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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 735-2015: Soil and sediment. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry Status: Valid
Basic dataStandard ID: HJ 735-2015 (HJ735-2015)Description (Translated English): Soil and sediment. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z18 Classification of International Standard: 13.080 Word Count Estimation: 21,257 Date of Issue: 2015-02-07 Date of Implementation: 2015-04-01 Quoted Standard: GB 17378.3; GB 17378.5; HJ 613; HJ/T 166 Regulation (derived from): Ministry of Environmental Protection Announcement 2015 No. 7 Issuing agency(ies): Ministry of Ecology and Environment Summary: This Standard specifies the determination of volatile halogenated hydrocarbons in soil and sediment in the purge and trap/gas chromatography - mass spectrometry. This Standard applies to the determination of chloride in soil and sediment and other 35 kinds of volatile halogenated hydrocarbons. Other volatile halogenated hydrocarbons if verified also apply to this standard. HJ 735-2015: Soil and sediment. Determination of volatile halohydrocarbons. Purge and trap gas chromatography 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. Soil and sediment. Determination of volatile halohydrocarbons.Purge and trap gas chromatography mass spectrometry National Environmental Protection Standard of the People 's Republic of China Determination of volatile halohydrocarbons in soil and sediments Purge and trap/gas chromatography - mass spectrometry Soil and sediment - Determination of volatile halohydrocarbons - Purge and trap gas chromatography mass spectrometry Released in.2015-02-07 2015-04-01 implementation Ministry of Environmental Protection released I directory Preface .ii 1 Scope of application2 normative reference documents3 Principle of the method4 reagents and materials5 instruments and equipment6 samples .3 7 Analysis Step 38 Results calculation and presentation9 precision and accuracy10 Quality assurance and quality control 11 Waste treatment .9 12 Precautions .9 Appendix A (normative appendix) The detection limit and the lower limit of the target Appendix B (informative) Target parameter determination reference parameter ..12 Appendix C (informative) method of precision and accuracyForewordFor the implementation of the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate soil and sediment Determination of volatile halogenated hydrocarbons, the development of this standard. This standard specifies the determination of 35 kinds of volatile halogenated hydrocarbons such as methyl chloride in soil and sediments. Purge and capture/gas chromatography Spectrum method. This standard is the first release. Appendix A to this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Harbin Environmental Monitoring Center Station. The standard verification unit. Heilongjiang Province Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Changchun City Environmental Monitoring Heart station, Anshan City Environmental Monitoring Center Station, Qiqihar City Environmental Monitoring Center Station and Daqing City Environmental Monitoring Center Station. This standard is approved by the Ministry of Environmental Protection on February 7,.2015. This standard is implemented as of April 1,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of volatile halohydrocarbons in soil and sediments Purge and trap/gas chromatography - mass spectrometry WARNING. The internal standards, substitutes and standard solutions used in the tests are volatile, toxic chemicals. Fume hood to operate; should be required to wear protective equipment, 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 halogenated hydrocarbons in soil and sediments. This standard is applicable to the determination of 35 kinds of volatile halogenated hydrocarbons such as methyl chloride in soil and sediments. Other volatile halogenated hydrocarbons such as The validation is also applicable to this standard. When the sampling amount of 5g, 35 kinds of volatile halogenated hydrocarbons detection limit of 0.3 ~ 0.4 μg/kg, the determination of the lower limit of 1.2 ~ 1.6 μg/kg. See Appendix A. for details.2 normative reference documentsThe contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. GB 17378.3 Marine Monitoring Specification Part 3 Sample Collection Storage and Transportation GB 17378.5 Marine monitoring regulations Part 5 Sediment analysis Determination of Dry Matter and Moisture in Soil Technical specification for soil environmental monitoring3 Principle of the methodThe volatile halogenated hydrocarbons in the sample are purged with high purity helium (or nitrogen) and adsorbed in the trap, Heat and re-blow with helium (or nitrogen), the volatile halogenated hydrocarbons in the trap are desorbed by heat, and the components are passed into the gas chromatographic fraction After the separation, with a mass spectrometer for testing. According to the retention time, fragment ion mass ratio and different ion abundance ratio qualitative, internal standard method Quantitative.4 reagents and materials4.1 Experimental water. secondary distilled water or water equipment prepared by water. Before use to be blank test, to confirm no target or The target concentration is lower than the method detection limit. 