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Delivery: <= 6 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 1227-2021: Water quality - Emergency determination of volatile organic compounds - Portable headspace/gas chromatography-mass Status: Valid
Basic dataStandard ID: HJ 1227-2021 (HJ1227-2021)Description (Translated English): Water quality - Emergency determination of volatile organic compounds - Portable headspace/gas chromatography-mass Sector / Industry: Environmental Protection Industry Standard Word Count Estimation: 34,385 Issuing agency(ies): Ministry of Ecology and Environment HJ 1227-2021: Water quality - Emergency determination of volatile organic compounds - Portable headspace/gas chromatography-mass---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 Emergency determination of volatile organic compounds Portable headspace/gas chromatography-mass spectrometry) National Ecological Environment Standard of the People's Republic of China Emergency Determination of Volatile Organic Compounds in Water Quality Portable Headspace/Gas Chromatography-Mass Spectrometry Water quality-Emergency determination of volatile organic compounds -Portable headspace/gas chromatography-mass 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 2021-12-16 2022-03-01 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 Reagents and materials...1 5 Instruments and equipment...2 6 Preparation before monitoring...2 7 Samples...2 8 Analysis steps...3 9 Result calculation and representation...5 10 Accuracy...7 11 Quality Assurance and Quality Control...7 12 Waste Disposal...7 13 Precautions...8 Appendix A (Normative Appendix) Method Detection Limits and Lower Limits of Determination for Target Compounds...9 Appendix B (informative) Total ion chromatograms of target compounds...11 Appendix C (Informative Appendix) Quantitative ions and auxiliary ions of target compounds...13 Appendix D (Informative) Method Accuracy...15 Portable Headspace/Gas Chromatography-Mass Spectrometry for Emergency Determination of Volatile Organic Compounds in Water Quality Warning. When using this method, pay attention to the dangers of the accident site and the surrounding environment, and do a good job of personal protection. 1 Scope of applicationThe standard specifies a portable headspace/gas chromatography-mass spectrometry method for the determination of volatile organic compounds in water. This standard is applicable to 56 kinds of volatile toluene in surface water, groundwater, domestic sewage, industrial wastewater and seawater in sudden environmental events. On-site emergency determination of organic matter. This method can also be used for qualitative and concentration estimation of other volatile organic compounds. In full scan mode, when the sample volume in the headspace vial is 10.0 ml, the gas injection volume is 8 ml, splitless injection, or Method detection of 56 target compounds with a sample volume of 20.0 ml in an empty vial, a gas injection volume of 100 ml, and a split ratio of 40.1 The limit of determination is 1 μg/L～3 μg/L, and the lower limit of determination is 4 μg/L～12 μg/L, 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/T 32210 Portable gas chromatography-mass spectrometer technical requirements and test methods HJ 442.9 Technical Specifications for Environmental Monitoring in Offshore Sea Areas Part IX Emergency and Special Monitoring in Offshore Sea Areas HJ 589 Technical specification for emergency monitoring of environmental emergencies3 Principles of the methodUnder certain temperature conditions, the volatile organic compounds in the sample in the headspace sampling bottle volatilize to the headspace and are carried into the portable by the carrier gas. It is enriched in the built-in adsorption tube of the gas chromatography-mass spectrometer, enters the gas chromatography for separation after thermal desorption, and is detected by a mass spectrometer detector. Quasi-substance mass spectrum and retention time comparison qualitative, internal standard method for quantification; for substances other than 56 target compounds, by comparing with standard substances The mass spectrum is qualitative, and its concentration is estimated based on the ratio of its response to that of the internal standard.4 Reagents and MaterialsUnless otherwise specified, analytical reagents that meet national standards were used in the analysis. 4.1 Experimental water. double distilled water or water prepared by pure water equipment. Before use, a blank test should be carried out to confirm that there is no interference peak within the retention time of the target compound or the concentration of the target compound is lower than the formula. detection limit. 4.2 Ascorbic acid (C6H8O6). 4.3 Methanol (CH3OH). pure by liquid chromatography. 4.4 Hydrochloric acid. ρ=1.19 g/ml, excellent grade. 4.5 Hydrochloric acid solution. Hydrochloric acid (4.4) and water are mixed in a volume ratio of 1.1. 