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HJ 921-2017 English PDF

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HJ 921-2017: Soil and sediment--Determination of organochlorine pesticides--Gas chromatography
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Basic data

Standard ID HJ 921-2017 (HJ921-2017)
Description (Translated English) Soil and sediment--Determination of organochlorine pesticides--Gas chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Word Count Estimation 19,194
Date of Issue 2017-12-28
Date of Implementation 2018-04-01
Regulation (derived from) Ministry of Environmental Protection Bulletin 2017 No. 85
Issuing agency(ies) Ministry of Ecology and Environment

HJ 921-2017: Soil and sediment--Determination of organochlorine pesticides--Gas chromatography


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People's Republic of China national environmental protection standards Soil and sediment-Determination of organochlorine pesticides -Gas chromatography 2017-12-28 Published 2018-04-01 implementation Directory Foreword .ii 1 Scope 1 2 Normative references 1 3 method principle 1

4 Reagents and materials

5 instruments and equipment

6 samples .3 7 Analysis Step 4 8 Results Calculation and Presentation 6 9 Precision and accuracy 7 10 Quality Assurance and Quality Control .7 11 Waste treatment .8 Appendix A (Normative) Detection limit and lower limit of the method 9 Appendix B (informative) method of precision and accuracy 10 Appendix C (informative) sample purification method .15

Foreword

In order to carry out "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, standardize the soil and sediments Determination of organochlorine pesticides, the development of this standard. This standard specifies the determination of soil and sediment 23 kinds of organochlorine pesticides by gas chromatography. Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Jiangsu Provincial Environmental Monitoring Center. This standard verification unit. Taizhou City Environmental Monitoring Center Station, Henan Province Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Dalian City Environmental Monitoring Center, Nanjing Environmental Protection Research Institute of Environmental Protection and Exit Inspection and Quarantine of Nanjing Electrical and Electronic Product Laboratory. This standard MEP approved on December 28, This standard since April 1,.2018 come into operation. This standard is interpreted by the MEP. Soil and sediments - Determination of organochlorine pesticides - Gas chromatography Warning. The organic solvents and reference materials used in the experiment are toxic substances, standard solution preparation and sample preparation Should be carried out in a fume hood; operation should be worn protective clothing as required to avoid direct contact with the skin and clothing.

1 scope of application

This standard specifies the determination of organochlorine pesticides in soil and sediment by gas chromatography. This standard applies to soil and sediment α - BHC, HCB, γ - BHC, β - BHC, δ - BHC, sulfur Dan I, aldrin, endosulfan II, epichlorohydrin, epichlorohydrin, o, p'-didehydrin, gamma-chlordane, alpha-chlordane, trans- p, p'-Drip, o, p'-Drip, Dieldrin, Endrin, o, p'-DDT, p, p'- p, p - DDT, mirex and other 23 kinds of organochlorine pesticides determination. If other organochlorine pesticides through the verification, can also be measured using this standard. When the sample volume was 10.0 g, the detection limit of 23 organochlorine pesticides was 0.04 μg/kg ~ 0.09 μg/kg. The limit is 0.16 μg/kg ~ 0.36 μg/kg. See Appendix A for details.

2 Normative references

This standard references the following documents or the terms. For undated references, the effective version applies to this standard. GB 17378.3 Marine monitoring code - Part 3. Sample collection, storage and transport GB 17378.5 Marine monitoring code - Part 5. Sediment analysis HJ 494 water sampling technical guidance HJ 613 Determination of soil dry matter and moisture Gravimetric method HJ 783 Extraction of organic matter from soils and sediments by pressurized fluid extraction HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring HJ/T 166 Soil Environmental Monitoring Technical Specifications

3 method principle

Organochlorine pesticides in soils or sediments are extracted, purified, concentrated, and fixed. After using the electron capture detector Phase detection. According to the retention time of qualitative, external standard method.

