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HJ 743-2015 English PDF

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HJ 743-2015: Soil and sediment. Determination of polychlorinated biphenyls (PCBs). Gas chromatography mass spectrometry
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Basic data

Standard ID HJ 743-2015 (HJ743-2015)
Description (Translated English) Soil and sediment. Determination of polychlorinated biphenyls (PCBs). Gas chromatography mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Classification of International Standard 13.080
Word Count Estimation 21,239
Date of Issue 2015-05-04
Date of Implementation 2015-07-01
Quoted Standard GB 17378.3; GB 17378.5; HJ 613; HJ/T 166
Regulation (derived from) Ministry of Environmental Protection Announcement 2015 No. 28
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the determination in soils and sediments more PCBs by gas chromatography - mass spectrometry. This standard applies to seven kinds of soils and sediments indicative of PCBs and more than 12 kinds of measurement coplanar PCBs are. Other PCBs are also available for the determination if verified. When the sample volume is 10.0g, when using selected ion scan mode, the method detection limit of PCBs 0.4 ~ 0.6 ��g/kg, measured in Appendix Ao

HJ 743-2015: Soil and sediment. Determination of polychlorinated biphenyls (PCBs). Gas chromatography mass spectrometry


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Soil and sediment. Determination of polychlorinated biphenyls (PCBs) National Environmental Protection Standard of the People 's Republic of China Soil and sediments of polychlorinated biphenyls Determination of gas chromatography - mass spectrometry Soil and sediment - Determination of Polychlorinated biphenyls (PCBs) Test mass spectrometry 2015-05-04 release 2015-07-01 implementation Ministry of Environmental Protection release I directory Preface .ii

1 Scope of application

2 normative reference documents

3 terms and definitions

4 Principle of the method

5 reagents and materials

6 instruments and equipment

7 samples .3

8 Analysis steps

9 Results calculation and representation

10 Precision and Accuracy 9 11 quality assurance and quality control 12 Waste treatment .10 Appendix A (normative) method of detection limit and lower limit of determination Appendix B (informative appendix) Determination of target reference parameter 13 Appendix C (informative) method of precision and accuracy 13

Foreword

For the implementation of the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate soil and sediment The determination of PCBs, the development of this standard. This standard specifies the determination of polychlorinated biphenyls in soil and sediments by gas chromatography-mass spectrometry. This standard is the first release. Appendix A of 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. Jiangsu Province Environmental Monitoring Center. The standard verification unit. Taizhou City Environmental Monitoring Center Station, Henan Province Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Ministry of Environmental Protection Nanjing Environmental Protection Science Research Institute and Nanjing Entry-Exit Inspection and Quarantine Bureau Electronic and Electrical Products Laboratory. The environmental protection department of this standard approved on May 4,.2015. This standard has been implemented since July 1,.2015. This standard is explained by the Ministry of Environmental Protection. 11 Scope of application This standard specifies the determination of polychlorinated biphenyls in soil and sediments by gas chromatography-mass spectrometry. This standard applies to the determination of seven indicative PCBs and 12 coplanar polychlorinated biphenyls in soil and sediments. other Polychlorinated biphenyls can also be determined by this method if verified. When the sampling amount is 10.0 g, the detection limit of PCB method is 0.4 ~ 0.6 μg/kg when the selected ion scanning mode is adopted, The lower limit of determination is 1.6 ~ 2.4 μg/kg, see Appendix A.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. For those who do not mind the date of the reference file, the valid version applies In 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 monitoring

3 terms and definitions

3.1 Indicative PCBs Soil and sediment - Determination of polychlorinated biphenyls - Gas chromatographic - mass spectrometry WARNING. The solvents and reagents used in the test are of some toxicity and some PCBs are highly carcinogenic, The process should be carried out in a fume hood, operating in accordance with the requirements of wearing protective equipment, to avoid solvent and reagents direct contact with the skin Skin and clothing. 2 refers to PCBs that are used as alternative monitoring of PCB contamination. 3.2 Coplanar PCBs Refers to non-contiguous or mono-ortho-substituted polychlorinated biphenyls in polychlorinated biphenyls, which is similar to dioxins.