4.6 Standard stock solution of volatile organic compounds. ρ=2000 mg/L. Commercially available certified standard solution, stored in accordance with the instructions. 4.7 Standard solution for volatile organic compounds. ρ=100 mg/L. Dilute the standard stock solution of volatile organic compounds (4.6) with methanol (4.3), and store it for 30 d in the refrigerator below 4°C, protected from light and sealed. 4.8 Internal standard standard stock solution. ρ=2000 mg/L. Fluorobenzene and 1,4-dichlorobenzene-d4 were selected as internal standards. The certified standard solution can be purchased directly and stored according to the instructions. satisfying this Other internal standards may also be used as long as the method requires and does not interfere with the determination of the target compound. 4.9 Internal standard standard solution. ρ=100 mg/L. Dilute the internal standard standard stock solution (4.8) with methanol (4.3), and store it for 30 d if it is refrigerated below 4 °C and protected from light. 4.10 Internal standard standard gas. the components are 1,3,5-tris(trifluoromethyl)benzene (100 μmol/mol), bromopentafluorobenzene (50 μmol/mol) or 4-Bromofluorobenzene (20 μmol/mol), stored in a steel cylinder, can be stored for 1 year, or refer to the relevant instructions of the standard gas certificate. for instrument tuning Harmony. 4.11 Carrier gas. nitrogen or helium, purity ≥99.999%.5 Instruments and equipment5.1 Sampling bottle. 40 ml amber glass bottle with silicone rubber-teflon gasketed screw cap. 5.2 Portable gas chromatography-mass spectrometer. with adsorption thermal desorption module, gas chromatography module (with temperature program function), and quadrupole Rod or ion trap mass spectrometry modules. The mass spectrometry module has a 70 eV electron impact (EI) ion source with full scan/selected ion scan, auto/ Functions such as manual tuning, spectral library search and quantitative analysis should meet the requirements of GB/T 32210.All samples pass through the tubing and All joints should be inertized. 5.3 Portable headspace sampler. The heating temperature is controlled between room temperature and 80 °C, and the temperature control accuracy is ±1 °C. 5.4 Capillary column. 15 m×0.25 mm×1.0 m or 10 m×0.1 mm×0.4 m, the stationary phase is 100% dimethylpolysilicon oxane, other equivalent capillary columns can also be used. 5.5 Built-in adsorption tube. Fill with adsorbents such as Tenax, Carbopack, silica gel, or other equivalent adsorbents. 5.6 Headspace vial. Use the glass headspace vial that is fitted with the Portable Headspace Sampler (5.3), with a Teflon-coated seal. 5.7 Commonly used instruments and equipment.6 Preparation before monitoringCheck the working status of the portable gas chromatograph-mass spectrometer, and confirm that the carrier gas (4.11), internal standard gas (4.10), Volatile organic compound standard solution (4.7) and internal standard standard solution (4.9), batteries, sampling bottles (5.1) and personal protective equipment, etc. Necessary spare parts.7 samples7.1 Sample Collection Sample collection of surface water, groundwater, domestic sewage, industrial wastewater and seawater, according to the actual situation of pollutants entering the water environment, Follow the relevant provisions of HJ 589 and HJ 442.9.When collecting the sample, the water sample should be filled with the sampling bottle (5.1) without leaving any head space. Avoid generating a lot of air bubbles. After sample collection, analysis should be carried out as soon as possible on site, and the determination should be completed within 24 hours. 7.2 Preparation of blank samples Use experimental water (4.1) as a blank sample.8 Analysis steps8.1 Instrument Reference Conditions 8.1.1 Headspace Sampler Reference Conditions Condition 1.heating equilibrium temperature. 50 ℃; heating equilibration time. 10 min; sampling needle temperature. 50 ℃; transfer line temperature. 60 ℃; The sample volume in the headspace vial (5.6) is 10.0 ml, and the gas injection volume is 8 ml, splitless. Condition 2.heating equilibrium temperature. 50 ℃; heating equilibration time. 10 min; sampling needle temperature. 50 ℃; transfer line temperature. 60 ℃; The sample volume in the headspace vial (5.6) is 20.0 ml, the gas injection volume is 100 ml, and the split ratio is 40.1. Or set according to the instrument instruction manual. 8.1.2 Thermal desorption reference conditions Thermal desorption temperature. 300 °C, pre-desorption time of adsorption tube. 0.1 min, and desorption time of adsorption tube. 0.5 min. Or set according to the instrument instruction manual. 8.1.3 Gas chromatography reference conditions Condition 1.Column pressure. 80 kPa; temperature program. 60 °C for 1 min, 6 °C/min to 80 °C, and 12 °C/min to increase to 80 °C 118 °C, and finally increased to 180 °C at 28 °C/min and held for 18 s. Condition 2.Column flow. 0.2 ml/min; programmed temperature. 