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HJ 890-2017: Soil and sediment. Determination of polychlorinated biphenyl mixtures. Gas chromatography
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Soil and sediment. Determination of polychlorinated biphenyl mixtures. Gas chromatography
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Basic data | Standard ID | HJ 890-2017 (HJ890-2017) | | Description (Translated English) | Soil and sediment. Determination of polychlorinated biphenyl mixtures. Gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Classification of International Standard | 13.080 | | Word Count Estimation | 18,175 | | Date of Issue | 2017-12-17 | | Date of Implementation | 2018-02-01 | | Quoted Standard | GB 17378.3; GB 17378.5; HJ 494; HJ 613; HJ 783; HJ/T 166 | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 73 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies gas chromatography for the determination of polychlorinated biphenyl compounds in soils and sediments. This standard is applicable to the determination of five kinds of polychlorinated biphenyl industrial products PCB1211, PCB1242, PCB1248, PCB1254 and PCB1260 in soil and sediment. Other PCB products may also be determined by this method if they pass the verification. When the sampling volume is 5g and the constant volume is 1.0 ml, the detection limit of 5 kinds of PCB products is 5��g/kg, and the lower limit of determination is 20��g/kg. | HJ 890-2017: Soil and sediment. Determination of polychlorinated biphenyl mixtures. Gas chromatography
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(Soil and sediment - Determination of PCB mixtures - Gas chromatography)
People's Republic of China national environmental protection standards
Soil and sediment - Determination of PCB mixtures
Gas chromatography
Soil and sediment-Determination of polychlorinated biphenyl
mixtures-Gas chromatography
2017-12-17 Published
2018-02-01 implementation
Ministry of Environmental Protection released
i directory
Foreword .ii
1 scope of application .1
2 Normative references .1
3 Terms and definitions .1
4 method principle .2
5 Interference and elimination .2
6 Reagents and materials .2
7 instruments and equipment .3
8 samples .4
9 Analysis steps .6
10 Results Calculation and Presentation 6
11 precision and accuracy 8
12 Quality Assurance and Quality Control .9
13 Waste Management 9
Appendix A (informative) method of precision and accuracy ..10
Appendix B (informative) standard sample to confirm the column chromatogram.11.11
Appendix C (Informative) Recommended Feature Recognition Peaks .12
Foreword
In order to carry out "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, regulate soil and sediment
Determination of PCBs in industrial mixtures, the development of this standard.
This standard specifies the determination of soil and sediment in the PCB by gas chromatography.
This standard Appendix A, Appendix B and Appendix C are informative appendix.
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. National Environmental Analysis Test Center.
This standard verification unit. Hunan Provincial Environmental Monitoring Center, Xiangtan City Environmental Monitoring Station, Wuxi City Environmental Monitoring Center, the Soviet Union
State Environmental Monitoring Center, Shandong Provincial Analysis and Testing Center and Beijing Jinxiu earth technology testing and analysis center.
This standard MEP approved on December 17,.2017.
This standard since February 1,.2018 implementation.
This standard is interpreted by the MEP.
1 soil and sediment polychlorinated biphenyls Determination of gas chromatography
Warning. The organic solvents and reagents used in this method have some toxicity. The experimental operation should be carried out in a fume hood and press
Provisions on wearing protective equipment, to avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of soil and sediment in the PCB by gas chromatography.
This standard applies to soil and sediment PCB1221, PCB1242, PCB1248, PCB1254 and PCB1260
A total of 5 kinds of PCBs determination of industrial products, other PCBs industrial products through the verification can also be measured using this method.
When the sample volume is 5 g and the volume of constant volume is 1.0 ml, the detection limits of the 5 PCBs industrial products by this method are
5 μg/kg, the lower limit of determination of 20 μg/kg.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this book
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 166 Soil Environmental Monitoring Technical Specifications
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
PCBs congeners
Polychlorinated biphenyls (PCBs), also known as chlorinated biphenyl, biphenyl ring is a hydrogen atom is replaced by a class of chlorine atoms formed
Synthetic organic compounds, from a chlorinated biphenyl to 10 chlorinated biphenyl, a total of 209 kinds of compounds, although the molecular formula of these compounds are different,
But there is a similar chemical structure, known as homologues.
3.2
Feature recognition peak diagnostic peak
Each polychlorinated biphenyl industrial product has between 70 and 80 identifiable peaks in the GC/ECD spectrum. Some of these chromatograms
Peak abundance larger, better separation, and the relative position and intensity of the surrounding peaks have obvious characteristics, easy to identify, known as special
Sign recognition peak.
