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Delivery: <= 5 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 643-2013: Solid waste. Determination of volatile organic compounds. Headspace-gas chromatography/mass method Status: Valid
Basic dataStandard ID: HJ 643-2013 (HJ643-2013)Description (Translated English): Solid waste. 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: 13.030.10 Word Count Estimation: 25,211 Quoted Standard: HJ/T 20; HJ/T 299; HJ/T 300 Regulation (derived from): ?Ministry of Environmental Protection Announcement 2013 No. 6 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the determination of volatile organic compounds in solid waste headspace/gas chromatography-mass spectrometry. This standard is applicable to solid waste solid waste leachate in 36 kinds of measurement and volatile organic compound HJ 643-2013: Solid waste. 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. Solid waste.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 solid waste Headspace/gas chromatography-mass spectrometry Solid waste -Determination of volatile organic compounds- Headspace-gas chromatography/mass method Published on.2013-01-21 2013-07-01 Implementation release Ministry of Environmental Protection ContentForeword. II 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..9 11 Quality Assurance and Quality Control 9 12 Waste treatment 11 13 Notes 11 Appendix A (informative) target detection limit and lower limit of measurement 12 Appendix B (informative) Determination of target compounds. Reference parameters. 15 Appendix C (informative) method of precision and accuracy. 17ForewordTo implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Environmental Pollution by Solid Waste This standard is formulated to protect the environment, protect human health, and regulate the determination of volatile organic compounds in solid waste. This standard specifies headspace/gas chromatography-mass spectrometry for the determination of volatile organic compounds in solid waste. 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 solid wastes by headspace/gas chromatography-mass spectrometry Warning. The internal standard, substitute and standard solution used in the test are volatile toxic compounds. The preparation process should be Operation in the fume hood; the sample preparation process should fully consider whether it is toxic or hazardous solid waste; Wear protective gear 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 solid waste. This standard applies to the determination of 36 volatile organic compounds in solid waste and solid waste leachate. If you pass the verification The standard is also applicable to the determination of other volatile organic compounds. When the amount of solid waste sample is 2 g, the detection limit of 36 target compounds is 0.8 μg/kg~4 μg/kg. Limit 4 μg/kg ~15 μg/kg. When the volume of solid waste leachate is 10 ml, the detection limit of 36 target compounds is 0.1. Gg/L~0.3 μg/L, the lower limit of measurement is 0.4 μg/L~2 μg/L. 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. HJ/T 20 Technical Specifications for Sampling and Sample Preparation of Industrial Solid Waste HJ/T 299 solid waste leaching toxicity leaching method sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity leaching method acetic acid buffer solution method3 Terms and definitionsThe following terms and definitions apply to this standard. 3.1 internal standards 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 standards 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 Refers to the addition of a known amount of the target to be tested to the sample. It is used to evaluate the recovery 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 Shipping Blank Trip Blank 10 ml matrix modifier and 2.0 g quartz sand were placed in the headspace bottle for sealing before sampling, taking them to the sample on site. When the sample is not opened, it will be shipped back to the laboratory with the sample, and the experiment will be carried out according to the same analysis steps as the sample. Check if the sample is contaminated during transportation. 3.6 full program blank whole program blank 10 ml matrix modifier and 2.0 g quartz sand were placed in the headspace bottle for sealing before sampling, taking them to the sample on site. Simultaneously open and seal with the sample vial, then transport it back to the laboratory with the sample, following the same analytical 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 materialsUnless otherwise stated, chromatographically pure reagents that meet national standards were used for the analysis. 