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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 605-2011: Soil and Sediment. Determination of Volatile Organic compounds. Purge and Trap Gas Chromatography/Mass Spectrometry Method Status: Valid
Basic dataStandard ID: HJ 605-2011 (HJ605-2011)Description (Translated English): Soil and Sediment. Determination of Volatile Organic compounds. Purge and Trap Gas Chromatography/Mass Spectrometry Method Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z18 Classification of International Standard: 13.080 Word Count Estimation: 22,237 Date of Issue: 2011-02-10 Date of Implementation: 2011-06-01 Quoted Standard: GB 17378.3; HJ/T 166 Regulation (derived from): Department of Environmental Protection Notice No. 9 of 2011 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the determination of volatile organic compounds in soils and sediments of the purge and trap/gas chromatography mass spectrometry. This standard applies to soils and sediments 65 kinds of volatile organic compounds measured. If the validation of this standard can be applied to the determination of volatile organic compounds other. HJ 605-2011: Soil and Sediment. Determination of Volatile Organic compounds. Purge and Trap Gas Chromatography/Mass Spectrometry 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.Purge and Trap Gas Chromatography/Mass Spectrometry Method National Environmental Protection Standard of the People's Republic Determination of volatile organic compounds in soils and sediments Purge and trap/gas chromatography-mass spectrometry Soil and sediment-Determination of volatile organic compounds -Purge and trap gas chromatography/mass spectrometry method Published on.2011-02-10 2011-06-01 Implementation Ministry of Environmental Protection released Ministry of Environmental Protection announcement No. 9 of.2011 In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and standardize environmental monitoring, the water is now approved. The determination of total mercury is determined by the Cold Atomic Absorption Spectrophotometry and other nine standards for national environmental protection standards. The standard name and number are as follows. I. Determination of total mercury in water - Cold atomic absorption spectrophotometric method (HJ 597-2011); 2. Determination of water quality ladders by sodium sulfite spectrophotometry (HJ 598-2011); 3. Determination of water quality ladders N-chlorohexadecylpyridine-sodium sulfite spectrophotometry (HJ 599-2011); 4. Gas chromatographic method (HJ 600-2011) for the determination of water quality ladders, black ropes, and dien ladders; 5. Determination of water quality of formaldehyde - Acetylacetone spectrophotometry (HJ 601-2011); 6. Determination of water quality 石墨 Graphite furnace atomic absorption spectrophotometry (HJ 602-2011); VII. Determination of water quality 火焰 Flame atomic absorption spectrophotometry (HJ 603-2011); VIII. Determination of total hydrocarbons in ambient air - Gas chromatography (HJ 604-2011); The above standards have been implemented since June 1,.2011 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection. From the date of implementation of the above standards, the following seven national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished. The name and number are as follows. 1. Determination of total mercury in water quality by cold atomic absorption spectrophotometry (GB 7468-87); 2. Determination of water quality ladders by sodium sulfite spectrophotometry (GB/T 13905-92); 3. Determination of water quality ladders by spectrophotometry (GB/T 13903-92); 4. Determination of water quality TNT, Hessian and Dien, gas chromatography (GB/T 13904-92); V. Determination of water quality formaldehyde acetylacetone spectrophotometry (GB 13197-91); VII. Determination of total hydrocarbons in ambient air Gas chromatography (GB/T 15263-94). Special announcement. February 10,.2011 ContentForeword..iv 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.2 7 samples.3 8 Analysis steps..4 9 Results calculation and representation..7 10 Precision and Accuracy 8 11 Quality Assurance and Quality Control.8 12 Notes 9 Appendix A (Normative Appendix) Detection limit, lower limit of measurement and minimum relative response factor of target 10 Appendix B (informative) Quantitative parameters of target 12 Appendix C (informative) The precision and accuracy of the method.14 IvForewordIn order to implement the Environmental Protection Law of the People's Republic of China, protect the environment, protect human health, and regulate the volatility of soil and sediment. This standard is established for the measurement method of the machine. This standard specifies the purge and