24 method principle
PCBs in soils and sediment samples were extracted with organic solvents and the extract was concentrated with concentrated sulfuric acid and purified on a silica gel column.
After volume determination by gas chromatography, electron capture detector detection. Retention time and peak shape of the sample peak passed the standard
Qualitative comparison of products, select 5 to 10 characteristics of identification peaks, with external standard quantitative.
5 Interference and elimination
Soil and sediments may exist in the BHC, organophosphorus pesticides, oxygenated compounds will not interfere with the determination of PCBs.
DDE, DDD and DDE at concentrations greater than 5 μg/kg interfere with quantification and should be avoided in the selection of characterization peaks
The peak time of the thing.
6 Reagents and materials
Unless otherwise stated, analytical grade reagents that meet national standards are used.
6.1 Experimental water
In a 1 L separatory funnel by adding 500 ml of deionized or distilled water and 100 ml of n-hexane, shaking 10 min standing
After the layer, the aqueous phase is released and stored in brown glass bottles for later use. Hexane can be reused 3 times.
6.2 n-Hexane (C6H14). pesticide residues, or PCBs were not detected after 100-fold concentration.
6.3 Dichloromethane (C2H2Cl2). pesticide grade, or 50 times concentrated PCBs were not detected.
6.4 acetone (C3H6O). pesticide residues, or PCBs were not detected.
6.5 Absolute ethanol (C2H5OH). HPLC grade, PCBs were not detected after 100 times concentration.
6.6 Nitric acid. ρ (HNO3) = 1.42 g/ml.
6.7 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml.
6.8 Potassium hydroxide (KOH). Purity 85%.
6.9 Sodium bicarbonate (NaHCO3).
6.10 Anhydrous sodium sulfate (Na2SO4).
Muffle furnace 450 ℃ burning 4 h, remove and put in a clean dryer standby.
6.11 Dichloromethane - n-hexane mixed solution. 1 1.
Mix with methylene chloride (6.3) and n-hexane (6.2) at a volume ratio of 1. 1.
6.12 nitric acid solution. ρ (HNO3) = 1 mol/L.
Take 6.9 ml of nitric acid (6.6), add 100 ml of water and mix well.
6.13 sulfuric acid solution. 1 9.
Take 10 ml of sulfuric acid (6.7), add 90 ml of water and mix.
6.14 Potassium hydroxide solution. ρ (KOH) = 0.05 g/ml.
Take 59 g potassium hydroxide (6.8) dissolved in a small amount of water, diluted to 1 L.
6.15 Potassium hydroxide - ethanol solution. 1 mol/L.
Weigh 33 g of potassium hydroxide (6.8) added to 500 ml of anhydrous ethanol (6.5), dissolved and mixed.
6.16 Sodium bicarbonate solution. ρ (NaHCO3) = 0.02 g/ml.
3 Weigh 2 g of sodium bicarbonate (6.9), dissolve in 100 ml of water and mix well.
6.17 PCB standards
PCB1221, PCB1242, PCB1248, PCB1254, PCB1260 and other commercial PCB standards.
Note. Some of the commercially available PCB series of standard samples of methanol solvent, methanol and n-hexane, petroleum ether and other non-polar solvents can not be any ratio
Dilution ratio should be greater than 15. 1.
6.18 PCB stock standard solution. ρ = 5.00 mg/L.
Dilute PCB standards with n-hexane (6.2) (6.17). Dark sealed in a standard sample bottle cold, at least
Save for 6 months.
6.19 copper wire (beads or powder).
Before use soaked in nitric acid solution (6.12) to remove the surface oxide layer, washed with water until neutral and then with acetone
(6.4) and n-hexane (6.2) three times.
6.20 Silica. 75 μm ~ 150 μm (200 mesh ~ 100 mesh).
130 ℃ activated 16 h, placed in a clean dryer standby.
6.21 alkaline silica gel.
Take silica gel (6.20) 98 g, add potassium hydroxide solution (6.14) 40 ml, shake well, into a powder, after bottling
Store in the dryer.
6.22 acidic silica gel.
Take silica gel (6.20) 56 g, add sulfuric acid (6.7) 44 g, shake well, into a powder, stored in a dry bottle
In the device.
6.23 Compound Silica Column. The following methods can be used to fill, you can also buy commercially available products.
Place a small glass wool (6.27) on the bottom of the column (7.6), add 40 ml of n-hexane (6.2) and fill in with water
1 g of sodium sulfate (6.10), 1 g of silica gel (6.20), 3 g of basic silica gel (6.21), 1 g of silica gel (6.20)
8 g, silica gel (6.20) 1 g, anhydrous sodium sulfate (6.10) 1 g. Release n-hexane to make it just above the silica gel column
Anhydrous sodium flush, stand-by.