4 Reagents and materials

Unless otherwise stated, analytical grade reagents that meet national standards are used. Experimental water for the new preparation of pure water or distilled water. 4.1 n-Hexane (C6H14). Chromatographic purity. 4.2 Acetone (CH3COCH3). Chromatography pure. 4.3 Dichloromethane (CH2Cl2). Chromatographic purity. 4.4 anhydrous sodium sulfate (Na2SO4). excellent grade pure. Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 4.5 acetone - n-hexane mixed solvent I. 1 1. Mix with acetone (4.2) and n-hexane (4.1) at a volume ratio of 1.1. 4.6 acetone - n-hexane mixed solvent Ⅱ. 1 9. Mix with acetone (4.2) and n-hexane (4.1) at a volume ratio of 1.9. 4.7 Organochlorine pesticide standard stock solution. ρ = 10 mg/L ~ 100 mg/L. Buy a commercially available certified standard solution, store at 4 ° C in a dark, airtight refrigerator or with reference to a standard solution certificate. Make Use should be returned to room temperature and shake. 4.8 Organochlorine pesticides standard solution. ρ = 1.0 mg/L. Dilute organochlorine pesticide standard stock solution with n-hexane (4.1) (4.7). Avoid light at 4 ℃ closed refrigeration, storage period of six months. 4.9 Magnesium silicate solid phase extraction column. commercially available, 1000 mg/6 ml. 4.10 quartz sand. 270 μm ~ 830 μm (50 mesh ~ 20 mesh). Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 4.11 Diatomaceous earth. 37 μm to 150 μm (400 mesh to 100 mesh). Baking in a muffle furnace at 450 ° C for 4 h, cooling and placing in a glass jar with a grit stopper and holding in a desiccator. 4.12 glass wool or glass fiber filter. 400 ° C in a muffle furnace baking 1 h, cooled and placed in a sealed glass jar sealed. 4.13 high purity nitrogen. purity ≥ 99.999%. 4.14 Endrin and p, p'-DDT mixed standard solution. ρ = 1.0 mg/L. Commercially available standard endrin and p, p'-DDT standard solutions were purchased and diluted with n-hexane (4.1). Sealed in the dark at 4 ℃ cold storage.

5 instruments and equipment

5.1 Gas Chromatograph. With Electronic Capture Detector (ECD) with Split/Splitless Inlet for Programmable Temperature. 5.2 Column 5.2.1 Column 1. Column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm, stationary phase 5% polydiphenylsiloxane and 95% polydimethylsiloxane, or other equivalent column. 5.2.2 Column 2. Column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm, stationary phase 14% Polynyl cyanopropyl silicone Alkane and 86% polydimethylsiloxane, or other equivalent column. 5.3 Extraction device. microwave extraction device, Soxhlet extraction device, pressurized fluid extraction device or a device with a considerable function, No grease lubricant is allowed on all interfaces. 5.4 Concentration device. Nitrogen blowing instrument, rotary evaporator, KD concentrator or equipment with a considerable function. 5.5 Sampling Bottles. Wide-mouth brown glass bottles or Teflon-lined screw-on glass bottles. 5.6 general laboratory equipment and equipment.