4.2 methanol (CH3OH). pesticide residues, before use to be tested to confirm that no target or target concentration is lower than the method of detection limit. 4.3 Standard stock solution. ρ =.2000mg/L. Direct purchase of commercially available standard solution. Store at or below -10 ° C or refer to the manufacturer's product description. Should be used when used Revert to room temperature and shake. Kaifeng in a dense bottle can be kept for a month. 4.4 standard use of liquid. ρ = 2.5 mg/L. 2 Take appropriate standard stock solution (4.3) and dilute it with methanol (4.2). In the dense bottle -10 ℃ below the dark preservation, Can save for a week. 4.5 internal standard stock solution. ρ =.2000mg/L. Fluorobenzene, 1-chloro-2-bromopropane, 4-bromofluorobenzene as internal standard. Can be purchased directly to prove the standard solution can also be used standard Quality preparation. Store in light below -10 ° C or refer to the manufacturer's product description. Use should be restored to room temperature, and shake. open Sealed in a dense bottle can be kept for a month. 4.6 internal standard use of liquid. ρ = 2.5mg/L. Take appropriate internal standard stock solution (4.5) and dilute it with methanol (4.2). In the dense bottle -10 ℃ below the dark preservation, Can save for a week. 4.7 Substitute stock solution. ρ =.2000mg/L. Use dichloromethane-d2,1,2-dichlorobenzene-d4 as a substitute. Can be purchased directly to prove the standard solution can also be used standard Quality preparation. Store in light below -10 ° C or refer to the manufacturer's product description. Use should be restored to room temperature, and shake. open Sealed in a dense bottle can be kept for a month. 4.8 Substitute liquid. ρ = 2.5mg/L. Take appropriate amount of the stock solution (4.7) and dilute it with methanol (4.2). In the dense bottle -10 ℃ below the light protection Save, save for a week. 4.9 4-bromofluorobenzene (BFB) solution. ρ = 25mg/L, can be directly purchased certified standard solution can also be prepared using standard materials. in -10 ° C or less in the dark to save or refer to the manufacturer's product description. Use should be restored to room temperature, and shake. After opening in the dense The bottle can be kept for one month. 4.10 quartz sand. 20 ~ 50 mesh. Before use, pass the test to confirm that no target or target is below the method detection limit. 4.11 helium. purity ≥ 99.999%, deoxidized by deoxidizer, molecular sieve dehydration.5 instruments and equipment5.1 Sampling equipment. shovel and stainless steel spoon. 5.2 Sampling Bottle. Polytetrafluoroethylene Silicone Tape Screw Cover 60ml wide-mouth glass bottle. 5.3 Vials. 40ml brown glass bottles and colorless glass bottles with PTFE cover screw cap. 5.4 Gas Chromatography-Mass Spectrometer. EI Ionization Source. 5.5 Column. quartz capillary column, length 30 m, inner diameter 0.25 mm, film thickness 1.4 μm, stationary phase 6% nitrile phenyl/94% Dimethylpolysiloxane, and other equivalent capillary columns may also be used. 5.6 Purge and trap device. suitable for soil sample determination. The capture tube was mixed with 1/3Tenax, 1/3 silica gel, 1/3 activated carbon Adsorbents or other equivalent adsorbents. 5.7 Microinjectors. 10 μl, 25 μl, 100 μl, 250 μl, 500 μl and 1000 μl. 5.8 Balance. Accuracy 0.01 g. 5.9 reciprocating oscillator. oscillation frequency of 150 times/min, can be fixed purge bottle. 5.10 brown dense bottle. 2 ml, with PTFE packing. 5.11 pH meter. accuracy of ± 0.05. 5.12 portable refrigerated containers. volume 20 L, the temperature below 4 ℃. 5.13 disposable Pasteur glass pipette. General laboratory equipment and equipment.6 samples6.1 Collection of samples Samples of soil samples and sediments were collected in accordance with the relevant requirements of HJ/T 166 and GB 17378.3. Can be used at the sampling site Portable VOC analyzer on the sample concentration of the high and low screening. Low concentrations of samples should be collected at least 3 copies of parallel samples. Mining Before the sample, place the magnetic stirrer in the vial (5.3), seal and weigh (to 0.01g). Approximately 5 g of sample was collected into the sample In the bottle, quickly remove the sample bottle thread and the outer surface of the adhesive sample, immediately sealed the sample bottle. Also collect a sample Sampling vials (5.2) for the determination of high levels of samples and moisture content. The samples were collected and placed in a portable freezer (5.12) Back to the lab. Note 1. When the initial screening of volatile halohydrocarbon content is greater than.200μg/kg, the sample is considered to be a high content sample. 