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HJ 922-2017 English PDF

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HJ 922-2017: Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography
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Basic data

Standard ID HJ 922-2017 (HJ922-2017)
Description (Translated English) Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Word Count Estimation 20,224
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 922-2017: Soil and sediment--Determination of polychlorinated biphenyls--Gas chromatography


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

3 Terms and definitions

4 method principle 2 5 Interference and elimination .2 6 Reagents and materials .2

7 instruments and equipment

8 samples .3 9 Analysis Step 5 10 Results Calculation and Presentation 6 11 Precision and accuracy .8 12 Quality Assurance and Quality Control .8 13 Waste treatment .9 Appendix A (Normative) Methods of detection limit and lower limit of determination Appendix B (informative) precision and accuracy of the method Appendix C (informative) sample purification method 16

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 PCBs, the development of this standard. This standard specifies the gas chromatography determination of 18 kinds of PCBs in soil and sediment. 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 Environmental Monitoring Center Station, Henan Province Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Dalian City Environmental Monitoring Center, Nanjing Environmental Protection Research Institute and the Nanjing Entry-Exit Inspection and Quarantine Electronic and Electrical Products 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 sediment - Determination of PCBs - Gas chromatography Warning. The solvents and reagents used in the experiment have some toxicity, some PCBs are carcinogenic, the standard Solution preparation and sample preparation process should be carried out in a fume hood; operation should be worn protective equipment, avoid direct contact with the skin and clothing.

1 scope of application

This standard specifies the determination of PCBs in soil and sediment by gas chromatography. This standard applies to the determination of 7 indicative PCBs and 12 coplanar polychlorinated biphenyls in soils and sediments. other PCBs, if verified, can also be measured using this standard. When the sample volume is 10.0 g, the detection limit of PCBs is 0.03 μg/kg ~ 0.07 μg/kg, and the lower limit of determination 0.12 μg/kg to 0.28 μg/kg. See Appendix A for details.

2 Normative references

This standard references the following documents or the terms of them. 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 Terms and definitions

3.1 Indicative PCBs PCBs Refers to PCBs that are used as alternative monitors for the contamination of PCBs, including 2,4,4'-trichlorobiphenyl (PCB28), 2,2 ', 5,5'-tetrachlorobiphenyl (PCB52), 2,2', 4,5,5'-pentachlorobiphenyl (PCB101), 2,3 ', 4,4 ', 5-pentachlorophenol (PCB118), 2,2 ', 3,4,4', 5'-hexachlorobiphenyl (PCB138), 2,2 ', 4,4', 5,5'-hexachlorobiphenyl (PCB153) , 2,2 ', 3,4,4', 5,5'-heptachlor biphenyl (PCB180) and other seven compounds. Co-planar PCBs coplanar PCBs Refers to polychlorinated biphenyls that are not ortho or ortho-ortho substituted in PCBs and are similar in their toxicity to dioxins, including 3,3 ', 4,4'-tetrachlorobiphenyl (PCB77), 3,4,4', 5-tetrachlorobiphenyl (PCB81), 2,3,3 ', 4,4'- Benzene (PCB105), 2,3,4,4 ', 5-Pentachlorobenzene (PCB114), 2,3', 4,4 ', 5-Pentachlorobenzene (PCB118), 2', 3,4,4 ', 5 - Pentachlorobenzene (PCB123), 3,3 ', 4,4', 5-Pentachlorobenzene (PCB126), 2,3,3 ', 4,4', 5-Hexachlorobiphenyl (PCB156), 2,3,3 ', 4 , 4 ', 5'-hexachlorobiphenyl (PCB 157), 2,3 ', 4,4', 5,5'-hexachlorobiphenyl (PCB 167), 3,3 ', 4,4', 5,5'-hexachlorobiphenyl 2,3,3 ', 4,4', 5,5'-heptachlorobiphenyl (PCB189) and other 12 kinds of compounds. Among them 2,3 ', 4,4', 5-Pentachlorobenzene (PCB118) also Is indicative of PCBs.

4 method principle

PCBs in soils or sediments are extracted, purified, concentrated and fixed. Electron capture detectors Gas chromatography. According to the retention time of qualitative, external standard method.

5 Interference and elimination

Other organic impurities in the sample, interference PCBs determination, the choice of sulfuric acid, magnesium silicate column, such as appropriate net Method to remove. After purification, there will still be other compounds and the target compound at the same time peak, interference determination, through another Different polarity of the column auxiliary qualitative. If required, confirm that the sensitivity meets the requirements by gas chromatography-mass spectrometry.