4 principle of the method

Extraction of polychlorinated biphenyls (PCBs) in soils or sediments by appropriate extraction methods (microwave extraction, ultrasonic extraction, etc.) According to the sample matrix interference, select the appropriate purification method (concentrated sulfuric acid sulfonation, copper powder desulfurization, Florisil column, silica gel column And other gel permeation purification column), the extract purification, concentration, constant volume, with gas chromatography - mass spectrometry separation, detection, within Quantitative method.

5 reagents and materials

Unless otherwise stated, analytical analytical reagents and experimental water are used in accordance with national standards. 5.1 Toluene (C7H8). Chromatographic pure 5.2 n-hexane (C6H14). pure chromatography. 5.3 Acetone (CH3COCH3). Chromatographic pure. 5.4 anhydrous sodium sulfate (Na2SO4). excellent grade pure. In the muffle furnace at 450 ℃ baking 4 hours after the cooling, placed in the dryer glass bottle in reserve. 5.5 Potassium carbonate (K2CO3). excellent grade pure. 5.6 nitric acid. ρ (HNO3) = 1.42 g/ml. 5.7 Nitric acid solution. 1 9. 5.8 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml. 5.9 N-Hexane - Acetone Mixed Solvents. 1 1. Mixed with n-hexane (5.2) and acetone (5.3) in a 1. 1 by volume ratio. 5.10 N-Hexane - Acetone Mixed Solvent. 9 1. Mixed with n-hexane (5.2) and acetone (5.3) at a volume ratio of 9. 1. 5.11 Potassium carbonate solution. ρ = 0.1 g/ml. Weigh 1.0 g of potassium carbonate (5.5) in water and set to 10.0 ml. 5.12 Copper powder (Cu). 99.5%. 3 before use with nitric acid solution (5.7) to remove the copper oxide surface of the oxide, with distilled water to remove the residual acid, and then acetone cleaning, And drying the copper powder under a nitrogen stream so that the copper powder has a bright surface. Pre-treatment. 5.13 Polychlorinated biphenyl standard stock solution. ρ = 10 ~ 100 mg/L. Prepared with n-hexane dilution of pure standard material, the standard solution at 4 ℃ under the light sealed cold storage, can be stored for six months. Can also be straight (See Polychlorinated Biphenyl Mixed Standard Solution or Single Component Polychlorinated Biphenyl Standard Solution), Storage Time See also A description of the standard solution certificate. 5.14 Standard use of polychlorinated biphenyls. ρ = 1.0 mg/L (reference concentration). The standard stock solution (5.13) was diluted with n-hexane (5.2). 5.15 internal standard stock solution. ρ = 1000 ~ 5000 mg/L. Select 2,2 ', 4,4'5,5'-hexabromobiphenyl or o-nitrobromobenzene as internal standard; when decachlor biphenyl is a non-test compound, Use of decachlor as an internal standard. Can also be purchased directly to prove the standard solution. 5.16 Internal standard liquid. ρ = 10 mg/L (reference concentration). The internal standard stock solution (5.15) was diluted with n-hexane (5.2). 5.17 Substitute stock solution. ρ = 1000 ~ 5000 mg/L. When 2,2 ', 4,4'5,5'-hexabromobiphenyl or tetrachloro-m-xylene is selected as a substitute, when the decabenium is a non-test compound, Also available as a substitute for decachlor. Can also be purchased directly to prove the standard solution. 5.18 Substitute liquid. ρ = 5.0 mg/L (reference concentration). The stock solution (5.17) was diluted with acetone (5.3). 5.19 decafluorotriphenylphosphine (DFTPP) solution. ρ = 1000 mg/L, the solvent is methanol 5.20 ten fluorotriphenylphosphine use of liquid. ρ = 50.0 mg/L Transfer to 500 μl of decarotluorotriphenylphosphine (DFTPP) solution (5.19) to a 10 ml volumetric flask with n-hexane (5.2) Capacity to mark, mix. 5.21 Florisil Column. 1000 mg, 6 ml. 5.22 Silica gel column. 1 000 mg, 6 ml. 5.23 Graphite carbon column. 1000 mg, 6 ml. 5.24 quartz sand. 20 ~ 50 mesh In the muffle furnace at 450 ℃ baking 4 hours after the cooling, placed in a glass bottle in the dryer to save. 5.25 diatomaceous earth (100 to 400 mesh) In the muffle furnace at 450 ℃ baking 4 hours after the cooling, placed in a glass bottle in the dryer to save. 46 instruments and equipment 6.1 Gas Chromatography-Mass Spectrometer. Capillary Split/Splitless Inlet with Constant or Constant Pressure Function; Column Thermostat Programmable Temperature; with EI source. 6.2 Column. quartz capillary column, length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm, stationary phase 5% - phenyl-methyl Polysiloxane, or equivalent column. 6.3 Extraction device. microwave extraction device, Soxhlet extraction device, probe type ultrasonic extraction device or a device with considerable function. Need to be used before and in the use of blank test, all interfaces are strictly prohibited the use of grease lubricant. 6.4 Concentration device. nitrogen blowing concentrator, rotary evaporator, KD concentrator or equipment with considerable function. 6.5 Sampling vials. wide mouth brown glass bottle or polytetrafluoroethylene liner screw glass bottle. 6.6 Common laboratory equipment and equipment.

