HJ 1242-2022 English PDFUS$489.00 · In stock
Delivery: <= 5 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 1242-2022: Water quality - Determination of 6 phthalate esters (PAEs) - Liquid chromatography-triple quadrupole mass spectrometry Status: Valid
Basic dataStandard ID: HJ 1242-2022 (HJ1242-2022)Description (Translated English): Water quality - Determination of 6 phthalate esters (PAEs) - Liquid chromatography-triple quadrupole mass spectrometry Sector / Industry: Environmental Protection Industry Standard Word Count Estimation: 21,259 Issuing agency(ies): Ministry of Ecology and Environment HJ 1242-2022: Water quality - Determination of 6 phthalate esters (PAEs) - 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. Water quality - Determination of 6 phthalate esters (PAEs) - Liquid chromatography-triple quadrupole mass spectrometry National Ecological Environment Standard of the People's Republic of China 6 kinds of phthalates in water quality Determination Liquid Chromatography-Triple Quadrupole Mass Spectrometry Water quality-Determination of 6 phthalate esters (PAEs) -Liquid chromatography-triple quadrupole mass spectrometry Posted on 2022-04-15 2022-11-01 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Principles of the method...1 4 Interference and cancellation...1 5 Reagents and materials...2 6 Instruments and equipment...3 7 Samples...3 8 Analysis steps...4 9 Result calculation and representation...7 10 Accuracy...8 11 Quality Assurance and Quality Control...10 12 Waste Disposal...10 13 Precautions...10 Appendix A (normative appendix) Method detection limit and lower limit of determination...11 Appendix B (informative) Accuracy of the method...12 Appendix C (informative appendix) Schematic diagram of trapping column installation...18 Determination of six phthalates in water quality liquid chromatography-triple quadrupole mass spectrometry Warning. The reagents and standard solutions used in this method have certain toxicity, and the preparation of reagents and sample preparation should be carried out in a fume hood When operating, wear protective equipment as required to avoid inhalation into the respiratory tract or contact with skin and clothing. 1 Scope of applicationThis standard specifies the liquid chromatography-triple quadrupole mass spectrometry method for the determination of six phthalates in water. This standard applies to surface water, groundwater, domestic sewage, industrial wastewater and seawater dimethyl phthalate (DMP), phthalate Diethyl formate (DEP), butyl benzyl phthalate (BBP), dibutyl phthalate (DBP), bis(2-phthalate) Determination of 6 kinds of phthalate compounds, including ethylhexyl) ester (DEHP) and di-n-octyl phthalate (DNOP). Acetonitrile extraction. when the sampling volume is 10.0 ml, the extraction volume is 5.0 ml, and the injection volume is 5 μl, the formula for the six target compounds is The detection limit of the method is 0.8 μg/L～9 μg/L, and the lower limit of determination is 3.2 μg/L～36 μg/L, see Appendix A for details. Hexane extraction. This method is only applicable to the determination of DBP and DEHP in surface water and groundwater. When the sampling volume is 100 ml, the extraction When the sample volume was 2.0 ml and the injection volume was 10 μl, the detection limits of DBP and DEHP were 0.4 μg/L and 0.3 μg/L, respectively. The lower limits are 1.6 μg/L and 1.2 μg/L, respectively, see Appendix A for details.2 Normative referencesThis 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 21749 Teaching Instruments and Equipment Safety Requirements Glass Instruments and Connecting Parts HJ 91.1 Technical Specification for Wastewater Monitoring HJ 91.2 Technical Specification for Surface Water Environmental Quality Monitoring HJ 164 Technical Specification for Groundwater Environmental Monitoring HJ 442.3 Technical Specifications for Environmental Monitoring in Offshore Seas Part III