5.1 Experimental water. double distilled water or water prepared by pure water equipment. Need to pass the blank test before use, confirm No interference peaks appeared in the retention time interval of the target compound or the target concentration therein was below the method detection limit. 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 In a muffle furnace (or box furnace), burn at 400 °C for 4h, place in a desiccator and cool to room temperature, transfer to the ground glass Store in a glass bottle. 5.4 Phosphoric acid (H3PO4)). excellent grade pure. 5.5 Glacial acetic acid (CH3COOH). excellent grade pure. 5.6 Sodium hydroxide (NaOH). excellent grade. 5.7 sodium hydroxide solution. c (NaOH) = 1 mol/L Weigh 40 g of sodium hydroxide (5.6), add to the beaker, and add a small amount of experimental water (5.1) to dissolve it. Transfer to a 1 L volumetric flask and bring up to volume. 5.8 Extractant 5.8.1 Extracting agent 1. Measure 5.7 ml of glacial acetic acid to 500 ml of experimental water (5.1), add 64.3 ml of sodium hydroxide solution (5.7), dilute to 1L with water. The pH of the solution after preparation should be 4.93 ± 0.05. 5.8.2 Leaching agent 2. Experimental water (5.1). 5.9 Matrix modifier Measure 500 ml of experimental water (5.1), add a few drops of phosphoric acid (5.4) to adjust pH ≤ 2, add 180 g of sodium chloride (5.3), Dissolve and mix. Store at 4 °C for 6 months. 5.10 Standard stock solution. ρ=1000 mg/L～5000 mg/L Standard certified solutions can be purchased directly or in standard materials. 5.11 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. 5.12 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. 5.13 Alternative standard solution. ρ=250 mg/L Toluene-d8 and 4-bromofluorobenzene were used as substitutes. A certified standard solution can be purchased directly. 5.14 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. 5.15 Quartz sand. 20 mesh ~ 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 Method detection limit. 5.16 Carrier gas. high-purity helium (≥99.999%), deoxidized by deoxidizer and 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. Electron Bombardment (EI) Ionization Source with 70 eV, NIST Mass Spectrometry Library, Manual/Automatic Tuning, Number According to acquisition, quantitative analysis and library search and other functions. 6.3 Capillary column. 60 m × 0.25 mm × 1.4 μm (6 % nitrile propyl, 94 % dimethylpolysiloxane fixative), Other equivalent capillary columns can also be used. 6.4 Headspace Sampler. with headspace bottle, gasket (PTFE/silicone or PTFE/butyl rubber), cap (screw cap or gland used at one time). 6.5 Zero-Headspace Extraction Vessel. 500-600 ml for leaching in the sample Hairy substance. 6.6 flip-type oscillator. speed is 30±2 r/min 6.7 Reciprocating Oscillator. The oscillation frequency is 150 times/min to fix the headspace bottle. 6.8 Ultrapure water preparation instrument or sub-boiling distiller. 6.9 pH meter. Accuracy is ±0.05. 6.10 Balance. Balance with an accuracy of 0.01 g. 6.11 Microinjectors. 5 μl, 10 μl, 25 μl, 100 μl, 500 μl, 1000 μl. 6.12 Brown compact bottle. 2 ml with Teflon liner and solid screw cap. 6.13 Disposable Pasteur glass pipettes. 6.14 Sampling bottle. 60 ml or 250 ml, threaded brown glass bottle with Teflon septa. 6.15 Sampling equipment. shovel and stainless steel medicine spoon. 6.16 Portable refrigerator. 20 L in volume and 4 °C below temperature. 6.17 Common instruments and equipment used in general laboratories.7 samples7.1 Sample collection and preservation Collect and store solid waste samples in accordance with HJ/T 20 regulations. Tool for collecting samples applied to metal The product should be purified before use. Samples can be taken at the sampling site using portable instruments for volatile organic determination Primary screening with high and low concentration. At least 3 parallel samples should be collected for all 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 considered to be a high content sample. Note 3. Do not stir solid waste during sample collection to avoid volatilization of organic matter in solid waste. Sampling personnel must do a good job Work. 7.1.2 Preservation of samples 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 More than 14 days. The sample storage area should be free of organic interference. 