6 samples

6.1 Sample Collection and Storage Soil samples were collected and stored according to the relevant requirements of HJ/T 166, and samples of marine sediments were related according to GB 17378.3 Requirements for collection and preservation, surface water sediment samples collected according to HJ/T 91 and HJ 494 requirements. Samples are saved in advance Clean the clean bottle (5.5), as soon as possible back to the laboratory analysis, the transport process should be sealed dark. If temporarily unable to analyze, It should be refrigerated at below 4 ℃ for 14 days. Sample extract (6.4.1) 4 ℃ below the dark storage, preservation The time is 40 days. 6.2 Sample Preparation Remove foreign matter (stones, leaves, etc.) from the sample and weigh two portions of sample at about 10 g (to the nearest 0.01 g). Soil samples A product for the determination of dry matter content; the other by adding an appropriate amount of anhydrous sodium sulfate (4.4), grinding homogenized into sand-like dehydration; If fruit is extracted by pressurized fluid extraction, it is dehydrated with diatomaceous earth (4.11). One sample of sediment is used to determine the moisture content and the other A reference soil sample is dehydrated. 6.3 Determination of moisture Determination of dry matter content of soil samples in accordance with HJ 613 implementation, determination of sediment moisture content in accordance with GB 17378.5 carried out. 6.4 Sample Preparation 6.4.1 Extraction 6.4.1.1 Microwave extraction The sample (6.2) all transferred to the extraction tank, adding 30 ml of acetone - n-hexane mixed solvent I (4.5), set the extraction The temperature was 110 ℃, microwave extraction 10 min. The extract is collected after centrifugation or filtration. 6.4.1.2 Soxhlet extraction The sample (6.2) was transferred to the Soxhlet extractor paper sleeve, 100 ml acetone-n-hexane mixed solvent (I 4.5) Extraction 16 h ~ 18 h, reflux rate of about 3 times/h ~ 4 times/h. The extract is collected after centrifugation or filtration. 6.4.1.3 Pressurized fluid extraction HJ 783 in accordance with the requirements of the extraction. Note. Other equivalent extraction methods may be used if verified. 6.4.2 dehydration Place a layer of glass wool or glass fiber filter (4.12) on the glass funnel, add about 5 g of anhydrous sodium sulfate (4.4) and then The extract (6.4.1) was directly filtered through a funnel to the concentration device (5.4), and then about 5 ml ~ 10 ml acetone - n-hexane Solvent I (4.5) The container containing the extract was thoroughly washed and filtered through a funnel to the above concentrator. 6.4.3 Concentration After the dehydration at 45 ℃ below the extract (6.4.2) concentrated to 1 ml, to be purified. To replace the solvent system, the extract was concentrated to 1.5 ml ~ 2.0 ml, with 5 ml ~ 10 ml of n-hexane (4.1) Replacement, and then concentrated extract to 1 ml, to be purified. 6.4.4 Purification The magnesium silicate solid phase extraction column (4.9) was washed with about 8 ml of n-hexane (4.1), and the magnesium silicate solid phase extraction column adsorbent Surface infiltration. Pipette the concentrated extract (6.4.3) onto a magnesium silicate solid phase extraction cartridge and leave for 1 min Effluent. Add 2 ml of acetone-n-hexane mixed solvent Ⅱ (4.6) and stay for 1 min, with 10 ml small concentrated tube to receive wash After degreasing, continue to wash the cartridge with acetone-n-hexane mixed solvent II (4.6) until the volume of the eluate received is 10 ml. Note. If verified, other equivalent methods can also be used to purify. See Appendix C. 6.4.5 concentrated volume The purified eluate (6.4.4) according to the 6.4.3 step concentration and volume to 1.0 ml, and then transferred to 2 ml sample vial, To be analyzed. 6.5 blank sample preparation A blank sample was prepared according to the same procedure as Sample Preparation (6.4), replacing the actual sample with quartz sand (4.10).

