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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 642-2013: Soil and sediment. Determination of volatile organic compounds-Headspace-gas chromatography/mass method Status: Valid
Basic dataStandard ID: HJ 642-2013 (HJ642-2013)Description (Translated English): Soil and sediment. Determination of volatile organic compounds-Headspace-gas chromatography/mass method Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z13 Classification of International Standard: 13.080 Word Count Estimation: 19,168 Quoted Standard: GB 17378.3; GB 17378.5; HJ 613; HJ/T 166 Regulation (derived from): ?Ministry of Environmental Protection Announcement 2013 No. 6 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the headspace measurement of volatile organic compounds in soil and sediment in/gas chromatography-mass spectrometry. This standard applies to 36 kinds of soil and sediment determination of volatile organic compounds. If validated, HJ 642-2013: Soil and sediment. Determination of volatile organic compounds-Headspace-gas chromatography/mass method---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 volatile organic compounds-Headspace-gas chromatography/mass method National Environmental Protection Standard of the People's Republic Determination of volatile organic compounds in soils and sediments Headspace/gas chromatography-mass spectrometry Soil and sediment-Determination of volatile organic compounds- Headspace-gas chromatography/mass method Published on.2013-01-21 2013-07-01 Implementation Ministry of Environmental Protection released ContentForeword. II Warning..1 1 Scope..1 2 Normative references..1 3 Terms and Definitions.1 4 principle of the method..2 5 reagents and materials. 2 6 instruments and equipment.3 7 samples.3 8 Analysis steps..4 9 Results calculation and representation..7 10 precision and accuracy..8 11 Quality Assurance and Quality Control 9 12 Waste treatment 10 13 Notes 10 The detection limit and lower limit of determination of Appendix A (normative appendix) method 11 Appendix B (informative) Determination of target compounds. Reference parameters. 12 Appendix C (informative) method of precision and accuracy. 14ForewordTo implement the Environmental Protection Law of the People's Republic of China, protect the environment, protect human health, and regulate soil and sediment This standard is developed for the determination of volatile organic compounds. This standard specifies headspace/gas chromatography-mass spectrometry for the determination of volatile organic compounds in soils and sediments. This standard is the first release. Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Anshan Environmental Monitoring Center Station, Environmental Protection Institute of the Ministry of Environmental Protection. This standard is verified by. Liaoning Provincial Environmental Monitoring Experimental Center, Shenyang Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Harbin Environmental Monitoring Center Station, Fushun Environmental Monitoring Center Station and Liaoyang Environmental Monitoring Center Station. This standard was approved by the Ministry of Environmental Protection on January 21,.2013. This standard has been implemented since July 1,.2013. This standard is explained by the Ministry of Environmental Protection. Determination of volatile organic compounds in soils and sediments Headspace/gas chromatography-mass spectrometry Warning. The internal standard, substitute and standard solution used in the test are volatile toxic compounds, and the solution preparation process should be Operate in a fume hood; wear protective gear as required to avoid contact with skin and clothing.1 Scope of applicationThis standard specifies headspace/gas chromatography-mass spectrometry for the determination of volatile organic compounds in soils and sediments. This standard applies to the determination of 36 volatile organic compounds in soils and sediments. If verified, this standard can also be adapted Used for the determination of other volatile organic compounds. When the sample amount is 2g, the detection limit of 36 targets is 0.8~4μg/kg, and the lower limit is 3.2~14μg/kg. See Appendix A for details.2 Normative referencesThe contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate. Used in this standard. GB 17378.3 Marine monitoring specification Part 3 Sample collection, storage and transportation GB 17378.5 Marine monitoring specification Part 5 Sediment analysis HJ 613 Determination of dry matter and moisture in soils - Gravimetric method HJ/T 166 Technical Specifications for Soil Environmental Monitoring3 Terms and definitionsThe following terms and definitions apply to this standard. 3.1 Internal standard Refers to a substance that is not contained in the sample but has similar physicochemical properties to the target to be tested. Usually added before sample analysis In, for the quantification of the target. 