chromatography-triple quadrupole for the determination of 15 carbamate pesticides in soil and sediment. Mass spectrometry. This standard applies to soil and sediments such as chlorpyrifos, methomyl, dioxin, aldicarb, chlorpyrifos, carbofuran, and 15 kinds of ammonia such as chlorpyrifos, carbaryl, ethyl thiophene, anti-蚜威, isoprocarb, zhongdingwei, methylthiocarb, chlorpyrifos and cotton ring Determination of carbamate pesticides. When the sample volume is 10 g, the sample volume is 1.0 ml, and the injection volume is 1.0 μl, 15 carbamate farmers The detection limit of the drug is 1 to 2 μg/kg, and the lower limit of determination is 4 to 8 μg/kg. See Appendix A for details.2 Normative referencesThis standard refers to the following documents or their terms. For undated references, the valid version applies to this standard. GB 17378.3 Marine monitoring specification Part 3. Sample collection, storage and transport GB 17378.5 Marine monitoring specification Part 5. Sediment analysis HJ 494 Water Quality Sampling Technical Guidance HJ 613 Determination of dry matter and moisture in soils - Gravimetric method HJ 783 Extraction of soil and sediment organic matter by pressurized fluid extraction HJ/T 166 Technical Specifications for Soil Environmental Monitoring3 Principle of the methodThe carbamate pesticide in the soil or sediment is extracted by organic solvent, purified by solid phase extraction column, concentrated, and made up to volume. It was determined by high performance liquid chromatography-triple quadrupole mass spectrometry and quantified by internal standard method according to retention time and characteristic ion characterization.4 interference and eliminationSubstances with similar retention times and molecular ion peaks interfere with the determination by changing the mobile phase and changing the quantification Ion pairs or high resolution mass spectrometry to eliminate interference. 25 reagents and materials Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. The pure water of the standard. 5.1 Methanol (CH3OH). liquid chromatography grade. 5.2 Dichloromethane (CH2Cl2). liquid chromatography grade. 5.3 Ammonium acetate (CH3COONH4). excellent grade pure. 5.4 anhydrous sodium sulfate (Na2SO4). The muffle furnace was fired at 450 ° C for 4 h, cooled slightly, and placed in a desiccator for use. 5.5 Methanol-dichloromethane mixed solvent. 1 2. Mix with methanol (5.1) and dichloromethane (5.2) in a volume ratio of 1.2. 5.6 Methanol-dichloromethane mixed solvent. 19. Mix with methanol (5.1) and dichloromethane (5.2) in a volume ratio of 1.9. 5.7 Ammonium acetate solution. c(CH3COONH4) = 5 mmol/L. Take 192.5 mg of ammonium acetate (5.3) and dissolve to a volume of 500 ml with water. 5.8 Methanol-ammonium acetate mixed solution. 2 3. Mix with methanol (5.1) and ammonium acetate solution (5.7) in a 2.3 volume ratio. 5.9 Standard stock solution of carbamate pesticide. ρ=100 mg/L. Purchase commercially available certified standard solutions directly and store them in accordance with the standard solution certificate. 5.10 Standard use solution for carbamate pesticides. ρ=10 mg/L. Take 500 μl of carbamate pesticide standard stock solution (5.9) in a 5 ml volumetric flask and dilute to volume with methanol (5.1). Mix well, place in a -18 ° C refrigerator, sealed, protected from light, and the shelf life is 6 months. 5.11 Standard internal standard stock solution. ρ=100 mg/L. Directly purchase commercially available carbaryl-D7 and methomyl-D3 certified standard solutions, and store them according to the standard solution certificate. 5.12 Internal standard standard use solution. ρ=10 mg/L. Take 500 μl of internal standard stock solution (5.11) in a 5 ml volumetric flask, dilute to volume with methanol (5.1), mix and place. -18 ° C refrigerator, sealed, protected from light, the shelf life is 6 months. 