7 Analysis steps

7.1 GC reference conditions Inlet temperature. 220 ℃; Injection mode. splitless injection to 0.75min after opening shunt, split outlet flow of 60ml/min; Carrier gas. high purity nitrogen (4.13), 2.0 ml/min, constant current; Makeup gas. high purity nitrogen (4.13), 20 ml/min; Column temperature program. The initial temperature of 100 ℃, 15 ℃/min heating to 220 ℃, holding 5 min, at 15 ℃/min Warming up to 260 ℃ for 20 min; Detector temperature. 280 ℃; Injection volume. 1.0 μl. 7.2 Calibration 7.2.1 The establishment of the standard curve Were appropriate amount of organochlorine pesticide standard solution (4.8), diluted with n-hexane (4.1), the preparation of standard series, The concentrations of organochlorine pesticides were 5.0 μg/L, 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L And 500 μg/L (this is the reference concentration). According to the instrument conditions (7.1) from low concentration to high concentration in order to standard series of solution injection, detection, record the target Retention time, peak height or peak area. The concentration of the target in a standard series of solutions is taken as abscissa, with its corresponding peak height or peak Area for the vertical axis, the establishment of a standard curve. 7.2.2 Standard sample chromatogram Under the recommended instrument reference conditions, the chromatograms for target 1 and 2 are shown in Figure 1 and Figure 2, respectively. 1.α - BHC; 2. Hexachlorobenzene; 3.γ - BHC; 4.β - BHC; 5.δ - BHC; 6. Endosulfan I; 7. Aldrin; 8. Endosulfan II; 9. Epichlorohydrin; 10. Epoxy heptachlor; 11. o, p'-Drip; 12. γ-Chlordane; 13. α-Chlordane; 14. Trans- Iraq; 16.o, p'- droplet; Dieldrin; 18. Endrin; 19. o, p'-DDT; 20. p, p'-drops; 21. cis- nonachlorohydrochloride; 22. p, p'- DDT; Mirex Fig.1 Reference GC chromatograms of 23 organochlorine pesticide standard samples (column 1, ρ = 100 μg/L) 1. Hexachlorobenzene; 2.α - BHC; 3. γ - BHC; 4. Endosulfan I; 5. Aldrin; 6. β - BHC; 7. δ - BHC; 8. Endosulfan II; 9. Epichlorohydrin; 10. Epoxy heptachlor; 11. o, p'-Drip; 12. γ-Chlordane; 13. α-Chlordane; 14. Trans- Iraq; 16. Dieldrin; 17. o, p'- Drip; 18. Endrin; 19. o, p'-DDT; 20. p, p'-drip; 21. cis-nonachloro; 22. p, p'- DDT; Mirex Figure 2 Reference gas chromatogram of 23 organochlorine pesticide standard samples (column 2, ρ = 100 μg/L) 7.3 Determination of the sample The determination of sample (6.4) is carried out according to the same instrument analysis conditions as established in the standard curve (7.2.1). 7.4 Determination of blank sample The blank sample (6.5) was measured according to the same instrument analysis conditions as the sample measurement (7.3).

8 results calculated and said

8.1 Qualitative analysis According to the retention time of the target qualitative. Before sample analysis, you should establish a retention time window t3S, t standard within 72h Column solution, the average retention time of a target, S standard solution of a standard solution of the average retention time of a standard deviation difference. When analyzing samples, the target retention time should be within the retention window. When the analysis of the target on the column is detected, it is necessary to use a different polarity of the column to help qualitative. The target is double When the column is detected, as detected, otherwise not detected. 8.2 Quantitative analysis According to the established standard curve (7.2.1), according to the target peak area or peak height, the use of external standard method. 8.3 Results Calculation 8.3.1 Calculation of soil sample results The target soil content ω1 (μg/kg), calculated according to equation (1). Where. ω1 - soil samples in the target content, μg/kg; ρ - calculated from the standard curve of the sample mass concentration of the target, μg/L; V-- sample volume, ml; m - Weigh the quality of the sample, g; wdm - dry matter content in the sample,%. 8.3.2 Calculation of Sediment Sample Results Target sediment content ω2 (μg/kg), calculated according to equation (2).  (2) Where. ω2 - sediment sample target content, μg/kg; ρ - calculated from the standard curve of the sample mass concentration of the target, μg/L; V-- sample volume, ml;   2   H 2O mw m - Weigh the quality of the sample, g; wH2O - moisture content of the sample,%. 8.4 results indicated When the test result is less than 1.00 μg/kg, the result is kept at the second decimal place. When the test result is greater than or equal to 1.00 μg/kg When the result holds three significant figures.