3.2 Surrogate Refers to a substance that is not contained in the sample but has similar physicochemical properties to the target to be tested. Generally in sample extraction or other Before the pretreatment, the recovery rate can be used to evaluate the influence of the sample matrix and the sample processing process on the analysis results. 3.3 Matrix spiked spike It means that a known amount of the target to be tested is added to the sample for evaluating the recovery rate of the target and the matrix effect of the sample. 3.4 Calibration verification standards Refers to a standard solution with a concentration near the midpoint of the calibration curve to confirm the validity of the calibration curve. 3.5 Transport blank strip blank 10 ml matrix modifier and 2.0g quartz sand were placed in the headspace bottle for sealing before sampling, and brought to the sampling field. The sample is not opened when it is sampled, and then shipped back to the laboratory with the sample, and the experiment is performed in the same analysis step as the sample for inspection. Whether the sample is contaminated during transportation. 3.6 Full program blank whole program blank 10 ml matrix modifier and 2.0g quartz sand were placed in the headspace bottle for sealing before sampling, and brought to the sampling field. Simultaneously open and seal the sample vial, then transport it back to the laboratory with the sample, and follow the same analysis steps as the sample. An experiment is performed to check whether the entire process from sample collection to analysis is contaminated.4 Principle of the methodUnder certain temperature conditions, the volatile components in the sample in the headspace bottle volatilize into the liquid space to generate vapor pressure. The liquid-solid three-phase reaches the thermodynamic dynamic equilibrium. The volatile organic compounds in the gas phase are separated by gas chromatography and then mass spectrometer Detection. Qualitative by comparison with standard material retention times and mass spectra, quantified by internal standard method.5 reagents and materials5.1 Experimental water. double distilled water or water prepared by pure water equipment. A blank test is required before use to confirm the target There is no interference peak in the retention time interval of the object or the concentration of the target therein is lower than the detection limit of the method. 5.2 Methanol (CH3OH). Chromatographic grade, pass the test before use to confirm the concentration of target compound or target compound Below the method detection limit. 5.3 Sodium chloride (NaCl). excellent grade pure After burning at 400 ° C for 4 h in a muffle furnace, it was placed in a desiccator and cooled to room temperature, and transferred to a ground glass bottle for storage. 5.4 Phosphoric acid (H3PO4)). excellent grade pure. 5.5 Matrix modifier Measure 500ml of experimental water (5.1), add a few drops of phosphoric acid (5.4) to adjust pH ≤ 2, add 180g of sodium chloride (5.3), Dissolve and mix. Store at 4 ° C for 6 months. 5.6 Standard stock solution. ρ=1000 mg/L～5000 mg/L Standard certified solutions can be purchased directly or in standard materials. 5.7 Standard use solution. ρ=10 mg/L～100 mg/L. Volatile targets such as dichloromethane, trans-1,2-dichloroethylene, 1,2-dichloroethane, cis-1,2-dichloroethylene and chloroacetate Standard intermediates such as olefins must be prepared separately, and the storage period is usually one week. The standard use solution of other targets is stored in compact. The shelf life is one month or prepared according to the manufacturer's instructions. 5.8 Internal standard solution. ρ=250 mg/L Fluorobenzene, chlorobenzene-d5 and 1,4-dichlorobenzene-d4 were selected as internal standards. A certified standard solution can be purchased directly. 5.9 Alternative standard solution. ρ=250 mg/L Toluene-d8 and 4-bromofluorobenzene were used as substitutes. A certified standard solution can be purchased directly. 5.10 4-bromofluorobenzene (BFB) solution. ρ=25 mg/L The certified standard solution can be purchased directly or can be prepared with a high concentration standard solution. 5.11 Quartz sand. 20~50 mesh. Before use, it is necessary to pass the test to confirm that the concentration of the target compound or target compound is lower than the method. The detection limit. 5.12 Carrier gas. high purity helium, ≥99.999%, deoxidized by deoxidizer, dehydrated by molecular sieve. Note 1. All the above standard solutions are treated with methanol as the solvent. The standard solution after preparation or unsealing should be placed in a compact bottle, and protected from light under 4 °C. Save, the shelf life is generally 30d. Recover to room temperature and mix before use.6 Instruments and equipment6.1 Gas Chromatograph. Capillary split/splitless inlet for temperature programming. 6.2 Mass Spectrometer. 70eV Electron Impact (EI) Ionization Source with NIST Mass Spectrometry Library, Manual/Automatic Tuning, Data Collection, quantitative analysis and library search functions. 6.3 Capillary column. 