6 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. 6.1 n-Hexane (C6H14). Chromatographic purity. 6.2 Acetone (CH3COCH3). Chromatography pure. 6.3 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. 6.4 Potassium carbonate (K2CO3). excellent grade pure. 6.5 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml. 6.6 acetone - n-hexane mixed solvent I. 1 1. Mix with acetone (6.2) and n-hexane (6.1) at a volume ratio of 1.1. 6.7 acetone - n-hexane mixed solvent Ⅱ. 1 9. Mix 1.9 volumes with acetone (6.2) and n-hexane (6.1). 6.8 Potassium carbonate solution. p = 0.1 g/ml. Weigh 100 g of potassium carbonate (6.4) dissolved in water, set to 1000 ml. 6.9 Polychlorinated biphenyls standard stock solution. ρ = 10.0 mg/L to 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. 6.10 PCB standard solution. ρ = 1.0 mg/L (reference concentration). Dilute PCB stock standard solution with n-hexane (6.1) (6.9). Avoid light at 4 ℃ closed refrigeration, storage period of six months. 6.11 Magnesium silicate solid phase extraction column. commercially available, 1000 mg/6 ml. Or according to the impurity content to choose other capacity of magnesium silicate SPE column. 6.12 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. 6.13 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. 6.14 glass wool or glass fiber filter. 400 ° C in a muffle furnace baking 1 h, cooled and placed in a sealed glass jar sealed. 6.15 high purity nitrogen. purity ≥ 99.999%.

7 instruments and equipment

7.1 Gas Chromatograph with Electronic Capture Detector (ECD) with Split/Splitless Inlet for Programmable Temperature. 7.2 Column 7.2.1 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. 7.2.2 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. 7.3 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. 7.4 Concentration device. Nitrogen blowing instrument, rotary evaporator, KD concentrator or equipment with a considerable function. 7.5 Sampling Bottles. Wide-mouth brown glass bottles or Teflon-lined screw-on glass bottles. 7.6 General laboratory commonly used instruments and equipment.

8 samples

8.1 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 (7.5), back to the laboratory analysis as soon as possible, the process of transportation should be sealed dark. If temporarily unable to analyze, It should be refrigerated at below 4 ℃ for 14 days. Sample extract (8.4.1) 4 ℃ below the dark storage, preservation The time is 40 days. 8.2 Preparation of samples 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 One for the determination of dry matter content; the other by adding an appropriate amount of anhydrous sodium sulfate (6.3), grinding into stream sand dehydration; such as If the fruit is extracted by pressurized fluid extraction, it is dehydrated with celite (6.13). One sample of sediment is used to determine the moisture content and the other A reference soil sample is dehydrated. 8.3 Determination of moisture Determination of dry matter content of soil samples performed according to HJ 613, Determination of moisture content of sediment samples in accordance with GB 17378.5 implementation. 8.4 Preparation of test specimens 8.4.1 Extraction 8.4.1.1 Microwave extraction Sample (8.2) was transferred to the extraction tank, and 30 ml acetone-n-hexane mixed solvent I (6.6) was added. Set extraction The temperature was 110 ℃, microwave extraction 10 min. The extract is collected after centrifugation or filtration. 8.4.1.2 Soxhlet extraction The sample (8.2) was transferred to the Soxhlet extractor paper sleeve, 100 ml acetone-n-hexane mixed solvent (I 6.6) Extraction 16 h ~ 18 h, reflux rate of about 3 times/h ~ 4 times/h. The extract is collected after centrifugation or filtration. 8.4.1.3 Pressurized fluid extraction HJ 783 in accordance with the requirements of the extraction. Note. Other equivalent extraction methods may be used if verified. 8.4.2 Dehydration Apply a glass wool or glass fiber filter (6.14) to the glass funnel and apply about 5 g of anhydrous sodium sulfate (6.3), then The extract (8.4.1) was filtered through a funnel directly to the concentration device (7.4), then 5 ml ~ 10 ml of acetone - n-hexane mixed Solvent I (6.6) The container containing the extract was thoroughly washed and filtered through a funnel to the above concentrator. 8.4.3 Concentration After the dehydration at 45 ℃ below the extract (8.4.2) 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 (6.1) Replacement, and then concentrated extract to 1 ml, to be purified. 8.4.4 Purification 8.4.4.1 Sulfuric acid purification If the extract color darker, you can first use sulfuric acid purification to remove most of the oxygenated organic compounds and some organochlorine medicine. The displacement solvent n-hexane extract (8.4.3) was transferred to 150 ml separatory funnel, slowly added 5 ml ~ 10 ml Sulfuric acid (6.5), mix gently and shake for 1 min. Stand aside stratification, discard the sulfuric acid layer. Repeat the above steps several times to sulfur Acid layer colorless. An appropriate volume of potassium carbonate solution (6.8) was added to the n-hexane extract, and after shaking, the layers were allowed to stand and the aqueous phase discarded. This procedure is repeated until the aqueous phase is neutral. Dehydration of the n-hexane extracts is carried out according to the same procedure as in 8.4.2. Note. In the sulfuric acid purification process, to prevent the heat explosion, add sulfuric acid and gently mix, continue to deflate, then slightly violent shake. 8.4.4.2 Magnesium silicate solid phase extraction column purification The magnesium silicate solid phase extraction column (6.11) was washed with about 8 ml of n-hexane (6.1), and the magnesium silicate solid phase extraction column adsorbent Surface infiltration. The concentrated extract (8.4.3) was transferred to a magnesium silicate solid phase extraction column with a straw for 1 min and then discarded Effluent. Add 2 ml acetone-n-hexane mixed solvent Ⅱ (6.7) 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 (6.7) 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 for details. 8.4.5 concentrated volume The purified eluate (8.4.4) according to the 8.4.3 step concentration and volume to 1.0 ml, then transferred to 2 ml sample vial, To be analyzed. 8.5 blank sample preparation A blank sample was prepared according to the same procedure as Sample Preparation (8.4), replacing the actual sample with quartz sand (6.12).