9 precision and accuracy

9.1 Precision Six laboratories performed a series of six samples of quartz sand spiked at concentrations of 2.00 μg/kg, 20.0 μg/kg and 80.0 μg/kg, respectively The relative standard deviations in the laboratory ranged from 2.1% to 10%, from 1.5% to 7.7% and from 0.47% to 5.7%, respectively. The relative standard deviations in the laboratory ranged from 4.7% to 15%, 1.3% to 8.5%, and 0.90% to 3.6%, respectively. The repeatability limits Were 0.27 μg/kg ~ 0.42 μg/kg, 1.9 μg/kg ~ 2.8 μg/kg and 3.7 μg/kg ~ 8.8 μg/kg respectively. The reproducibility limits were 0.41 μg/kg to 0.80 μg/kg, 2.0 μg/kg to 4.3 μg/kg, and 4.0 μg/kg to 10.3 μg/kg. See Appendix B. 9.2 Accuracy Six laboratories measured quartz spiked samples at spiking levels of 2.00 μg/kg, 20.0 μg/kg and 80.0 μg/kg, respectively, The spiked recoveries ranged from 77.0% to 116%, from 73.6% to 105% and from 92.0% to 105%, respectively. The final spike recoveries were 84.9% ± 25.4% -102% ± 18.8%, 77.5 ± 13.2% ± 96.4% ± 11.2%, 94.4 ± 4.8% ± 104% ± 2.0%. plus Sandy soils with a standard concentration of 20.0 μg/kg and six sediment samples from Taihu Lake were measured repeatedly for 6 replicates. The spiked recoveries ranged from 60.5% -108% and 58.5% -119% respectively, and the final recoveries of the spiked samples were 67.4% ± 9.2% -108% ± 4.2% and 68.1% ± 19.6% ~ 109% ± 34.4%. See Appendix B. 10 Quality Assurance and Quality Control 10.1 blank experiment Analyze at least one laboratory blank every 20 samples or batches (less than 20 samples/batch) for a measure of the target Should be below the detection limit of the method. 10.2 standard curve The correlation coefficient of the standard curve is ≥0.995. For each 20 samples or batches (less than 20 samples/batches), a standard curve midpoint concentration solution should be analyzed, which measures The relative deviation of the result from the initial curve at this point should be ≤20%. Otherwise, the standard curve should be redrawn. 10.3 Determination of parallel samples Analyze at least one parallel sample per 20 samples or batches (less than 20 samples/batch), and determine the results of a single parallel sample The relative deviation should be less than 20%. 10.4 Blank spiked sample determination Analyze at least one blank, spiked sample every 20 samples or batches (less than 20 samples/batch) with a recovery of 75% ~ Between 105%. 10.5 Substrate spike determination Analyze at least one spiked sample every 20 samples or batches (less than 20 samples/batch) at the spiked concentration of the original sample Degree of 1 to 5 times, soil, sediment spiked sample recovery rate should be between 60% to 120%. 10.6 Instrument Performance Check The chromatographic system should be checked before or every 24 h. Inject 1.0 μl of endrin and mix p, p'-DDT Standard solution (4.14), determine the degradation rate, according to formula (3) ~ formula (5) calculation. If in addition to the above compounds detected In addition, the detection of endrin, endrin, and p, p'-dihydropyran, p, p'-drops, it is indicated that endrin and p, p'- DDT decomposition occurs, if the degradation rate of a single component ≥ 15% or the sum of the degradation rate of both ≥ 30%, the need for injection Mouth and column head for maintenance. After the system inspection, before the determination of the sample. (3) (4) Total degradation rate% = DDT degradation rate% Endrin degradation rate% (5) 11 Waste treatment Waste generated during the experiment should be collected centrally and sent to a qualified unit for disposal. %% Peak area drops and drops DDT degradation rate of 100 Peak area drops Iraqi drops DDT () () %% Peak area of endrin Aldrin ketone Endrin degradation rate of 100 Peak area endrin endrin endrin aldosterone ketone () () Appendix A. (Normative) Method detection limit and determination of the lower limit Table A.1 shows the method of detection of the target and the lower limit of determination. Table A.1 detection limits and lower limits of determination No. Compound Name CAS No. The detection limit (g/kg) Lower limit of determination (g/kg) 1 α-BHC 6 319-84-6 0.06 0.24 2 Hexachlorobenzene 118-74-1 0.07 0.28 3 γ-BHC 6 58-89-9 0.06 0.24 4 β-BHC 6 319-85-7 0.05 0.20 5 δ-BHC 6 319-86-8 0.06 0.24 6 Endosulfan I 959-98-8 0.07 0.28 7 Aldrin 309-00-2 0.09 0.36 8 Endosulfan II 33213-65-9 0.05 0.20 Epoxide Heptachlor 1024-57-3 0.05 0.20 10 Epoxy Heptachlor 28044-83-9 0.06 0.24 11 o, p'-Dritiol 3424-82-6 0.06 0.24 12 α-Chlordane 5103-71-9 0.05 0.20 13 γ-Chlordane 5103-74-2 0.05 0.20 14 Trans-nonachloro 39765-80-5 0.05 0.20 15 p, p'-Drip I-72-55-9 0.05 0.20 16 o, p'- drops 53-19-0 0.06 0.24 17 Dieldrin 60-57-1 0.04 0.16 18 Endrin 72-20-8 0.07 0.28 19 o, p'-DDT 789-02-6 0.09 0.36 20 p, p'- droplet 72-54-8 0.06 0.24 21 cis-nonahydrochloride 5103-73-1 0.05 0.20 22 p, p'-DDT 50-29-3 0.06 0.24 23 mirex 2385-85-5 0.07 0.28