Water Quality Monitoring in Offshore Seas3 Principles of the methodPhthalates were extracted from water with acetonitrile or n-hexane as solvent, and separated and detected by liquid chromatography-triple quadrupole mass spectrometry. According to retention time and characteristic ion identification, internal standard method for quantification.4 Interference and cancellationDibutyl phthalate (DBP) and diisobutyl phthalate (DIBP) are isomers with relatively short chromatographic retention times. close, the DIBP interference can be excluded by the standard addition method.5 Reagents and MaterialsUnless otherwise stated, analytical reagents that meet national standards were used in the analysis, and the experimental water was newly prepared without target compounds. pure water. 5.1 Acetonitrile (CH3CN). chromatographically pure. 5.2 Methanol (CH3OH). chromatographically pure. 5.3 Acetone (CH3COCH3). chromatographically pure. 5.4 n-hexane (C6H14). chromatographically pure. 5.5 Isopropanol ((CH3)2CHOH). chromatographically pure. 5.6 Formic acid (HCOOH). chromatographically pure. 5.7 Sodium hydroxide (NaOH). excellent grade pure. 5.8 Hydrochloric acid (HCl). ρ=1.19 g/ml, excellent grade. 5.9 Sodium chloride (NaCl). Before use, it should be placed in a muffle furnace and burned at 400 °C for 4 hours. After cooling, it should be put into a ground glass bottle and sealed with aluminum foil, and placed in a desiccator. internal storage. Shelf life should not exceed 2 weeks. 5.10 Formic acid solution. Pipette 2 ml of formic acid (5.6) into a 1 L volumetric flask pre-added with an appropriate amount of experimental water, and make up to volume with experimental water. 5.11 Sodium hydroxide solution. ρ(NaOH)=0.4 g/ml. Weigh 40 g of sodium hydroxide (5.7) and dissolve it in 100 ml of experimental water. 5.12 Hydrochloric acid solution. Mix with hydrochloric acid (5.8) and water in a volume ratio of 1.1. 5.13 Standard stock solution of phthalates. ρ=100 mg/L～1000 mg/L. Certified standard solutions can be purchased, target compounds include dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate phthalate, dibutyl phthalate, bis(2-ethylhexyl) phthalate, and di-n-octyl phthalate, and the solvent is methanol. Reserve The liquid should be stored in accordance with the product manual. 5.14 Standard intermediate solution of phthalates. ρ=20.0 mg/L. Take an appropriate amount of the phthalate compound stock solution (5.13) and dilute it with acetone (5.3). The standard intermediate solution should be refrigerated and sealed below 4 °C. Sealed and protected from light, the shelf life is 2 months. 5.15 Standard solution for phthalates. ρ=2.00 mg/L. Take an appropriate amount of the phthalate compound intermediate solution (5.14) and dilute it with acetone (5.3). The standard solution should be refrigerated and sealed below 4°C. Sealed and protected from light, the shelf life is 2 months. 5.16 Internal standard stock solution. ρ=100 mg/L～1000 mg/L. Certified standard solutions can be purchased, and the internal standards are dimethyl phthalate-d4 (DMP-d4), diethyl phthalate-d4 (DEP-d4), Butylbenzyl phthalate-d4 (BBP-d4), dibutyl phthalate-d4 (DBP-d4), bis(2-ethylhexyl) phthalate Ester-d4 (DEHP-d4) and di-n-octyl phthalate-d4 (DNOP-d4) in methanol. The stock solution is stored in accordance with the product manual. 5.17 Internal standard solution. ρ=10.0 mg/L. Take an appropriate amount of internal standard stock solution (5.16) and dilute it with acetone (5.3). The internal standard solution should be refrigerated, sealed, and protected from light below 4 °C. Shelf life is 2 months. 5.18 Syringe filter. the filter membrane is 0.22 μm polyvinylidene fluoride, polypropylene or polytetrafluoroethylene. Esters were spiked at 5.00 μg/L and 50.0 μg/L, and dibutyl phthalate and bis(2-ethylhexyl) phthalate were spiked at The 50.0 μg/L surface water and seawater spiked samples were determined repeatedly for 6 times. the relative standard deviations of the surface water spiked samples in the laboratory were 2.0%-16% and 2.3%-15%; the relative standard deviations in the laboratory of seawater spiked samples were 2.8%-13% and 1.3%-13%, respectively. 