6.24 Silica gel column. Commercial column, 1000 mg/6 ml, polyethylene or polypropylene column.
6.25 Diatomaceous earth. 75 μm to 150 μm (200 mesh to 100 mesh).
Muffle furnace 450 ℃ burning 4 h, remove and put in a clean dryer standby.
6.26 quartz sand. 150 μm ~ 830 μm (100 mesh ~ 20 mesh).
Muffle furnace 450 ℃ burning 4 h, remove and put in a clean dryer standby.
6.27 clean glass wool.
6.28 high purity nitrogen. purity ≥ 99.999%.
7 instruments and equipment
7.1 Gas Chromatograph. with split/splitless inlet, temperature programmed function, and electron capture detector.
7.2 Column. Quartz capillary column.
Analytical column. non-polar, 30 m 0.25 mm 0.25 μm, 100% polymethylsiloxane fixative, or other equivalent chromatographic
column;
Confirm column. medium polarity, 30 m 0.25 mm 0.25 μm, 14% cyanopropylphenyl-86% dimethylpolysiloxane fixative,
4 or other equivalent column.
7.3 Extraction device. Soxhlet extraction device, automatic Soxhlet extractor, accelerated solvent extractor or other equivalent extraction
Device.
7.4 Concentration device. nitrogen blowing concentrator, rotary evaporator, KD concentrator, parallel centrifugal evaporator or other performance equivalent
device of.
7.5 glass reflow device.
7.6 Column. 300 mm long, 10 mm ~ 15 mm ID, glass column with Teflon piston on the bottom.
7.7 Analytical Balance. Feel 0.01 g.
7.8 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 water bodies were collected according to the relevant requirements of HJ 494
Samples of the material, in accordance with the relevant requirements of GB 17378.3 collected marine sediment samples. After the sample is collected, it is protected from light at 4 ° C
Storage, within 30 d to complete the extraction, within 40 d to complete the analysis of the extract.
8.2 Preparation of samples
Remove the foreign material from the sample and weigh 5 g (accurate to 0.01 g) into the round bottom flask. When using Soxhlet extraction,
The sample was added an appropriate amount of anhydrous sodium sulfate (6.10), ground into a sand-like, into the extraction tube. For the higher sulfur deposition
Add sample amount of copper powder (6.19). When using pressurized fluid extraction, add appropriate amount of diatomaceous earth (6.25) to the sample and mill
To block-free, into the extraction cell. For high sulfur sediment samples add appropriate amount of copper powder (6.19).
Preparation of air-dried soil and sediment samples, respectively, according to HJ/T 166 and GB 17378.3 related parts to operate.
8.3 Determination of moisture
Weigh the sample at the same time, according to HJ 613 determination of soil samples dry matter content, measured in accordance with GB 17378.5 sediment
Sample moisture content.
8.4 Preparation of test specimens
8.4.1 Extraction
8.4.1.1 Lye reflux
In a round bottom flask containing the sample, add potassium hydroxide - ethanol solution (6.15) 50 ml, boiling water bath reflux 1 h, will
The supernatant was transferred to a separatory funnel pre-filled with 100 ml of n-hexane (6.2) and 500 ml of water and the alkaline residue was eluted with 20 ml
Ethanol (6.5) was washed three times and combined into a separatory funnel. After adjusting the solution to neutral with sulfuric acid solution (6.13), extract for 5 min
~ 10 min, stand still stratified, discard the water sample.
8.4.1.2 Pressurized fluid extraction
Put the extraction tank and the receiving bottle correspondingly, extractant is dichloromethane-n-hexane mixed solution (6.11), extraction temperature
5100 ℃, heating time 5 min, extraction time 5 min, extraction cycle 2 times, extraction nitrogen purge 60 s. Or according to HJ 783
Set and optimize extraction conditions.
8.4.1.3 Soxhlet extraction and automatic Soxhlet extraction
The cartridge into the Soxhlet extraction tube, connect the extraction device, turn on the heater, control the speed, dichloromethane -
The mixed solution of alkanes (6.11) was refluxed for 16 h. Or in accordance with the extraction conditions optimized for Soxhlet extraction 4 h ~ 6 h.