60 °C for 1 min, 20 °C/min to 80 °C, and then 40 °C/min Raised to 220 °C and held for 1 min. Or set according to the instrument instruction manual. 8.1.4 Reference conditions for mass spectrometry Ion source. EI; ionization energy. 70 eV; scanning mode. full scan; scanning range. 41 u～300 u. Or set according to the instrument instruction manual. Refer to Appendix B for the total ion chromatogram obtained by measuring the standard substance of the target compound under the reference conditions. Note. When the detection limit of the target compound does not meet the standard limit requirements, the ion scanning mode can be selected. 8.2 Calibration 8.2.1 Tuning After starting up, firstly check the instrument performance of the portable gas chromatograph-mass spectrometer (5.2) according to the instrument manual. to protect To verify the accuracy of the test results, after the startup, the mass spectrometer function should be tuned. device usage requirements. Every 12 hours, the mass spectrometer function should be retuned. If the tuning substance is 1,3,5-tris(trifluoromethyl)benzene and bromopentafluoro benzene, the abundance of key ions should meet the requirements of Table 1; if the tuning substance is perfluorotributylamine, the abundance of key ions should meet the requirements of Table 2. Otherwise, the parameters of the mass spectrometer should be adjusted; if other substances are used for tuning, the relevant requirements of the instrument manual should be met. Table 1 Abundance standards of key ions when 1,3,5-tris(trifluoromethyl)benzene and bromopentafluorobenzene are simultaneously tuned Mass-to-charge ratio (m/z) Ion abundance range Mass-to-charge ratio (m/z) Ion abundance range 50 0.5% to 2.5% of peak 117 50% to 70% of peak 167 117 55 2% to 5% of peak 117 213 10% to 20% of peak 117 69 8% to 16% of peak 117 246 15% to 40% of peak 117 93 15% to 25% of peak 117 263 5% to 15% of peak 117 117 Base peak, 100% relative abundance 282 5% to 15% of peak 117 Table 2 Key ion abundance requirements of perfluorotributylamine Mass-to-charge ratio (m/z) Ion abundance range Mass-to-charge ratio (m/z) Ion abundance range 69 base peak, 100% relative abundance 100 5% to 50% of 69 peak 131 20% to 70% of peak 69 264 5% to 50% of peak 69 8.2.2 Plotting the calibration curve 8.2.2.1 Prefabricated calibration curve Dilute the volatile organic compound standard solution (4.7) to prepare the target compound mass concentrations of 2.0 μg/L, 5.0 μg/L, 10.0 ml of standard series solutions of 10.0 μg/L, 20.0 μg/L, 40.0 μg/L (this concentration is the reference concentration). Then add 1.0 μl Use standard standard solution (4.9) to make the internal standard concentration in the sample 10.0 μg/L, immediately seal the headspace vial (5.6), mix well, and follow the instrument The reference conditions (8.1) are measured sequentially from low concentration to high concentration, and the calibration curve is drawn and stored in the instrument. At the emergency monitoring site, if If the calibration check meets the relevant requirements in 11.3, quantify using a pre-made calibration curve. 8.2.2.2 Field calibration At the emergency monitoring site, if the calibration check does not meet the relevant requirements in 11.3, the calibration should be redrawn with at least 2 non-zero concentration points. The standard curve, the target compound mass concentrations were 10.0 μg/L and 40.0 μg/L (this concentration is the reference concentration). 8.2.3 Average relative response factor method The relative response factor (RRFi) of a target compound at point i in the standard series is calculated according to formula (1). n--standard series points. 8.2.4 Calibration curve method Taking the concentration of the target compound as the abscissa, taking the ratio of the quantitative ion response value of the target compound to the quantitative ion response value of the internal standard compound The product of the concentration of the internal standard compound is taken as the ordinate, and a calibration curve is established. 8.3 Sample concentration prediction Before the sample is measured, the quick-check method, sample dilution or other methods specified in the instrument manual should be used, combined with the on-site investigation, to predict. Determine the sample concentration. 8.4 Determination of samples If the estimated concentration of the sample is lower than 40 μg/L, directly take 10.0 ml of the sample into the headspace vial (5.6), and quickly add 1.0 l Use the internal standard standard solution (4.9), immediately seal, mix well, and wait for the test. If the sample is predicted to have a higher concentration, dilute it with experimental water (4.1) to the concentration range analyzed by the method. Take another 10.0 ml of the diluted sample Quickly add 1.0 l Internal Standard Standard Solution (4.9) to the headspace vial (5.6), seal it immediately, mix well, and wait for measurement. Measure the sample according to the same operation steps and instrument conditions as the pre-made calibration curve (8.2.2.1). 