6.2 Storage of samples After the sample reaches the laboratory, it should be analyzed as soon as possible. If you can not timely analysis, the sample should be stored below 4 ℃, shelf life For 14 d. There should be no organic interference in the sample storage area. 6.3 Preparation of the sample 6.3.1 Preparation of low content samples Remove the vial (5.3) and wait until the room temperature is returned (accurate to 0.01 g). Add 5.0ml of experimental water (4.1), 10 μl of the substitutes (4.8) and 10 μl of the internal standard (4.6), to be tested. 6.3.2 Preparation of high content samples Remove the sample vials in the laboratory (5.2). After returning to room temperature, take 5 g of the sample in the vial (5.3) and quickly 10.0 ml of methanol (4.2) was added and sealed and shaken at a frequency of 150 times/min on a reciprocating oscillator (5.9) for 10 min. After standing for settling, approximately 1.0 ml of the extract was removed with a disposable Pasteur glass pipette (5.13) to a 2 ml brown dense flask (5.10) , If necessary, the extract can be centrifuged. The extract can be stored in the freezer at 4 ℃, the shelf life of 14d. After returning the extract to room temperature before analysis, 5 g of quartz sand (4.10) was added to the vial (5.3), 5.0 ml of (4.1), 10 μl to 100 μl of methanol extract, 10 μl of the extract (4.8) and 10 μl of the internal standard (4.6) Seal, to be tested. Note 2. If the concentration of the target compound in the methanol extract is high, it can be appropriately diluted by adding methanol. Note 3. If the concentration is too low or not detected by high-content methods, the sample should be re-analyzed using a low content method. 6.4 Preparation of blank samples 6.4.1 Low content of solid waste blank sample The sample was prepared in 5 g of quartz sand (4.10) and a low content blank sample was prepared according to 6.3.1. 6.4.2 High content of solid waste blank sample The sample was prepared in 5 g of quartz sand (4.10) and a high level blank sample was prepared according to 6.3.2. Determination of Moisture Determination of water content of soil samples According to HJ 613 implementation, the determination of water content of sediment samples in accordance with GB 17378.5 implementation.7 Analysis steps7.1 Instrument reference conditions 47.1.1 Purge and trap device reference conditions Purge flow. 40 ml/min, purge temperature. 40 ° C, purge time. 11 min; dry blowing time. 2 min; desorption temperature Degree. 180 ° C, desorption time. 3 min; baking temperature..200 ° C, baking time. 10 min; transmission line temperature. 110 ° C. 7.1.2 Gas chromatograph reference conditions Program temperature. 35 ℃ (5 min) 5 ℃/min 180 ℃ 20 ℃/min.200 ℃ (5 min); inlet temperature. 180 ℃; 20. 1; carrier gas. helium; interface temperature. 230 ° C; column flow. 1.2 ml/min. 7.1.3 Mass spectrometer reference conditions Ionization mode. EI; ion source temperature..200 ° C; transmission line temperature. 230 ° C; electron accelerating voltage. 70 eV; Scanning mass range. 35 amu ~ 300amu. Quantitative method. Select ion (SIM) method, quantitative ion See Appendix B. 7.2 Calibration 7.2.1 Instrument performance check The performance of the gas chromatograph - mass spectrometer should be checked before analyzing the sample daily. Take 1 μl of 4-bromofluorobenzene (4.9) solution directly into the solution Gas chromatographic analysis. The critical ion abundance of 4-bromofluorobenzene should meet the requirements in Table 1, otherwise the mass spectrometer and some Parameter to adjust or clean the ion source. Table 1 BFB critical ion abundance standard Mass ratio (m/z) ion abundance standard mass ratio (m/z) ion abundance standard 50% of the base of 15% to 40% 174 is greater than 50% of the base peak 75% of the base peak of 60% to 60% 175 174 peak of 5% to 9% 95 base, 100% relative abundance 176 174 peak 95% to 101% 96% of the base peak of 5% to 9% 177 176 peak of 5% to 9% 173 Less than 174 peaks 2% - - 7.2.2 Drawing of calibration curves With a micro-syringe were removed a certain amount of standard use of liquid (4.4) and the use of alternative liquid (4.8), to contain 5g stone (4.10), 5.0ml of experimental water (4.1) in the vial (5.3), the preparation of the target and the substitutes were 5, 10,25,50,100 ng of the standard series, and were added 10μl internal standard liquid (4.6), immediately sealed. Follow the instrument Test conditions (7.1) followed by injection analysis, the target quantification of the response value of the ion and the internal standard quantitative response value of the value of ions As the ordinate, the target content and the content of the standard content of the object as the abscissa, draw the calibration curve. Figure 1 is in this standard The chromatogram of the target under the condition of the instrument. 