9 Analysis steps

9.1 GC reference instrument conditions Inlet temperature. 250 ℃; Injection mode. splitless injection to 0.75min after opening shunt, split outlet flow of 60ml/min; Carrier gas flow. high purity nitrogen (6.15), 2.0 ml/min, constant current; Makeup gas. high purity nitrogen (6.15), 20 ml/min; Column temperature program. The initial temperature of 100 ℃, 15 ℃/min heating to 220 ℃, hold 5 min, with 15 ℃/min liter Temperature to 260 ℃, hold 20 min; Detector temperature. 280 ℃; Injection volume. 1.0 μl. 9.2 Calibration 9.2.1 The establishment of calibration curve Were appropriate amount of PCB standard solution (6.10), diluted with n-hexane (6.1), the preparation of the standard series, and more The mass concentrations of PCBs 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 (9.1) 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. 9.2.2 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. 17.5 20 22.5 25 27.5 30 32.5 35 min Hz ECD1 A, (DXN2010 \\ 101117000010.D) 1.PCB28; 2.PCB52; 3.PCB101; 4.PCB81; 5.PCB77; 6.PCB123; 7.PCB118; 8.PCB114; 9.PCB153; PCB105; PCB138; PCB126; PCB1367; PCB146; PCB157; PCB141; PCB169; Figure 1 Reference GC chromatogram of 18 PCB standards (column 1, ρ = 100 μg/L) 1.PCB28; 2.PCB52; 3.PCB101; 4.PCB81; 5PCB777; 6, PCB123; 7.PCB118; 8.PCB114; 9.PCB153; PCB105; PCB138; PCB126; PCB137; PCB167; PCB146; PCB157; PCB141; PCB169; PCB1818. Figure 2 Reference Gas Chromatogram of 18 PCB Standards (Column 2, ρ = 100 μg/L) 9.3 Sample Determination The determination of sample (8.4) is carried out according to the same instrument analysis conditions as established in the standard curve (9.2.1). 9.3.2 Blank test The blank sample (8.5) was measured according to the same instrument analysis conditions as the sample measurement (9.3). 10 Results Calculation and Presentation 10.1 Qualitative analysis According to the retention time of the target qualitative. Before sample analysis, you should establish a retention time window t3S, t for the standard series of solutions 12 14 16 18 20 22 min Hz ECD2 B, (DXN2010 \\ 101220000017.D) In a target within 72 h retention time average, S standard solution of a target in an average retention time standard deviation. 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. 10.2 Quantitative analysis According to the established standard curve (9.2.1), according to the target peak area or peak height, the use of external standard method. 10.3 Results Calculation 10.3.1 Calculation of soil sample results The target soil content ω1 (μg/kg), calculated according to equation (1).  dm mw (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 of the sample,%. 10.3.2 Calculation of results in sediment samples Target sediment content ω2 (μg/kg), calculated according to equation (2).   2   H 2O mw (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; m - Weigh the quality of the sample, g; wH2O - moisture content of the sample,%. 10.4 results show When the determination result is less than 1.00 μg/kg, the result will remain two digits after the decimal point. When the measurement result is greater than or equal to 1.00 μg/kg, The result retained three significant figures. 