6 laboratories Dimethyl terephthalate, diethyl phthalate, butyl benzyl phthalate, di-n-octyl phthalate Esters were spiked at 5.00 μg/L and 80.0 μg/L, and dibutyl phthalate and bis(2-ethylhexyl) phthalate were spiked at 80.0 μg/L of domestic sewage and industrial wastewater spiked samples were determined 6 times repeatedly. the relative standard deviation in the laboratory of the domestic sewage spiked sample. The differences are 3.4%-14% and 1.3%-14%, respectively; the relative standard deviations in the laboratory of industrial wastewater spiked samples are 2.6%-15% and 2.6%, respectively. 2.0% to 15%. 10.1.2 n-hexane extraction The 6 laboratories spiked dibutyl phthalate at concentrations of 1.60 μg/L, 3.20 μg/L, 4.80 μg/L and dibutyl phthalate, respectively. (2-Ethylhexyl)ester spiked at 1.60 μg/L, 4.80 μg/L, 8.00 μg/L uniform blank spiked samples were determined in 6 replicates. The intra-laboratory relative standard deviations were 6.4%-13%, 2.8%-7.1%, and 2.5%-5.8%; the inter-laboratory relative standard deviations were 8.8%～9.1%, 5.7%～6.5% and 5.3%～6.4%; the repeatability limits are 0.4 μg/L, 0.5 μg/L～0.7 μg/L and 0.5 μg/L～ 0.8 μg/L; the reproducibility limits were 0.6 μg/L, 0.7 μg/L～1.1 μg/L, and 0.9 μg/L～1.6 μg/L, respectively. Six laboratories spiked dibutyl phthalate at 1.60 μg/L, 4.00 μg/L, and bis(2-ethylhexyl) phthalate, respectively Surface water and groundwater spiked samples with ester spiked concentrations of 1.60 μg/L and 8.00 μg/L were determined in 6 replicates. The relative standard deviations in the laboratory are 2.9% to 15% and 3.0% to 15%, respectively; the relative standard deviations of the groundwater spiked samples in the laboratory are 5.2% to 16% and 3.0% to 9.9%. See Appendix B for precision results statistics. 10.2 Correctness 10.2.1 Acetonitrile extraction 6 laboratories are dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate, n-Octyl ester spiked at 4.00 μg/L, 40.0 μg/L, 120 μg/L and dibutyl phthalate, bis(2-ethylhexyl) phthalate Uniform blank spiked samples with ester spiked concentrations of 40.0 μg/L, 80.0 μg/L, and 120 μg/L were determined in 6 replicates. the spiked recoveries ranged from The perimeters were 84%-128%, 85%-110%, and 86%-110%, respectively, and the final values of the spiked recoveries were 95%±17%-110%±23%, respectively. 94%±18%～104%±12%, 92%±8%～102%±11%. 6 laboratories are dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate, n-Octyl ester spiked at 5.00 μg/L, 50.0 μg/L and dibutyl phthalate, bis(2-ethylhexyl) phthalate spiked The spiked samples of surface water and seawater with a concentration of 50.0 μg/L were repeatedly determined for 6 times. the recovery rate of the spiked samples of surface water in the laboratory was within the range of 83% to 125% and 81% to 114%, respectively; the recovery rates of the spiked seawater samples in the laboratory ranged from 78% to 119% and 78% to 119%, respectively. 83%～114%; Dimethyl terephthalate, diethyl phthalate, butyl benzyl phthalate, di-n-octyl phthalate Ester spiked at 5.00 μg/L, 80.0 μg/L and dibutyl phthalate, bis(2-ethylhexyl) phthalate spiked at 80.0 μg/L of domestic sewage and industrial wastewater spiked samples were determined in 6 replicates. domestic sewage spiked samples were spiked and recovered in the laboratory The recovery rates ranged from 73% to 121% and 86% to 112%, respectively; the spiked recovery rates of industrial wastewater spiked samples in the laboratory ranged from 79% to 112%, respectively. 111% and 82% to 112%. 