8.4.2 Purification
8.4.2.1 sulfuric acid purification
The extraction solvent conversion solvent for n-hexane, add about 5 ml ~ 10 ml of sulfuric acid (6.7), shake for a moment after standing layered, abandoned
The sulfuric acid phase is removed and the sulfuric acid wash is repeated until the sulfuric acid phase is colorless. Add 100 ml sodium bicarbonate solution (6.16), shake 2 min,
Stand stratification, discard the water phase and repeat until the water sample pH is neutral. In a glass funnel, first load a small amount of glass
Wool (6.27), then about 10 g of anhydrous sodium sulfate (6.10) and 15 ml of n-hexane (6.2), discard
detergent. The extract was added and collected in a pear-shaped flask. Concentrate to about 2 ml with suitable concentration equipment, transfer to scale test
Tube.
8.4.2.2 silica gel column purification
In column (7.6), install a small amount of glass wool (6.27) first. Add 20 ml of n-hexane (6.2) beforehand
Add 3.0 g of silica gel (6.20) to the cup, stir, pour into the column and wash the beaker with a small amount of n-hexane (6.2)
Into the column, emit excess n-hexane 0.5 cm above the silica gel layer, add a small amount of anhydrous sodium sulfate (6.10). Will be thick
The reduced sample is added to the column and the graduated tube is washed with 2 ml of n-hexane (6.2) and added to the column. Will be 40 ml
Hexane (6.2) was added to the dropping funnel, and the dropping funnel was connected to the column, the flow rate was adjusted to about 1 drop per second,
Collect with a pear-shaped bottle.
For the substrate is relatively clean samples can also be purified using a commercial silica gel column (6.24). Use 10 ml before use
Clean the silica gel column (6.24) with n-hexane (6.2). When the liquid level is 1 mm ~ 2 mm above the packing layer, concentrate
Quantitatively transfer the sample to the purification column and rinse with 12 ml of n-hexane (6.2) to control the appropriate flow rate and receive with a graduated test tube.
8.4.2.3 desulfurization
For sediment samples containing elemental sulfur, copper wire (beads) (6.19) were placed in the eluent to desulfurize and the copper surface became black
After treatment with a nitric acid solution (6.12) to the surface of the copper metal luster, followed by water, acetone (6.4) and n-hexane (6.2)
After washing, put it into the sample again and repeat several times until the surface of the copper does not turn dark.
8.4.3 concentrated volume
The eluate was concentrated using a concentrator (7.4) to about 2 ml, transferred to a graduated tube and concentrated to a final volume of 1.0
ml, test.
Note. For soil samples with higher concentrations of PCBs or less interference, the extract can be directly transferred to n-hexane and concentrated to 2 ml left
Right, all transferred to a column of silica gel (6.23) with 100 ml of n-hexane (6.2) elution, the eluate was collected, the volume was concentrated to 1.0 ml
After testing.
68.5 Preparation of blank samples
Replace the actual sample with quartz sand (6.26) and prepare a blank sample according to the same procedure as sample preparation (8.4).
9 Analysis steps
9.1 Instrument reference conditions
Inlet temperature. 225 ° C; splitless injection, split after 1.0 min, split ratio 50. 1; column pressure. 110 kPa; column
Temperature. 100 ° C for 2 min, 15 ° C/min to 160 ° C, and then 5 ° C/min to 300 ° C for 10 min;
Injection volume. 1.0 μl; make-up gas (makeup gas). 50 ml/min; electron capture detector (ECD) temperature. 300 ° C.
Confirm the column temperature. 60 ℃ for 2 min, 30 ℃/min heating to 160 ℃, then 3 ℃/min heating to 260 ℃,
Hold for 7 min.
9.2 calibration curve established
The standard stock solution of PCBs (6.18) was diluted with n-hexane to give a concentration of 0.05 μg/ml, 0.10 μg/ml,
0.25 μg/ml, 0.50 μg/ml, 1.00 μg/ml standard series of solutions. According to the instrument reference conditions (9.1) for analysis,
Get the chromatogram of different concentrations, the concentration of each standard series of solutions as the abscissa, with its corresponding feature to identify the peak area
And for the vertical axis, draw the calibration curve.
When the sample PCBs concentration is high or interference is not obvious, the concentration of each standard series of solutions can be abscissa to
PCBs total peak area and the vertical axis, the establishment of the calibration curve.
9.3 Sample Determination
The prepared sample (8.4) is measured according to the same instrument analysis conditions as the calibration curve (9.2).
9.4 Blank test
The prepared blank sample (8.5) is subjected to the same instrument analysis conditions as the sample measurement (9.3).