5-chloroethane; 6-trichlorofluoromethane; 7-1, 1-dichloroethylene; 8-chloropentane; Keywords dichloromethane-d2; 9-dichloromethane; 10-trans-1,2-dichloroethylene; 11-1,1-dichloroethane; 12-2,2-dichloropropane; , 2-dichloro 14-1 bromoethane; 15-bromoform; 16-1,1,1-trichloroethane; 17-carbon tetrachloride; 18-1,1-dichloropropene; 19-1,2-dichloro Ethane; 20-fluorobenzene; 21-trichlorethylene; 22-1,2-dichloropropane; 23-dibromomethane; 24-bromodichloromethane; 25-cis-1,3-dichloropropen; Trans-1,3-dichloropropene; 27-1-chloro-2-bromopropane; 28-1,1,2-trichloroethane; 29-tetrachlorethylene; 30-1,3-dichloropropane; 31-dibromo-1 Chloroethane; 32-1,2-dibromoethane; 33-1,1,1,2-tetrachloroethane; 34-bromoform; 35-4- bromofluorobenzene; 36-1, 2-tetrachloroethane; 37-1,2,3- Trichloropropane; 38-1,2-dichlorobenzene-d4; 39-1,2-dibromo-3-chloropropane; 40-hexachlorobutadiene Figure 1 Chromatogram of the target compound 7.2.2.1 Establish the calibration curve with the average response factor The relative response factor (iRRF) of the standard series i (target) (or substitutes) is calculated according to equation (1). (1) Where iRRF - the relative response factor for the i-th target (or substitute) in the standard series; IA - the response value of the quantified ions of the i-th target (or substitute) in the standard series; ISiA - the response value of the corresponding target ion in the standard series of the i-th target (or substitute) ISi - the content of the internal standard in the standard series, ng; I - the content of the i point of the standard series (or substitutes), ng. The average relative response of the target (or substitute) is calculated according to equation (2). (2) Where. RRF - the average relative response factor for the target (or substitute); RRF RRF = 1 ISi ISi ARRF i 6iRRF - the relative response of the i-point target (or substitute) in the standard series; N - standard series points. RRF standard deviation, according to formula (3) to calculate. (3) The relative standard deviation of RRF is calculated according to equation (4). (4) The relative standard deviation (RSD) of the standard series of target (or substitutes) relative response factor (RRF) should be less than or equal to 20%. 7.2.2.2 Draw the calibration curve with the least squares method The response ratio of the target compound and the corresponding internal standard is the ordinate, the concentration ratio is the abscissa, and the least squares method is used Calibration curve, the correlation coefficient of the standard curve ≥ 0.990. If the correlation coefficient of the calibration curve is less than 0.990, a non-line may also be used The sexual fit curve is calibrated, but should be calibrated using at least six concentration points. 7.3 Sample determination The prepared sample (6.3) was measured according to the instrument reference conditions (7.1). 7.4 blank test The prepared blank sample (6.4) was measured according to the instrument reference conditions (7.1). Calculation and representation of results 8.1 Qualitative analysis Data were collected in full scan mode, with the relative retention time (RRT) of the target compound in the sample, assisted qualitative ions and The ratio of the standard ion abundance ratio (Q) to the standard solution is qualitative. The relative retention time of the target compound in the sample and the school Quasi-Curve The relative retention time of the compound should be within ± 0.06. Auxiliary qualitative ion of the target compound in the sample and Quantum ion peak area ratio (Q sample) vs. standard curve Target compound Auxiliary qualitative ion and quantified ion peak area ratio (Q standard) Relative deviation control within ± 30%. Calculate the relative retention time RRT according to equation (5) ISRT RTRRT x (5) Where. RRT - relative retention time; RTX - retention time of target, min; RTIS - retention time of the internal standard, min. Mean relative retention time (RRT). Relative retention time average of the same target compound in the standard series RRFRRF SD 0 distance RRF SDRSD 7 According to the formula (6) to calculate the auxiliary qualitative ion and quantitative ion peak area ratio (Q) AQ (6) Where. At - quantitative ion peak area; Aq - auxiliary qualitative ion peak area. 8.2 Quantitative analysis Calculated according to the response value of the target and internal standard quantitation ions. When the quantitation ions of the target in the sample interfere with, Auxiliary ion quantification can be used, as detailed in Appendix B. 8.2.1 Calculation of target content (or substitutes) 1 m 8.2.1.1 Calculate with the average relative response factor When the target (or substitute) is calibrated using the average relative response factor, the content of the target is 1 m according to equation (7) Calculation. (7) Where. 1m - the content of the target (or substitute), ng; XA - the response value of the target ion (or substi......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 735-2015_English be delivered?Answer: Upon your order, we will start to translate HJ 735-2015_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 735-2015_English with my colleagues?Answer: Yes. The purchased PDF of HJ 735-2015_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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