10.2.2 n-hexane extraction The 6 laboratories spiked dibutyl phthalate at concentrations of 1.60 μg/L, 3.20 μg/L and 4.80 μg/L and dibutyl phthalate, respectively. (2-ethylhexyl)ester spiked at 1.60 μg/L, 4.80 μg/L and 8.00 μg/L uniform blank spiked samples were tested in 6 replicates Determination. The recovery rates of standard additions ranged from 90% to 122%, 92% to 109%, and 91% to 105%, respectively. The final values of the standard addition recoveries were 103%±19%～108%±19%, 99%±13%～100%±12%, 98%±11%～98%±13%. Six laboratories spiked dibutyl phthalate at 1.60 μg/L, 4.00 μg/L, and bis(2-ethylhexyl) phthalate, respectively Surface water and groundwater spiked samples with ester spiked concentrations of 1.60 μg/L and 8.00 μg/L were determined in 6 replicates. Surface water spiked samples The recovery rates of standard addition in the laboratory ranged from 85% to 116% and 85% to 129%, respectively; respectively 77% to 122% and 75% to 130%. Please refer to Appendix B for the statistics of accuracy results. 11 Quality Assurance and Quality Control 11.1 Blank Analysis Every 20 samples or every batch (less than 20 samples/batch), at least 1 laboratory blank and full procedure blank sample shall be determined. The results should be below the method detection limit. 11.2 Calibration A standard curve should be established for each batch of samples, and the linear correlation coefficient should be greater than or equal to 0.995, otherwise the standard curve should be re-established. Every 20 samples or every batch (less than 20 samples/batch) should measure 1 standard solution at the middle concentration point of the standard curve. The relative error between the result and the concentration at this point should be within ±20%, otherwise the standard curve should be re-established. 11.3 Parallel samples Every 20 samples or every batch (less than 20 samples/batch), at least 1 parallel sample is determined, when the determination result is greater than or equal to the lower limit of determination , the relative deviation of the parallel double-sample determination results should be within ±30%. 11.4 Matrix spikes At least 1 matrix spike was measured every 20 samples or every batch (less than 20 samples/batch). The recovery rate of the matrix spike should be 70%~ between 130%. 12 Waste Disposal The waste generated during the experiment should be collected by classification, stored in a centralized manner, and marked accordingly, and the qualified units should be entrusted for disposal according to law. 13 Notes 13.1 There is background interference in the determination of phthalates, so samples should be collected and stored during sample analysis. Be careful to avoid contact or use of plastic products throughout. 13.2 The liquid chromatography should install a trapping column or modify the liquid chromatography system to avoid phthalates in the liquid chromatography system interference. 13.3 More than 20% isopropanol should be added to the needle washing solution of the injection needle to eliminate the residue of the injection needle after the high concentration sample is tested. 13.4 The sampling bottle is soaked with potassium dichromate lotion for 3 to 5 times, and then rinsed with tap water and distilled water respectively, and then the glass bottle is blown dry. Seal it with a plug or aluminum foil, wash it 3 to 5 times with the corresponding extraction solvent before sampling, and use it immediately after washing and drying. used during the experiment The experimental materials and glassware were cleaned 3 to 5 times with the corresponding extraction solvent before use, and used immediately after cleaning. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 1242-2022_English be delivered?Answer: Upon your order, we will start to translate HJ 1242-2022_English as soon as possible, and keep you informed of the progress. The lead time is typically 3 ~ 5 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of HJ 1242-2022_English with my colleagues?Answer: Yes. 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