60 m × 0.25 mm; film thickness 1.4 μm (6 % nitrile propylphenyl, 94% dimethylpolysiloxane fixative), Other equivalent capillary columns can also be used. 6.4 Headspace Sampler. with headspace bottle, gasket (PTFE/silicone or Teflon/butyl rubber), cap (snail) Screw cap or gland used at one time). 6.5 Reciprocating Oscillator. The oscillation frequency is 150 times/min to fix the headspace bottle. 6.6 Ultrapure water preparation instrument or sub-boiling distiller. 6.7 Balance. Balance with an accuracy of 0.01g. 6.8 Microinjectors. 5 μl, 10 μl, 25 μl, 100 μl, 500 μl, 1000 μl. 6.9 Sampling equipment. shovel and stainless steel medicine spoon. 6.10 Portable refrigerator. 20L volume, temperature below 4 °C. 6.11 Brown compact bottle. 2 ml with Teflon liner and solid screw cap. 6.12 Sampling bottle. 60 ml threaded brown wide-mouth glass bottle with Teflon-silica liner screw cap. 6.13 Disposable Pasteur glass pipettes. 6.14 Common instruments and equipment used in general laboratories.7 samples7.1 Sample collection and preservation 7.1.1 Sample Collection Soil samples were collected and stored in accordance with the relevant regulations of HJ/T 166. In accordance with the relevant provisions of GB 17378.3 Collection and storage of sediment samples. The tool for collecting samples should be applied to metal products and should be purified before use. Can be taken Samples were screened at a high concentration and low concentration using a portable instrument for the determination of volatile organic compounds. All samples should be Collect at least 3 parallel samples. Use a shovel or a medicine spoon to collect the sample into the vial (6.12) as soon as possible and fill it as much as possible. Quickly remove sample vial The sample adhered to the grain and the outer surface, and the sample bottle is sealed. Put it in a portable freezer and bring it back to the lab. Note 2. When the concentration of volatile organic compounds in the sample is greater than 1000 μg/kg, the sample is regarded as a high content sample. Note 3. Do not stir the soil and sediment during sample collection to avoid evaporation of organic matter in soil and sediment. 7.1.2 Sample storage Samples should be analyzed as soon as they are sent to the laboratory. If it cannot be analyzed immediately, it should be sealed and stored below 4 °C, and the shelf life is not exceeded. After 7 days. The sample storage area should be free of organic interference. 7.2 Preparation of samples 7.2.1 Low content sample Remove the sample vial from the laboratory. After returning to room temperature, weigh 2g of the sample into the headspace bottle and quickly move it into the top empty bottle. Add 10ml matrix modifier (5.5), 1.0μl substitute (5.9) and 2.0μl internal standard (5.8), immediately seal and oscillate The oscillation on the device was oscillated at a frequency of 150 times/min for 10 min, to be tested. 7.2.2 High content sample If the preliminary screening of volatile organic compounds at the site is high or low, the determination result is greater than 1000μg/kg. High content sample. High-content samples were prepared as follows, and the vials for high-content sample testing were removed and allowed to return to room temperature. Weigh 2g of sample into the headspace bottle, quickly add 10 ml of methanol (5.2), seal, and shake on the shaker at 150 times/min The frequency oscillates for 10 min. After standing to settle, remove about 1 ml of extract with a disposable Pasteur glass pipette to 2 ml. In a brown glass bottle, the extract can be centrifuged if necessary. The extract can be stored in a refrigerator at 4 ° C, guaranteed The deposit period is 14 days. After returning the extract to room temperature before analysis, add 2 g of quartz sand (5.11), 10 ml of matrix to an empty headspace vial. Modifier (5.5) and 10 to 100 μl methanol extract. Add 2.0 μl of internal standard (5.8) and substitute (5.9) and seal immediately. Oscillation on the oscillator was oscillated at a frequency of 150 times/min for 10 min, to be tested. Note 4. If the concentration of the target compound in the methanol extract is high, it can be appropriately diluted by adding methanol. Note 5. If the concentration value is too low or not detected by the high content method, the sample should be re-analyzed using the low content method. 7.3 Preparation of blank samples 7.3.1 Low content blank sample Replace the sample with 2g quartz sand and prepare a low content blank sample according to the procedure of 7.2.1. 7.3.2 High content blank sample Replace the high-content sample with 2g quartz sand (5.11) and prepare a high-content blank sample according to the procedure in 7.2.2. 7.4 Determination of moisture The moisture content of the soil sample is determined according to HJ 613, and the moisture content of the sediment sample is determined according to GB 17378.5. Row.8 Analysis steps8.1 Instrument Reference Conditions Different working conditions of different models of headspace sampler, gas chromatograph and mass spectrometer should be different according to the instructions of the instrument. The book is operated. The recommended reference conditions for this standard are as follows. 