Appendix B

(Informative) The precision and accuracy of the method Tables B.1 and B.2 show the precision and accuracy of the method such as repeatability limit, reproducibility limit and spike recovery. Table B.1 Summary of methods for precision Serial number of the compound name Spike level (μg/kg) The measurement results average value (μg/kg) Laboratory relative Standard deviation range (%) Laboratory phase The standard deviation (%) Repeatability r (μg/kg) Reproducibility limit R (μg/kg) 1 α-BHC 2.00 1.93 3.1 ~ 7.4 13 0.33 0.75 20.0 18.5 2.6 ~ 4.7 2.3 1.9 2.1 80.0 79.9 0.47 ~ 2.5 1.6 4.3 5.3

2 hexachlorobenzene

2.00 1.83 4.9 ~ 9.0 12 0.35 0.67 20.0 18.3 1.5 ~ 6.3 1.9 2.7 2.7 80.0 81.1 0.82 ~ 2.0 0.90 3.8 4.1 3 γ- BHC 2.00 1.88 3.3 ~ 7.9 14 0.34 0.80 20.0 18.2 2.6 ~ 6.2 5.7 2.3 3.6 80.0 79.8 0.83 ~ 3.0 3.2 4.6 8.3 4 β-BHC 2.00 1.95 2.1 ~ 7.7 8.3 0.33 0.54 20.0 17.9 3.2 ~ 7.5 7.1 2.7 4.3 80.0 75.6 0.78 ~ 3.6 2.6 4.2 6.7 5 δ- BHC 2.00 1.92 6.3 ~ 10 7.8 0.41 0.56 20.0 17.1 2.8 ~ 7.7 4.6 2.4 3.1 80.0 76.7 0.49 ~ 2.6 1.1 4.6 4.8

6 endosulfan I

2.00 1.89 4.4 ~ 8.6 4.7 0.36 0.41 20.0 18.0 3.6 ~ 6.1 3.9 2.4 3.0 80.0 78.0 0.84 ~ 2.0 1.0 3.8 4.0

7 Aldrin

2.00 2.05 3.3 ~ 6.8 9.1 0.33 0.60 20.0 18.6 3.3 ~ 4.8 2.3 2.1 2.3 80.0 78.2 0.86 ~ 2.6 2.3 3.7 6.1

8 endosulfan II

2.00 1.87 4.2 ~ 10 8.5 0.38 0.56 20.0 18.2 3.4 ~ 6.1 4.6 2.4 3.2 80.0 79.9 0.68 ~ 3.7 1.0 4.9 5.1