7 samples

7.1 Collection and storage of samples Soil samples were collected and stored in accordance with the relevant requirements of HJ/T 166, and the sediment samples were in accordance with the relevant requirements of GB 17378.3 Collection and preservation. The samples are stored in a clean, clean, wide-mouthed brown glass or polytetrafluoroethylene liner, Transport should be sealed in the process, as soon as possible back to the laboratory analysis. Such as temporarily can not be analyzed, should be stored below 4 ℃ cold storage Time is 14 d, the sample extraction solution below 4 ℃ dark storage time is 40 d. 7.2 Preparation of the sample Remove the foreign matter (stones, leaves, etc.) from the sample and weigh about 10 g (accurate to 0.01 g) of the sample, the soil sample One in accordance with the determination of dry matter content of HJ 613, the other by adding an appropriate amount of anhydrous sodium sulfate (5.4), grinding homogenized into flow sand, If extracted with pressurized fluid, it is dehydrated with diatomaceous earth (5.23). Sediment samples were prepared according to GB 17378.5 Rate, another reference to soil samples dehydrated. Preparation of dry soil and sediment samples, can refer to HJ 166 and GB 17378.3 related parts to operate. collection Drying and screening of samples should avoid direct sunlight and cross-contamination between samples. 7.3 Determination of moisture Determination of dry matter content of soil samples According to HJ 613, the moisture content of sediment samples was measured according to GB 17378.5 carried out. 7.4 Pretreatment of the sample 7.4.1 Extraction Using microwave extraction or ultrasonic extraction, can also be used Soxhlet extraction, pressurized fluid extraction. If a substitute is used to indicate the sample Full recovery efficiency, you can weighed in the sample to be extracted by adding a certain amount of alternative use of liquid (5.18), so that substitutes 5 concentration near the midpoint of the standard curve. 7.4.1.1 Microwave extraction Weigh the sample 10.0 g (according to the sample concentration of the compound to be measured to increase or reduce the amount of sample) in the extraction tank, add Into 30 ml of n-hexane-acetone mixed solvent (5.9). Extraction temperature was 110 ℃, microwave extraction time was 10 min. Collection of extraction liquid. 7.4.1.2 Ultrasonic extraction Weigh 5.0 ~ 15.0 g sample (according to the sample concentration of the compound to be measured to increase or reduce the amount of sample), placed in the glass Beaker, add 30 ml of n-hexane - acetone mixed solvent (5.9), with a probe ultrasonic extraction device, continuous ultrasonic extraction 5 min, Collect the extraction solution. The extraction process was repeated three times and the extraction solution was combined. 7.4.1.3 Soxhlet extraction Approximately 10.0 g of the prepared sample was weighed with a paper sleeve (which could be appropriately increased or decreased depending on the concentration of the compound to be tested in the sample ), Add 100 ml of n-hexane-acetone mixed solvent (5.9), extract 16-18 h, reflux rate of about 10 times/h. Collection of mention Take the solution. 7.4.1.4 pressurized fluid extraction Weigh 5.0 ~ 15.0 g sample (according to the sample concentration of the compound to be measured to increase or reduce the amount of sample), according to the sample The appropriate extraction volume of the volume of the extraction tank, into the sample, n-hexane - acetone mixed solvent (5.9) as the extraction solution, according to the following parameters The extraction conditions were as follows. extraction temperature 100 ℃, extraction pressure 1500 psi, static extraction time 5 min, elution 60% Volume, nitrogen purge time 60 s, extraction cycle times 2 times. Collect the extraction solution. 7.4.2 Filtration and dehydration If the extract can not be completely separated from the solid sample, centrifugation can be taken after the supernatant or filter separation. Such as the presence of significant water extract, the need for dehydration. In the glass funnel pad a layer of glass wool or glass fiber filter, shop Add about 5 g of anhydrous sodium sulfate (5.4), the extract directly through the funnel to filter into the concentrates, with about 5 ~ 10 ml Alkane-acetone mixed solvent (5.9) The washing vessel was thoroughly washed and the washings were also filtered through a funnel into a concentrated vessel. Finally reused Wash the anhydrous sodium sulfate with a little of the above mixed solvent. 