trap/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. Dalian Environmental Monitoring Center. This standard is verified by. Liaoning Provincial Environmental Monitoring Experimental Center, Anshan Environmental Monitoring Center Station, Jiangsu Environmental Monitoring Center, Shanghai Municipal Environmental Monitoring Center and Henan Environmental Monitoring Center Station. This standard was approved by the Ministry of Environmental Protection on February 10,.2011. This standard has been implemented since June 1,.2011. This standard is explained by the Ministry of Environmental Protection. Determination of volatile organic compounds in soils and sediments Purge and trap/gas chromatography-mass spectrometry Warning. The internal standard, substitutes and standard samples used in the experiment are volatile toxic chemicals, and the solution should be prepared in a fume hood. In the operation, the protective equipment should be worn as required to avoid contact with skin and clothing.1 Scope of applicationThis standard specifies the purge and trap/gas chromatography-mass spectrometry for the determination of volatile organic compounds in soils and sediments. This standard applies to the determination of 65 volatile organic compounds in soils and sediments. If verified by this standard, it can also be applied to other volatilization. Determination of sex organic matter. When the sample amount is 5 g and the full-scan analysis is performed by standard quadrupole mass spectrometry, the detection limit of the target is 0.2-3.2 μg/kg. The lower limit is 0.8 to 12.8 μg/kg. See Appendix A for details.2 Normative referencesThe contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this standard. GB 17378.3 Marine monitoring specification Part 3. Sample collection, storage and transport 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, for mesh Quantitative analysis of the standard. 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. Usually before sample extraction or other pretreatment By adding, 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 A blank reagent water is placed in the sample vial in the laboratory prior to sampling and brought to the sampling site. Do not open when sampling, then follow The sample is shipped back to the laboratory and tested in the same operating steps as the sample to check for contamination during transport. 3.6 Full program blank whole program blank A blank reagent water is placed in the sample vial in the laboratory prior to sampling and brought to the sampling site. Simultaneously with the sample vial Cover and seal, then transport it back to the laboratory with the sample, and test it in the same way as the sample, for inspection from sample collection to analysis Whether the process is contaminated.4 Principle of the methodThe volatile organic compounds in the sample are enriched in the trap tube by high-purity helium (or nitrogen) purge, and the trap tube is heated and reversed with high purity helium gas. The components which are blown and thermally desorbed enter the gas chromatograph and are separated, and then detected by a mass spectrometer. By comparing with the standard mass spectrum of the target to be tested The comparison and retention time were qualitative and the internal standard method was used for quantification.5 reagents and materials5.1 Blank reagent water. double distilled water or water prepared by pure water equipment. A blank test is required before use to confirm that there is no interference peak in the retention time interval of the target or that the target substance is rich. The degree is below the method detection limit. 5.2 Methanol (CH3OH). Analytical grade of pesticide residues. 5.3 Standard stock solution. ρ = 1 000 ~ 5 000 mg/L. Commercially available certified standard solutions can be purchased directly or formulated with standard materials. 5.4 Standard use solution. ρ=10.0～100.0 mg/L. Standard use of volatile targets such as dichlorodifluoromethane, methyl chloride, trichlorofluoromethane, ethyl chloride, methyl bromide and vinyl chloride Prepared separately, the shelf life is usually one week, the standard use of other target materials is one month, or according to the manufacturer's instructions. 5.5 Internal standard solution. ρ=25 μg/ml. Fluorobenzene, chlorobenzene-D5 and 1,4-dichlorobenzene-D4 should be used as internal standards. Can be purchased directly from commercially available certified standard solutions, or with high quality Formulated in a standard solution. 5.6 Alternative standard solution. ρ = 25 μg/ml. Dibromofluoromethane, toluene-D8 and 4-bromofluorobenzene should be used as alternatives. Can be purchased directly from commercially available certified standard solutions, or with high quality Formulated in a concentration standard solution. 