8.5 Blank test Replace the sample with experimental water (4.1), and carry out the blank sample according to the same operation steps and instrument conditions as the sample determination (8.4). Determination.9 Result calculation and presentation9.1 Target compounds 9.1.1 Qualitative Analysis By comparing the retention time, mass-to-charge ratio of fragment ions and their abundance ratios of the target in the sample and the target in the standard series, the The target is characterized. The retention time of the target compound in the sample should be controlled within t±3S, where t is the concentration level of the initial calibration The average retention time of each target compound, S is the standard deviation of the retention time of each concentration level of the target compound in the initial calibration. target All ions with relative abundance higher than 30% in the standard mass spectrum of the compound should be present in the sample mass spectrum, and qualitatively combined with the on-site situation judge. If there is obvious background interference in the actual sample, the background influence should be subtracted from the comparison. 9.1.2 Quantitative analysis Quantitative calculations were performed using the calibration curve method or the average relative response factor method. When the quantitative ion of the target compound in the sample interferes, Auxiliary ions can be used for quantification. See Appendix C for quantitative ions and auxiliary ions. 9.1.3 Result calculation 9.1.3.1 Average Relative Response Factor Method When the average relative response factor method is used for calibration, the mass concentration ρx of the target compound in the sample is calculated according to formula (3). 9.2 Off-target compounds 9.2.1 Qualitative Analysis The measurement is performed in a full scan mode, and the mass spectrum of the sample is compared with the mass spectrum of the standard material in the library. The mass spectrum of the standard material in the library is relatively abundant. All ions with a degree higher than 30% should be present in the sample mass spectrum, the signal-to-noise ratio of the qualifier ions should be greater than 3.1, the main qualifier ion and the auxiliary The peaks of the ion peaks of the qualifier ions should be maximally co-elute in the same scan segment. According to the matching degree of mass spectrum and spectral library, combined with the actual situation on site The qualitative results of the samples were obtained by judging the condition. 9.2.2 Concentration estimation Integrate the chromatographic peaks of the total ion chromatogram of the qualitative target external compound and internal standard in the sample, and the mass concentration of the target external compound The degree ρx is estimated according to formula (5), and the internal standard adjacent to the retention time is selected as the quantitative internal standard. 9.3 Result representation The number of decimal places in the determination result is consistent with the detection limit of the method, and a maximum of 3 significant figures are reserved. For non-target compounds, the original information such as mass spectrum and search judgment results should be attached to the qualitative results. 10 Accuracy 10.1 Precision Six laboratories performed six replicates of 56 unified samples with VOC concentrations of 10.0 g/L, 100 µg/L, 500 g/L. Repeat determination. the relative standard deviations within laboratories were 1.8%-26%, 1.1%-24%, and 1.1%-24%; the relative standard deviations between laboratories were The differences are. 2.0%～15%, 6.1%～23%, 4.7%～17%; the repeatability limits are. 1.7 μg/L～4.2 μg/L, 12 μg/L～ 39 µg/L, 66 µg/L～187 µg/L; reproducibility limits are. 1.7 µg/L～5.3 µg/L, 28 µg/L～68 µg/L, 90 µg/L～ 300 µg/L. See Table D.1 in Appendix D for summary precision data. 10.2 Correctness Six laboratories performed six replicates of surface water samples spiked at 10.0 µg/L, 100 µg/L for 56 VOCs Determination. The recoveries of standard additions ranged from 89.8% to 114% and 91.7% to 105%, respectively. Six laboratories performed six replicates of industrial wastewater samples spiked at 50.0 µg/L and.200 µg/L for 56 volatile organic compounds. Repeat determination. The recovery rates of standard additions ranged from 82.8% to 112% and 91.0% to 105%, respectively. One laboratory carried out 6 repetitions of 56 volatile organic compounds spiked with 10.0 µg/L and 100 µg/L domestic sewage samples. Repeat determination. the recovery rates of......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 1227-2021_English be delivered?Answer: Upon your order, we will start to translate HJ 1227-2021_English as soon as possible, and keep you informed of the progress. The lead time is typically 4 ~ 6 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of HJ 1227-2021_English with my colleagues?Answer: Yes. 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