7.4.3 Concentrate and replace the solvent The use of nitrogen blowing concentration method, can also be used by rotary evaporation concentration, KD concentration and other enrichment methods. Nitrogen blowing concentrator set the temperature of 30 ℃, a small flow of nitrogen to extract the extract to the required volume. If you need to replace the solvent system, The extract is concentrated to 1.5 to 2.0 ml, and the concentrator tube wall is washed with about 5 to 10 ml of solvent, and then concentrated to a small flow rate of nitrogen The required volume. 7.4.4 Purification Such as the darker color of the extract can be first concentrated sulfuric acid purification, can remove most of the organic compounds, including some organic chlorine pesticide. When the pesticide and the polychlorinated hydrocarbons are interfered with in the sample extract, the fluororbury column or silica gel column column The presence of significant pigment interference, the use of graphite carbon column purification. Sediment samples contain a large amount of elemental sulfur when disturbed Removed with activated copper powder. 7.4.4.1 concentrated sulfuric acid purification 6 concentrated sulfuric acid before purification, the solvent must be replaced with n-hexane. Follow the procedure in 7.4.3 to replace the solvent of the extract N-hexane and concentrated to 10-50 ml. The solution was placed in a 150 ml separatory funnel and about one tenth of the extraction was added Product of sulfuric acid (5.8), shaking 1 min, standing stratification, discarded sulfuric acid layer. Repeat the steps to the two-phase interface as described above Clear and were colorless and transparent. To the n-hexane extract, a potassium carbonate solution (5.11) corresponding to one half volume thereof was added, After shaking, place the layer, discard the water phase. Repeat steps 2 to 4 above until the aqueous phase is neutral, followed by step 7.4.2 The n-hexane extract was dehydrated. Note 1. in the concentrated sulfuric acid purification process, to prevent the heat explosion, concentrated sulfuric acid slowly after the first shake, constantly deflated, and then a little vigorous shaking. 7.4.4.2 desulfurization The volume of the extract is preconcentrated to 10 to 50 ml. If concentrated sulfur crystallization, can be used to centrifuge the crystal deposition in the glass The bottom of the container, and then use the dropper carefully transferred out of all the solution. Approximately 2 g of activated copper powder was added to the above extraction concentrate (5.12), the oscillation mixture at least l ~ 2 min, the solution sucked out with the copper powder, transferred to a clean glass container, To be further purified or concentrated. 7.4.4.3 Fluororim column purification The fluororbury column was washed with about 8 ml of n-hexane to keep the column adsorbent surface wetted. The extract was pre-concentrated to the procedure according to 7.4.3 About 1.5 to 2 ml, with a straw to transfer it to the fluororbury column for 1 min, let the solution out of the column and discard, keep the column Adsorbent surface infiltration. Add about 2 ml of n-hexane-acetone mixed solvent (5.10) and stay for 1 min, with 10 ml of small concentrated The eluate was received and the column was washed with n-hexane/acetone solution (5.10) until the volume of the eluted solution was received to 10 ml until. 7.4.4.4 silica gel column purification The silica gel column was washed with about 10 ml of n-hexane. The extract was concentrated and replaced with n-hexane, which was purified by silica gel column See Section 7.4.4.3 for step steps. 