5.7 4-bromofluorobenzene (BFB) solution. ρ = 25 μg/ml. It can be purchased directly from a commercially available certified standard solution or prepared with a high quality standard solution. 5.8 Helium. Purity (volume fraction) is 99.999% or more. 5.9 Nitrogen. Purity (volume fraction) is 99.999% or more. Note. All the above standard solutions are treated with methanol as solvent, stored at 4 ° C or less in the dark or with reference to the manufacturer's product description. Should be restored to before use Mix at room temperature.6 Instruments and equipment6.1 Vials. 60 ml brown wide-mouth glass bottles with Teflon-silica-lined screw caps (or larger than 60 ml glass of other sizes) Bottle), 40 ml brown glass bottle and colorless glass bottle. 6.2 Sampler. Disposable plastic syringe or stainless steel dedicated sampler. 6.3 Gas Chromatograph. With split/splitless inlet, it can control the electronic pressure of the carrier gas and can be programmed. 6.4 Mass spectrometer. Electron bombardment (EI) ionization source, scanning from 35 u to 270 u in 1 s; with NIST mass spectrometer, manual/auto tuning Harmonics, data acquisition, quantitative analysis and library search. 6.5 Purge and trap device. The purging device can heat the sample to 40 ° C, and the trap tube is mixed with 1/3 Tenax, 1/3 silica gel and 1/3 activated carbon. Adsorbent or other equivalent adsorbent. If a purge and trap without an autosampler is used, the purge tube should be equipped with at least 5 g Sample and 10 ml of water. 6.6 Capillary column. 30 m × 0.25 mm, 1.4 μm film thickness (6% nitrile propyl phenyl 94% dimethyl polysiloxane fixative); or use other Capillary column for equivalent performance. 6.7 Balance. Accuracy is 0.01 g. 6.8 Hermetic syringe. 5 ml. 6.9 Microinjectors. 10, 25, 100, 250 and 500 μl. 6.10 Brown glass bottle. 2 ml with Teflon-silica liner and solid screw cap. 6.11 Disposable Pasteur glass pipettes. 6.12 Shovel. 6.13 Medicine spoon. PTFE or stainless steel. 6.14 Common instruments and equipment used in general laboratories.7 samples7.1 Sample collection The collection of soil and sediment samples is based on the relevant provisions of HJ/T 166 and GB 17378.3, respectively. Can be used at the sampling site for the swing The portable instrument for the determination of the organic matter measures the sample at a high level of the target. At least 3 parallel samples should be collected for all samples And use a 60 ml vial (or larger than 60 ml vials of other sizes) to collect another sample for high-volume samples. Volatile organic matter and sample moisture content. 7.1.1 Sampling method for manual injection method This sampling method is suitable for a purging and trapping device without an autosampler. Use a shovel or a spatula to collect the sample as quickly as possible into a 60 ml vial (or larger than 60 ml vials of other sizes) and fill as much as possible. Quickly remove the sample from the vial thread and the attached surface and seal the vial. 7.1.2 Sampling method for automatic injection mode This sampling method is suitable for purging and trapping devices with an autosampler. Place a clean magnetic stir bar in each 40 ml brown vial before sampling, seal, label and weigh (accurate to 0.01 g), record its weight and indicate on the label. When sampling, use the sampler to collect the appropriate amount of sample into the sample vial and quickly remove the vial. The sample is adhered to the thread and the sample adhered to the outer surface. Note 1. If a sample is taken using a disposable plastic syringe, the diameter of the syringe section should extend into the neck of the 40 ml vial. Syringe section at the end of the syringe The points should be cut off before sampling. A syringe can only be used to collect one sample. If a stainless steel special sampler is used, the sampler must be equipped with a booster. The soil can be pushed into the vial. Note 2. If the target content in the sample is initially determined to be less than.200 μg/kg, about 5 g sample is collected; if the target content in the sample is initially determined to be greater than or equal to At.200 μg/kg, approximately 1 g and 5 g samples should be taken separately. 7.2 Preservation of samples Samples should be refrigerated after collection. It should be analyzed as soon as possible after being shipped back to the laboratory. The sample storage area in the laboratory should be free of organic interference at 4 °C. The following save time is 7 days. 7.3 Determination of moisture content of the sample Take 5 g (accurate to 0.01 g) sample at (105 ± 5) °C for at least 6 h, divide the difference in sample quality before and after drying by drying The mass of the pre-sample is multiplied by 100 to calculate the sample moisture content w (%) to the nearest 0.1%.8 Analysis steps8.1 Instrument Reference Conditions 8.1.1 Purge and trap reference conditions Purge flow rate. 40 ml/min; purge temperature. 