5.13 Solid phase extraction column. Graphitized carbon black/N-propyl ethylene diamine composite filler column (500 mg/6 ml) or other properties A similar solid phase extraction column. 5.14 Diatomaceous earth. 0.6 to 0.9 mm (30 to 20 mesh). 5.15 Quartz sand. 150 ~ 830 μm (200 ~ 100 mesh). The muffle furnace was fired at 450 ° C for 4 h, cooled slightly, and placed in a clean dryer for later use. 5.16 Filter. 0.22 μm PTFE or other equivalent material. 5.17 Nitrogen. purity ≥ 99.99%. 5.18 Argon. purity ≥ 99.99%.6 Instruments and equipment6.1 High Performance Liquid Chromatography - Triple Quadrupole Mass Spectrometer. 36.1.1 Mass spectrometer. Triple quadrupole mass spectrometer with electrospray ion source with multiple reaction monitoring. 6.1.2 Chromatograph. Gradient elution function. 6.1.3 Column. Low-bond octadecylsilane-bonded silica gel column with a particle size of 1.7 μm and a column length of 50 mm. The inner diameter is 2.1 mm. Other columns with similar properties that meet the analytical requirements can also be used. 6.2 Freeze dryer. 6.3 Extraction device. pressurized fluid extractor (with extraction tank below 50 ml), Soxhlet extraction device, automatic Soxhlet extraction Instrument or other equivalent extraction device. 6.4 Concentrator. Nitrogen blown concentrator, rotary evaporator or other equivalent equipment. 6.5 Analytical balance. The sensitivity is 0.01 g. 6.6 Common instruments and equipment used in general laboratories.7 samples7.1 Sample collection and preservation Collect and store soil samples in accordance with the relevant requirements of HJ/T 166, and collect water bodies according to the relevant requirements of HJ 494 Samples of marine sediments were collected according to the relevant requirements of GB 17378.3. After sample collection, seal and avoid at 0~4°C Light preservation, extraction completed within 7 days. 7.2 Preparation of samples Remove foreign matter (branches, leaves, stones, etc.) from the sample and mix the sample thoroughly. If the sample has a high moisture content, It should be dried first with a freeze dryer (6.2). Weigh two samples of approximately 10 g (accurate to 0.01 g). One sample of the soil sample is used to determine the dry matter content; the other is used for extraction. When using pressurized fluid extraction, add Add appropriate amount of diatomaceous earth (5.14) and put it into the extraction tank. When using Soxhlet extraction, add an appropriate amount of anhydrous sodium sulfate (5.4) and load Extract the tube. One sample of the sediment is used to determine the water content; the other is used for extraction, and the extraction method is based on the soil sample. 7.3 Determination of moisture The dry matter content of the soil samples was determined according to HJ 613, and the moisture content of the sediment samples was determined in accordance with GB 17378.5. 7.4 Preparation of samples 7.4.1 Extraction 7.4.1.1 Pressurized fluid extraction The carbamate pesticide in the sample was extracted with a methanol-dichloromethane mixed solvent (5.5) at a pressure of 10.34 Mpa. The extraction temperature is 80oC, the heating time is 5 min, the static extraction time is 5 min, the flushing amount is 80%, and the nitrogen is purged for 60 s after extraction. Cycle extraction 3 times. Or set and optimize the extraction conditions according to HJ 783. 7.4.1.2 Soxhlet extraction Place the filter cartridge in the Soxhlet extractor return tube and add.200 ml methanol-dichloromethane mixed solvent to the round bottom solvent bottle. 4 (5.5), extracted for 12 h, and the reflux rate is controlled at 4-6 times/h. After the extraction is completed, the round bottom solvent bottle is taken out and concentrated. Note. Other equivalent extraction methods can be used if verified. 7.4.2 Concentration The extract (7.4.1) was concentrated to nearly 1.0 ml with a concentrating device (6.4) to be purified. 