7.2 Preparation of samples 7.2.1 Low-volume samples of solid waste 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 10 ml matrix modifier (5.9), 1.0 μl substitute (5.13) and 2.0 μl internal standard (5.12), immediately sealed, vibrating The oscillation on the vortex was oscillated at a frequency of 150 times/min for 10 min, to be tested. 7.2.2 High-volume samples of solid waste If the preliminary screening of volatile organic compounds at the site is high or low, the determination result is greater than 1000 μg/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 2 g of sample into a headspace bottle, quickly add 10 ml of methanol (5.2), seal, and 150 on the shaker (6.7) The frequency of the second/min is oscillated for 10 min. After standing to settle, remove about 1 ml of extract with a disposable Pasteur glass pipette. In a 2 ml brown glass bottle, the extract can be centrifuged if necessary. The extract can be stored in a refrigerator at 4 ° C. The shelf life is 14 days. After returning the extract to room temperature before analysis, add 2.0 g of quartz sand (5.15), 10 ml to an empty headspace vial. Matrix modifier (5.9) and 10 μl to 100 μl methanol extract. Add 2.0 μl of internal standard (5.12) and substitute (5.13), Immediately sealed and oscillated at 150 times/min on the oscillator (6.7) 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. 7.2.3 Solid waste leachate sample A solid waste leachate sample was prepared by leaching a method of performing HJ/T 299 or HJ/T 300. Take 10 ml of leachate and move in In the headspace vial, add 1.0 μl of the replacement (5.13) and 2.0 μl of the internal standard solution (5.12) and immediately seal and test. 7.3 Preparation of blank samples 7.3.1 Low-volume blank sample of solid waste Replace the sample with 2.0 g quartz sand (5.15) and prepare a low content blank sample according to the procedure of 7.2.1. 7.3.2 Solid waste high content blank sample Replace the high-content solid waste sample with 2.0 g quartz sand (5.15) and prepare a high-content blank sample according to the procedure in 7.2.2. 7.3.3 Blank sample of solid waste leachate According to the extraction method of HJ/T 299 or HJ/T 300, put the extractant (5.8) in the headspace bottle and add 1.0 μl Substance (5.13) and 2.0 μl internal standard use solution (5.12), immediately sealed and tested.8 Analysis steps8.1 Instrument Reference Conditions Different working conditions of different types of headspace preparation instrument, gas chromatograph and mass spectrometer are different, and should be in accordance with the instructions for use 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 °C ~ 85 °C; heating equilibrium time 50 min; sampling needle temperature 100 ° C; transmission line temperature 110 ° C, the transmission line is deactivated, quartz capillary column with an inner diameter of 0.32mm; pressure equilibrium time 1 min; The injection time was 0.2 min; the needle setting time was 0.4 min; the headspace bottle pressure was 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 (keep 15 min). Inlet temperature. 250 °C. Interface temperature. 230 °C. Carrier gas. helium; inlet pressure. 18 psi. Enter Sample mode. 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 2 μl 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 (1) Determination of the calibration curve of solid waste Add 2 g of quartz sand (5.15), 10 ml of matrix modifier (5.9) to the 5 top empty bottles, and then divide into each bottle. Do not add a certain amount of standard use solution (5.11), the concentration of volatile organic compounds is 5, 10, 20, 50, 100 μg/L; Add a substitute (5.13) to each headspace bottle and add 2.0 μl of the internal standard solution (5.12) to seal immediately. The concentration of the calibration series is shown in Table 2. The prepared standard series sample was oscillated on the oscillator (6.7) at a frequency of 150 times/min. For 10 min, analyze the samples from low to high concentrations, establish a calibration curve or calculate the average response factor. In this standard The standard total ion chromatogram of 36 volatile organic compounds was analyzed and determined under the specified 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; 10,11-1,2-dichloroethanebenzene; internal standard 1-fluorobenzene; 12-trichl......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 643-2013_English be delivered?Answer: Upon your order, we will start to translate HJ 643-2013_English as soon as possible, and keep you informed of the progress. 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