8.1.1 Headspace Sampler Reference Conditions Heating equilibrium temperature 60~85 °C; heating equilibrium time 50 min; sampling needle temperature 100 ° C; transmission line temperature 110 ° C; The transfer line is deactivated and has a quartz capillary column with an inner diameter of 0.32 mm; the pressure equalization time is 1 min; when injecting 0.2 min; needle setting time 0.4 min; headspace bottle pressure 23 psi. 8.1.2 Gas Chromatograph Reference Conditions Temperature programmed. 40 ° C (for 2 min) 8 ° C/min 90 ° C (for 4 min) 6 ° C/min.200 ° C (guarantee Hold 15 min). Inlet temperature. 250 °C. Interface temperature. 230 °C. Carrier gas. helium; inlet pressure. 18 psi. Injection method. Split injection, split ratio. 5.1. 8.1.3 Mass Spectrometer Reference Conditions Scanning range. 35 amu~300 amu. Scan speed. 1 sec/scan. Ionization energy. 70 eV. Ion source temperature. 230 °C. Quadrupole temperature. 150 °C. Scan mode. full scan (SCAN) or selective ion (SIM) scan. 8.2 Calibration 8.2.1 Instrument performance check The GC/MS system must perform an instrument performance check before daily analysis. Pipette 2μl of BFB solution (5.10) Direct injection through the GC inlet and analysis by GC/MS. The critical ion abundance of BFB obtained by GC/MS system should be Meet the criteria specified in Table 1, otherwise some parameters of the mass spectrometer need to be adjusted or the ion source cleaned. Table 1 4-bromofluorobenzene ion abundance standard Mass-to-charge ratio ion abundance standard mass-to-charge ratio abundance standard 95 base peak, 100% relative abundance 175 mass 174 5% to 9% 96% 95% 5% to 9% 176 Quality 95% to 105% 174 173 is less than 25% of mass 174 177 is 5% to 10% of mass 176 174 is greater than 50% of mass 95 8.2.2 Drawing of the calibration curve Add 2 g of quartz sand (5.11), 10 ml of matrix modifier (5.5) to the 5 top empty bottles, and then divide into each bottle. Do not add a certain amount of standard use solution (5.7), the target compound concentration is 5, 10, 20, 50, 100μg/L; Add a certain amount of substitute (5.9) to each headspace bottle, and add 2.0μl of internal standard solution (5.8), immediately seal. The concentration of the calibration series is shown in Table 2. The configured standard series sample is oscillated on the oscillator at a frequency of 150 times/min Oscillate for 10 min, analyze the samples from low to high concentrations, draw a calibration curve or calculate the average response factor. In this standard The standard total ion chromatogram of 36 volatile organic compounds was determined by standard conditions, as shown in Figure 1. Table 2 Calibration Series Concentration Calibration series concentration (μg/L) Substitute concentration (μg/L) Internal standard concentration (μg/L) 1-chloroethylene; 2-1,1-dichloroethylene; 3-dichloromethane; 4-trans-1,2-dichloroethylene; 5-1,2-dichloroethane; 6-cis-1, 2-dichloroethylene; 7- Chloroform; 8-1,1,1-trichloroethane; 9-carbon tetrachloride; 10-1,2-dichloroethanebenzene; 11-fluorobenzene (internal standard 1); 12-trichloroethylene; 13-1,2- Dichloropropane; 14-bromodichloromethane; 15-toluene-d8 (alternative 1); 16-toluene; 17-1,1,2-trichloroethane; 18-tetrachloroethylene; 19-two Bromochloromethane; 20-1,2-dibromoethane; 21-chlorobenzene-d5 (internal standard 2); 22-chlorobenzene; 23-1,1,1,2-tetrachloroethane; 24- Ethylbenzene; 25-room- Xylene p-xylene; 26-o-xylene styrene; 27-bromoform; 28-4-bromofluorobenzene (substitute 2); 29-1,1,2,2-tetrachloroethane; 30-1,2,3-trichloropropane; 31-1,3,5-trimethylbenzene; 32-1,2,4-trimethylbenzene; 33-1,3-dichlorobenzene; 34-1,4-dichlorobenzene-d4 (internal standard 3); 35-1,4-dichlorobenzene; 36-1,2-dichlorobenzene; 37-1 , 2,4-trichlorobenzene; 38-six Chloroprene. Figure 1 36 kinds of volatile organic compounds standard total ion flow diagram 8.2.2.1 Establishing a calibration curve with an average relative response factor The relative response factor (RRFi) of the target (or surrogate) in point i of the standard series, calculated according to formula (1) Count. ISi ISi i A ARRF ρ ρ×= (1) In the formula. The relative response factor of the i-th target (or surrogate) in the RRFi-standard series; The response value of the quantified ion of the i-th target (or substitute) in the Ai-standard series; The i-th point in the AISi-standard series corresponds to the target (or substitute) corresponding to the internal standard quantitation ion response value; The concentration of the internal standard in the ρIS-standard series, 50 μg/L; The mass concentration of the i-th target (or substitute) in the ρi-standard series, μg/L. The average relative response factor RRF of the target (or substitute) is calculated ac......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 642-2013_English be delivered?Answer: Upon your order, we will start to translate HJ 642-2013_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 642-2013_English with my colleagues?Answer: Yes. The purchased PDF of HJ 642-2013_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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