7.4.3 Purification Activate the solid phase extraction column (5.13) at a rate of 2 ml/min with 5.0 ml of methanol-dichloromethane mixed solvent (5.6). Transfer the concentrate (7.4.2) to the column head just before the filler is exposed to air, before the filler is about to be exposed to air. The extraction column was eluted with 5.0 ml of a methanol-dichloromethane mixed solvent (5.6), and the eluate was collected in a graduated tube. Note. When using different batches of extraction column to purify the sample, the amount of elution solvent should be determined experimentally. 7.4.4 Concentration after purification Concentrate the eluate (7.4.3) below 30oC to near-dry with a nitrogen blow concentrator (6.4), and add 20 μl of internal standard. Liquid (5.12), make up to 1.0 ml with methanol-ammonium acetate mixed solution (5.8), filter membrane (5.16), to be tested. The treated samples should be stored frozen in a refrigerator below -18 ° C and analyzed in 30 days. 7.5 Preparation of blank samples A blank sample was prepared by replacing the actual sample with quartz sand (5.15) in the same manner as in sample preparation (7.4).8 Analysis steps8.1 Reference measurement conditions 8.1.1 Chromatographic conditions Mobile phase. mobile phase A methanol (5.1), mobile phase B ammonium acetate solution (5.7), gradient elution procedures are shown in Table 1. flow Speed. 0.2 ml/min; injection volume. 1.0 μl; column temperature. 45oC. Table 1 Gradient elution procedure Time (min) mobile phase A (%) mobile phase B (%) 5.0 99 1 5.5 99 1 7.0 40 60 8.1.2 Mass spectrometry conditions Electrospray source, positive ion mode, capillary voltage. 3000 V, desolvation gas temperature. 350oC, source temperature. 110oC, Desolvent gas flow. 500 ml/min, cone flow. 50 ml/min. The detection method is multi-reaction monitoring. See the specific conditions. 5 Table 2. Note. For different mass spectrometers, the parameters may vary and the mass spectrometry parameters should be optimized to the optimum before measurement. Table 2 Target multiple reaction monitoring conditions Numbered compound monitoring ion pair (m/z) cone voltage (V) collision energy (V)1 kill line237.1 >71.9* 12 10 237.1 >90.1 12 12 2 灭多威 163.4 >88.4* 15 9 163.4 >106.0 15 103 Dioxin224.4 >123.4* 25 15 224.4 >167.1 25 134 Aldicarb208.5 >116.3* 10 10 208.5 >88.9 10 85 worms224.4 >167.4* 18 9 224.1 >109.1 18 106 grams of Budweiser222.4 >165.4* 25 15 222.4 >123.0 25 147 Killer210.5 >111.3* 20 13 210.5 >168.1 20 128 carbaryl202.4 >145.2* 20 18 202.4 >127.1 20 169 ethion226.4 >107.2* 15 9 226.4 >164.1 15 12 10 anti-random 239.5 >72.4* 18 19 239.5 >182.2 18 18 11 Isoprocarb 194.5 >95.0* 15 12 194.5 >137.2 15 12 12 Zhong Dingwei 208.4 >95.3* 15 12 208.4 >152.0 15 15 13 methylthiocarb 226.4 >169.4* 20 13 226.4 >121.0 20 12 14 murder 208.4 >109.4* 20 15 208.4 >151.2 20 16 15 Cotton Bell 400.5 >238.2* 12 8 400.5 >91.1 12 10 16 灭多威-D3 166.1 >88.1* 15 9 17 Carbaryl-D7 209.0 >152.1* 20 18 Note. Band * is a quantitative ion pair. 8.1.3 Correction of the mass spectrometer Perform mass spectrometer mass and resolution calibration according to the instrument manual, and test after the instrument performance is normal. 68.2 Calibration 8.2.1 Establishment of the standard curve Transfer the appropriate amount of carbamate pesticide standard solution (5.10) to a 5 ml volumetric flask and add 100 μl of internal label. Quasi-use liquid (5.12), diluted with methanol-ammonium acetate mixed solution (5.8) to the mark, to prepare a standard of at least 5 concentration points Series, standard series concentrations are 0.02 μg/ml, 0.05 μg/ml, 0.10 μg/ml, 0.20 μg/ml and 0.50 μg/ml (This is the reference concentration). The standard series solution is injected sequentially from low concentration to high concentration, and analyzed according to the measurement conditions (8.1). Taking the target concentration as the abscissa, the ratio of the peak area of the target and the corresponding internal standard concentration to the peak area of the corresponding internal standard For the ordinate, a standard curve is established. 