9 epoxy heptachlor

2.00 2.05 3.7 ~ 6.1 7.3 0.27 0.49 20.0 18.8 2.5 ~ 6.1 6.3 2.1 3.8 80.0 82.1 0.76 ~ 5.7 1.3 6.7 6.7 10 Epoxy Heptachlor 2.00 1.88 5.5 ~ 9.1 7.5 0.38 0.52 20.0 18.6 3.4 ~ 5.3 3.9 2.2 2.9 80.0 80.8 0.51 ~ 5.4 2.1 8.1 8.7 Serial number of the compound name Spike level (μg/kg) The measurement results average value (μg/kg) Laboratory relative Standard deviation range (%) Laboratory phase The standard deviation (%) Repeatability r (μg/kg) Reproducibility limit R (μg/kg) 11 o, p'- trickle Iraq 2.00 1.90 4.5 ~ 9.4 9.4 0.40 0.62 20.0 19.3 2.5 ~ 5.0 5.8 2.0 3.6 80.0 81.6 2.9 ~ 4.4 1.8 8.5 8.8 12 α-Chlordane 2.00 1.83 3.9 ~ 10 6.6 0.39 0.49 20.0 15.5 3.7 ~ 7.5 8.5 2.1 4.2 80.0 77.3 1.8 ~ 5.2 3.6 7.5 10.3 13 γ-Chlordane 2.00 1.99 3.1 ~ 8.3 8.3 0.35 0.56 20.0 18.7 3.1 ~ 4.4 1.9 2.1 2.1 80.0 77.6 0.74 ~ 5.7 3.0 6.9 9.1 14 trans-nonachloro 2.00 1.83 4.9 ~ 9.0 12 0.34 0.68 20.0 18.7 2.3 ~ 4.4 1.3 2.0 2.0 80.0 79.7 0.73 ~ 4.1 0.9 4.3 4.5 15 p, p'- trickle Iraq 2.00 1.83 3.0 ~ 8.7 12 0.35 0.69 20.0 18.4 2.3 ~ 5.5 4.2 2.1 2.9 80.0 79.7 0.81 ~ 4.2 1.6 5.4 6.0 16 o, p'- droplet 2.00 1.94 3.0 ~ 7.3 13 0.30 0.74 20.0 18.1 2.6 ~ 6.3 3.2 2.7 2.9 80.0 80.2 0.94 ~ 3.1 1.1 4.5 4.8 17 Dieldrin 2.00 1.95 4.7 ~ 8.4 11 0.34 0.68 20.0 18.2 1.5 ~ 6.2 5.7 2.3 3.6 80.0 80.1 3.2 ~ 5.0 1.6 8.8 8.9 18 Endrin 2.00 1.76 4.5 to 10 5.9 0.39 0.46 20.0 17.0 3.2 ~ 7.7 4.8 2.8 3.4 80.0 79.4 1.8 ~ 3.7 3.3 6.6 9.5 19 o, p'- DDT 2.00 2.02 3.9 ~ 8.3 6.9 0.36 0.51 20.0 17.4 2.8 ~ 6.1 3.5 2.2 2.7 80.0 82.2 0.70 ~ 5.5 1.9 6.0 7.0 20 p, p'- drops 2.00 1.76 3.1 ~ 9.0 6.4 0.33 0.44 20.0 18.3 2.7 ~ 6.4 2.2 2.6 2.7 80.0 82.9 0.83 ~ 3.9 1.0 5.2 5.2 21 cis-nonachloro 2.00 1.70 4.5 ~ 7.8 15 0.30 0.76 20.0 17.9 1.5 ~ 6.2 4.2 2.4 3.0 80.0 79.9 0.73 ~ 5.7 3.3 6.1 9.3 22 p, p'- DDT 2.00 1.87 3.9 ~ 10 5.8 0.42 0.49 20.0 18.4 2.8 ~ 5.1 5.7 2.1 3.5 80.0 79.8 0.85 ~ 4.1 1.0 4.5 4.7 23 Mirex 2.00 1.94 3.1 to 7.4 13 0.33 0.76 20.0 17.7 2.0 ~ 5.0 1.7 2.0 2.0 80.0 79.5 0.81 ~ 4.2 1.5 5.3 5.8 Table B.2 Summary of Method Accuracy No. Compound Name Sample Type Spike level (μg/kg) Spike recovery range (%) Spike recovery final value (%) 1 α-BHC White quartz sand 2.00 77.0 ~ 109 96.2 ± 24.8 20.0 88.9 ~ 94.5 92.3 ± 4.2 80.0 98.5 ~ 103 99.6 ± 3.2 Sandy soil 20.0 77.5 ~ 83.8 80.6 ± 4.6 Taihu Lake sediments 20.0 85.1 ~ 90.0 87.5 ± 3.8

2 hexachlorobenzene

White quartz sand 2.00 77.7 ~ 110 91.3 ± 21.2 20.0 89.4 ~ 93.3 91.2 ± 3.4 80.0...

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