40 ° C; preheating time. 2 min; purge time. 11 min; dry blowing time. 2 min; Pre-desorption temperature. 180 ° C; desorption temperature. 190 ° C; desorption time. 2 min; baking temperature..200 ° C; baking time. 8 min; Transmission line temperature..200 ° C. The rest of the parameters are set according to the instruction manual of the instrument. 8.1.2 Gas Chromatography Reference Conditions Inlet temperature..200 ° C; carrier gas. helium; split ratio. 30.1; column flow (constant current mode). 1.5 ml/min; temperature program. 38 ° C (1.8 min) → 10/min ° C → 120 ° C → 15/min ° C → 240 ° C (2 min). 8.1.3 Mass Spectrometry Reference Conditions Scanning mode. full scan; scanning range. 35 ~ 270 u; ionization energy. 70 eV; electron multiplier voltage. with tuning voltage To; interface temperature. 280 ° C; the rest of the parameters are set according to the instrument manual. Note 1. In order to improve the sensitivity, the selective ion scanning method can also be used for analysis. The characteristic ion selection is referred to Appendix B. 8.2 Calibration 8.2.1 Instrument performance check Pipette 1~2 μl BFB solution (5.7) with a micro syringe, directly into the gas chromatograph for analysis or add 5 ml blank reagent The water (5.1) was injected into the gas chromatograph by a purging and trapping device for analysis. Key ion abundance of BFB obtained by quadrupole mass spectrometry Meet the standards specified in Table 1, otherwise you need to adjust the parameters of the mass spectrometer or consider cleaning the ion source. If the instrument software cannot be automatically determined When the critical ion abundance of BFB meets the criteria in Table 1, the average value of the ion abundance of the peak scanning point and the two scanning points before and after it can be taken. Key ion abundance is obtained after deducting the background value and should meet the criteria in Table 1. The background value can be selected from the 20 scan points before the BFB peak. At any point, the background value should be due to column bleed or instrument background ions. Note 2. BFB key ion abundance standards can be performed with reference to the instrument manufacturer's instructions when using ion traps or other types of mass spectrometers. Table 1 BFB key ion abundance standards Mass ion abundance standard mass ion abundance standard 50% 95% of 5% to 40% 174 is greater than 50% of mass 95 75 quality 95% to 80% 175 quality 174 5% to 9% 95 base peak, 100% relative abundance 176 quality 174 93% ~ 101% 96% 95% 5% to 9% 177 Quality 5% 5% to 9% 173 is less than 2% of mass 174 - - 8.2.2 Drawing of the calibration curve Transfer a certain amount of standard use solution (5.4) and substitute standard solution (5.6) to blank reagent water (5.1) with a micro syringe. The standard series of target and substitute mass concentrations of 5.00, 20.0, 50.0, 100 and.200 μg/L were prepared. 5.00 ml of the above standard series to 40 ml vials with a gas tight syringe (if no autosampler is added, join directly To the purge tube, add 10.0 μl of the internal standard solution (5.5), so that the internal standard concentration of each point is 50.0 μg/L. By instrument Refer to condition (8.1), measure from low concentration to high concentration, record the retention time and quantitative deviation of the standard series target and corresponding internal standard. The response value of the sub (first or second characteristic ion). Figure 1 shows the total ion chromatogram of the target under the instrument conditions specified in this standard. Abundance 2.00 time -- > 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 1-dichlorodifluoromethane; 2-chloromethane; 3-chloroethylene; 4-bromomethane; 5-chloroethane; 6-trichlorofluoromethane; 7-1,1-dichloroethylene; 8-acetone; - iodomethane; 10-disulfide Carbon; 11-dichloromethane; 12-trans-1,2-dichloroethylene; 13-1,1-dichloroethane; 14-2,2-dichloropropane; 15-cis-1. 2-dichloroethylene; 16-2-butanone; 17-bromochloride Methane; 18-chloroform; 19-dibromofluoromethane; 20-1,1,1-trichloroethane; 21-carbon tetrachloride; 22-1,1-dichloropropene; 23-benzene; 24-1 ,2-dichloroethane; 25-fluorobenzene; 26-trichloroethylene; 27-1,2-dichloropropane; 28-dibromomethane; 29-monobromodichloromethane; 30-4-methyl-2-pentanone; 31-to......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 605-2011_English be delivered?Answer: Upon your order, we will start to translate HJ 605-2011_English as soon as possible, and keep you informed of the progress. 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