8.2.2 Calculation of average relative response factor The relative response factor iRRF of the target in point i of the standard series is calculated according to formula (1). ISi ISi i A RRF (1) In the formula. iRRF - the relative response factor of the i-th target in the standard series; iA - the peak area of the i-th target in the standard series; ISiA - the peak area of the internal standard; ISi - concentration of internal standard, μg/ml; I - The concentration of the target at the i-th point in the standard series, μg/ml. The average relative response factor RRF of the target is calculated according to formula (2). RRF RRF I 1 (2) In the formula. RRF - the average relative response factor of the target; iRRF - the relative response factor of the i-th target in the standard series; N-standard series points, 5. 8.3 Sample determination The measurement of the sample (7.4) was carried out in the same manner as in the standard curve establishment (8.2.1). 8.4 Blank test The blank sample (7.5) was measured in the same manner as in the sample measurement (8.3). 79 Calculation and representation of results 9.1 Qualitative analysis According to the qualitative analysis of retention time, under the same experimental conditions, the retention time of the target in the sample and the standard solution For the retention time of the standard, the deviation should be less than or equal to 0.1 min. S/N of the target peak (the letter of the target in the instrument) No./Instrument Noise) is greater than or equal to 3. The relative abundance of a certain component of a sample in the sample samK and the standard solution close to the concentration The relative abundance of the neutral ionic ions stdK is compared, and the deviation is in accordance with Table 3, and it can be determined that the target is present in the sample. The total ion chromatograms of 15 carbamate pesticides and 2 internal standards are shown in Figure 1. The relative abundance of a certain component of the sample, samK, is calculated according to formula (3). Sam A K (3) Where. samK ─ the relative abundance of a component of a sample in the sample, %; 2A - the peak area (or peak height) of a qualitative ion pair of a component in the sample; 1A - The peak area (or peak height) of a given pair of quantitative ions in a sample. The relative abundance of a certain component of a standard solution, stdK, is calculated according to formula (4). Std Std Std K (4) Where. stdK ─ the relative abundance of a component of a standard solution, %; 2stdA - the peak area (or peak height) of a qualitative ion pair of a component in a standard solution; 1stdA—The peak area (or peak height) of a quantitative ion pair of a component in a standard solution. Table 3 Maximum allowable deviation of relative ion abundance in qualitative confirmation/% Indicator evaluation criteria stdK stdK >50 20< stdK ≤50 10< stdK ≤20 stdK ≤10 The maximum allowable deviation of samK is ±20 ±25 ±30 ±50 9.2 Quantitative analysis 9.2.1 Calculated using the average relative response factor The concentration of the target in the sample is calculated according to formula (5). RRFA IS ISx i (5) Where. i - the concentration of the target in the sample, mg/L; xA - the peak area of the target; Peak area of the ISA-internal standard; 8IS - concentration of internal standard, 0.2 μg/ml; RRF - The average relative response factor of the target. Time 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 180301carbamate--137 16. MRM of 1 Channel ES 400.5 > 238.2 2.26e5 5.09 5.11 5.14 180301carbama......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 961-2018_English be delivered?Answer: Upon your order, we will start to translate HJ 961-2018_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 961-2018_English with my colleagues?Answer: Yes. The purchased PDF of HJ 961-2018_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. 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