7.4.4.5 graphite carbon column purification The graphite carbon column was washed with about 10 ml of n-hexane. The extract was concentrated and replaced with n-hexane. When the PCB was analyzed, toluene was used Solvent for the elution solution, the specific elution steps see 7.4.4.3, collecting toluene eluent volume of 12 ml; analysis in addition to PCB81, PCB77, PCB126 and PCB169 other than the PCB, but also can be used hexane - acetone mixed solution (5.10) for the wash The specific procedure is shown in 7.4.4.3 and the volume of eluent collected is 12 ml. Note 2. Each batch of newly purchased Flory silica column, silica gel column, graphite carbon column and other purification column, are required to do blank test to determine its no impact test When the impurity is interrupted, it can be used. 7.4.5 Concentration and internal standard The purified eluate was concentrated in a 7.4.3 step and set to 1.0 ml. Take 20 μl of internal standard use of the liquid, add concentrated volume After the sample, mix and transfer to 2 ml vials, to be analyzed. 7.5 blank sample preparation The blank sample was prepared by the same procedure as the pretreatment (7.4) of the sample using quartz sand (5.24) instead of the actual sample. 78 Analysis steps 8.1 Instrument reference conditions 8.1.1 Gas chromatographic conditions Inlet temperature. 270 ° C, splitless injection; column flow. 1.0 ml/min; oven temperature. 40 ° C at 20 ° C/min Heated to 280 ° C for 5 min; injection volume. 1.0 μl. 8.1.2 Mass spectrometry conditions Quadrupole temperature. 150 ° C; ion source temperature. 230 ° C; transmission line temperature. 280 ° C; scan mode. select ion Scanning (SIM), the primary selection of polychlorinated biphenyls See Appendix B; Solvent Delay Time. 5 min. 8.2 Calibration 8.2.1 Instrument performance check Before the sample was analyzed, the gas chromatographic-mass spectrometry system was run with 1 μl of decafluorotriphenylphosphine (DFTPP) solution (5.20) Performance check, the resulting abundance of mass ions should meet the requirements of Table 1. Table 1 DFTPP key ion and ion abundance evaluation table Mass ion m/z abundance evaluation quality ion m/z abundance evaluation 51 Strength of 19-60% of 19 pieces of.199.199% of the strength of 198 fragments of 5-9% 68 strength less than 69 pieces of debris 2% 275 strength of 198 fragments of 10-30% 70 Strength Less than 69 pieces of 2% 365 Strength greater than 198% of debris 1% 127 Strength of 196 pieces of 40-60% 441 present but no more than 443 pieces of strength 197 Strength Less than 198% of debris 442 Strength greater than 198% of debris 40% 198 base, relative strength 100% 443 strength of 442 fragments of 17-23% 8.2.2 Drawing of standard curves Standard series is prepared with standard use of polychlorinated biphenyls (5.14). If the sample is analyzed, a substitute is used to indicate full recovery (5.18), the standard series of compounds and substitutes for PCBs are. & lt; RTI ID = 0.0 & gt; 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L, 500 μg/L, respectively. So that the concentration of.200 μg/L. 8.2.3 Drawing of standard curves Analyze according to the instrument reference conditions (8.1) to obtain the mass spectra of the target compounds at different concentrations, The retention time of the compound and the peak area (or peak height) of the quantitative ion mass spectrum. 8.3 Determination Take the test sample (7.3) and make the same analysis according to the same analytical procedure as the standard curve. 8.4 blank test Take the blank sample (7.4) and perform the same analytical procedure as the standard curve. Calculate and represent results 9.1 Qualitative analysis The retention time (RRT), auxiliary qualitative ion and target ion peak area ratio (Q) of the target in the sample were compared with the standard Comparison of goods to qualitative. The characteristic ions of the PCBs are shown in Appendix B. The retention time of the target compound in the sample is the expected retention time (ie, the average relative retention time in the standard sample) The relative standard deviation should be controlled within ± 3%; the target qualitative ion and target ion peak area ratio of the target compound in the sample The relative deviation of the expected Q value (ie, the ratio of the peak area of the target curve to the qualifying ion and the target ion) should be controlled at ± 30%. Polych...

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