11 precision and accuracy 11.1 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 11%, from 1.5% to 7.8% and from 0.49% to 6.2%, respectively Laboratory relative standard deviation ranged from 2.3% to 14%, 1.3% to 8.5% and 1.0% to 3.6%, respectively; the repeatability limits were 0.26 μg/kg ~ 0.44 μg/kg, 1.8 μg/kg ~ 2.8 μg/kg and 3.7 μg/kg ~ 8.7 μg/kg respectively.The reproducibility limits were 0.29 μg/kg ~ 0.78 μg/kg, 2.0 μg/kg to 4.1 μg/kg, 4.0 μg/kg to 9.5 μg/kg. See Appendix B. 11.2 Accuracy Six laboratories tested spiked quartz sand samples spiked at concentrations of 2.00 μg/kg, 20.0 μg/kg and 80.0 μg/kg, respectively The recoveries ranged from 77.0% to 115%, from 73.6% to 104% and from 98.1% to 102%, respectively. The spiked recoveries were the highest The final values were 86.9% ± 15.2% ~ 105% ± 15.2%, 77.5% ± 13.1% ~ 96.4% ± 11.1%, 93.6% ± 1.8% ~ 100% ± 2.5%. Sandy soil spiked at a concentration of 20.0 μg/kg, sediment samples from Taihu Lake at a spiking concentration of 5000 μg/kg Of the soil standard samples were repeated 6 times determination, the standard recoveries were. 63.2% ~ 94.1%, 59.7% ~ 124% 80.1% ~ 115%. The final value of spiked recoveries were 67.9% ± 6.5% ~ 90.9% ± 4.8%, 63.2% ± 5.4% ~ 116% ± 13.8%, 85.8% ± 3.3% ~ 113% ± 8.0%. See Appendix B. 12 Quality Assurance and Quality Control 12.1 blank experiment Analyze at least one laboratory blank every 20 samples or batches (less than 20 samples/batch) and determine their target The value should be below the detection limit of the method. 12.2 Standard Curve The correlation coefficient of the standard curve is ≥0.995. Every 20 samples or batches (less than 20 samples/batch) should be analyzed in a curve of the intermediate concentration point standard solution, the test Set the results and the initial curve at this point the concentration of the relative deviation should be ≤ 20%, or should be re-drawn standard curve. 12.3 Determination of parallel samples Analyze at least one parallel sample per 20 samples or batches (less than 20 samples/batch), and determine the number of single parallel samples The relative deviation of the fruit should be less than 20%. 12.4 Blank spiked sample determination Analyze at least one blank spiked sample every 20 samples or batches (less than 20 samples/batch) at 65% ~ Between 120%. 12.5 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 The concentration of 1 to 5 times the soil, sediment spiked sample recovery rate should be between 60% to 120%. 13 Waste treatment The wastes generated in the experiment should be collected centrally and uniformly stored for delivery to a qualified unit for unified disposal. 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 The name of the compound abbreviation CAS number The detection limit (g/kg) Lower limit of determination (g/kg) 1 2,4,4'-trichlorobiphenyl PCB28 7012-37-5 0.04 0.16 2 2,2 ', 5,5'-tetrachlorobiphenyl PCB52 35693-99-3 0.05 0.20 3 2,2 ', 4,5,5'-Pentachlorobenzene PCB101 37680-73-2 0.04 0.16 4 3,4,4 ', 5-tetrachlorobiphenyl PCB81 70362-50-4 0.05 0.20 5 3,3 ', 4,4'-tetrachlorobiphenyl PCB77 32598-13-3 0.05 0.20 6 2 ', 3,4,4', 5-Pentachlorobenzene PCB123 65510-44-3 0.04 0.16 7 2,3 ', 4,4', 5-Pentachlorobenzene PCB118 31508-00-6 0.04 0.16 8 2,3,4,4 ', 5-Pentachlorobenzene PCB 114 74472-37-0 0.06 0.24 9 2,2 ', 4,4', 5,5'-Hexachlorobiphenyl PCB153 36065-27-1 0.07 0.28 10 2,3,3 ', 4,4'-Pentachlorobenzene PCB105 32598-14-4 0.04 0.16 11 2,2 ', 3,4,4', 5'-Hexachlorobiphenyl PCB138 35065-28-2 0.04 0.16 12 3,3 ', 4,4', 5-Pentachlorobenzene PCB126 57465-28-8 0.04 0.16 13 2,3 ', 4,4', 5,5'-Hexachlorobiphenyl PCB167 52663-72-6 0.04 0.16 14 2,3,3 ', 4,4', 5-Hexachlorobiphenyl PCB 156 38380-08-4 0.04 0.16 15 2,3,3 ', 4,4', 5'-Hexachlorobiphenyl PCB157 69782-90-7 0.04 0.16 16 2,2 ', 3,4,4', 5,5'-Heptachlorobiphenyl PCB180 35065-29-3 0.04 0.16 17 3,3 ', 4,4', 5,5'-Hexachlorobiphenyl PCB169 32774-16-6 0.04 0.16 18 2,3,3 ', 4,4', 5,5'-Heptachlorobiphenyl PCB189 39635-31-9 0.03 0.12

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 No. Compound

content

(Μg/kg) Laboratory relative standard Deviation range (%) Relative standard between laboratories deviation(%) Repeatability r (Μg/kg) Reproducibility limit R (Μg/kg) 1 PCB28 2.00 4.5 ~ 10 5.9 0.39 0.46 20.0 2.6 ~ 6.4 1.9 2.6 2.7 80.0 1.0 ~ 3.6 1.0 4.9 4.9 2 PCB52 2.00 3.9 ~ 8.3 6.9 0.36 0.51 20.0 1.5 ~ 6.2 5.7 2.2 3.3 80.0 0.49 ~ 2.6 1.7 6.2 6.3 3 PCB101 2.00 3.1 ~ 9.0 6.4 0.29 0.29 20.0 3.2 ~ 7.8 4.9 1.9 2.7 80.0 0.84 ~ 2.0 1.0 4.9 5.2 4 PCB81 2.00 4.9 ~ 9.5 14 0.38 0.39 20.0 2.9 ~ 6.1 3.5 2.2 3.0 80.0 0.86 ~ 2.6 1.8 5.7 5.9 5 PCB77 2.00 3.3 ~ 7.9 8.2 0.40 0.58 20.0 3.2 ~ 5.5 1.7 2.0 2.2 80.0 0.75 ~ 3.6 1.8 4.3 7.0 6 PCB123 2.00 2.1 ~ 10 6.6 0.38 0.51 20.0 3.5 ~ 5.3 2.3 2.4 2.5 80.0 0.50 ~ 3.5 2.7 5.6 6.4 7 PCB118 2.00 5.7 ~ 9.6 8.3 0.33 0.54 20.0 3.1 ~ 5.3 4.3 2.2 2.6 80.0 0.82 ~ 4.4 1.3 4.4 5.6 8 PCB114 2.00 4.9 ~ 8.6 2.3 0.35 0.78 20.0 2.8 ~ 4.2 3.8 2.8 3.4 80.0 0.70 ~ 3.8 1.2 3.7 4.0 9 PCB153 2.00 4.4 ~ 7.0 2.3 0.32 0.43 20.0 3.2 ~ 5.3 4.9 2.3 3.6 80.0 0.53 ~ 5.9 1.1 4.3 5.3 10 PCB105 2.00 3.3 ~ 7.9 7.2 0.36 0.53 20.0 2.0 ~ 5.0 4.7 1.8 2.9 80.0 3.1 ~ 5.6 1.7 8.7 8.8 11 PCB138 2.00 6.0 ~ 10 2.5 0.44 0.46 20.0 3.4 ~ 4.9 1.4 2.2 2.2 80.0 3.0 ~ 4.5 2.0 8.1 8.6 No. Compound

content

(Μg/kg) Laboratory relative standard Deviation range (%) Relative standard between laboratories deviation(%) Repeatability limit r (μg/kg) Reproducibility limit R (Μg/kg) 12 PCB126 2.00 3.8 ~ 8.1 2.6 0.35 0.35 20.0 3.4 ~ 6.1 3.6 2.4 2.8 80.0 1.2 ~ 6.2 1.9 6.7 7.4 13 PCB167 2.00 5.0 ~ 9.6 3.0 0.37 0.38 20.0 3.4 ~ 5.3 3.9 2.2 2.9 80.0 2.1 ~ 4.2 1.3 7.4 7.5 14 PCB156 2.00 2.6 ~ 11 8.9 0.36 0.38 20.0 2.5 ~ 5.0 5.8 2.0 3.6 80.0 1.8 ~ 5.2 2.5 7.9 9.1 15 PCB157 2.00 5.9 ~ 8.2 6.0 0.39 0...

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