10 Results Calculation and Presentation
10.1 Qualitative analysis
Optimize the instrument conditions, respectively, the determination of PCB standards (PCB1221, PCB1242, PCB1248, PCB1254
And PCB 1260) and the actual sample, comparing the standard spectrum with the sample spectrum, identifying the peak retention time and relative
Strength, to determine the type of PCBs pollution. For mixed contamination, the sample chromatogram peak will cover low-chlorinated, medium-chlorinated and high-chlorinated
Generational regions, low profile of sample and standard spectra, can be characterized by means of GC/MS with PCB1242/PCB1254 (1.
1) as a standard, quantitative. The chromatograms of PCBs standard samples on the analytical column are shown in Figure 1.
Note. See Appendix B for column chromatograms.
7 Note 1. The same compound in different products in different content, when the chromatographic conditions fixed, the same compound peak retention time of the same.
Note 2. The location of 7 kinds of indicative PCBs (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, PCB180)
In Figure 1 were identified.
Figure 1 PCBs standard sample chromatogram on the analytical column
10.2 Quantitative analysis
After determining the type of PCBs contamination, the corresponding standard sample is used and the sum of the peak areas identified by the characteristics is determined by the external standard method
Quantitative. When selecting a set of signature recognition peaks for quantitation, try to identify the front, middle and back regions of PCBs homologues
Choose different chlorine content of the peak, and to avoid DDE, DDD and DDT and other interferents. The number of characteristic recognition peaks is 5 to 10
A suitable, see Appendix C.
When the concentration of PCBs in the sample exceeds the calibration curve range, dilute it appropriately.
10.3 Results Calculation
10.3.1 Calculation of soil sample results
PCBs in soil samples W1 (μg/kg) calculated according to equation (1).
8 Where. W1 - PCBs in the sample content, μg/kg;
ρ-- concentration of PCBs in the sample, μg/ml;
V-- volume of sample volume, ml;
M - sample weight, g;
Wdm - Sample dry matter content,%;
D - dilution factor.
10.3.2 Calculation of Sediment Sample Results
PCBs in sediment samples W2 (μg/kg) according to equation (2) Calculated.
Where. W2 - PCBs in the sample content, μg/kg;
ρ-- concentration of PCBs in the sample, μg/ml;
V-- volume of sample volume, ml;
M - sample weight, g;
W-- sample moisture content,%;
D - dilution factor.
10.4 results show
When the test result is less than 100 μg/kg, keep to the whole digit; when the test result is greater than or equal to 100 μg/kg, keep 3
Effective digits.
11 precision and accuracy
11.1 precision
Six laboratories tested PCBs in soils and sediments at 218 μg/kg, 1.09 mg/kg and 5.46 mg/kg, respectively
Uniform samples were measured 6 times repeatedly. the relative standard deviation in the laboratory ranged from 7.9% to 12%, 3.8% to 9.0%
4.5% ~ 8.7%. The relative standard deviations of laboratory were 1.7%, 2.7% and 2.9% respectively. The repeatability limits were 56 μg/kg,
0.20 mg/kg, 0.90 mg/kg; reproducibility limits were. 59 μg/kg, 0.22 mg/kg, 0.98 mg/kg, see Appendix A
Table A.1.
11.2 Accuracy
Six laboratories separately measured three spiked samples of PCB1242 in soil and sediment,
The standard concentrations were 218 μg/kg, 1.09 mg/kg and 5.46 mg/kg, respectively. Repeated determination of each sample 6 times, the standard recovery rate
(1)
(2)
The results showed that the final recoveries were 85.5% -89.5%, 85.9% -93.5% and 89.3% -96.7% respectively, and the final recoveries were 87.4% ±
3.3%, 90.3% ± 5.4%, 92.9% ± 5.6%, see Appendix A Table A.2.
12 Quality Assurance and Quality Control
12.1 blank
A laboratory blank is determined for every 20 samples or batches (less than 20 samples/batch). The blank result should be less than the square
Law detection limit.
12.2 Calibration curve
Correlation coefficient of calibration curve r > 0.995. After each analysis of 15 to 20 samples, determine the standard series of intermediate concentration point,
Measurement results and the standard value of the relative error within ± 25%, the calibration curve can continue to use, or need to re-establish the calibration
curve.
Note. When the calibration curve is wide, it can be fitted by the quadratic equation.
12.3 Parallel samples
At least one sample should be selected for parallel determination every 20 samples or batches (less than 20 samples/batch), as opposed to
Deviations should be within 35%.
12.4 Matrix spiked samples
At least one sample should be selected for matrix spiking experiments every 20 samples or batches (less than 20 samples/batch)
The matrix recovery rate should be 70% ~ 130%.
13 Waste treatment
Organic waste and waste generated from the experiment should be collected in a centralized manner and stored in a centralized manner, and sent to a qualified unit for unified disposal.
Appendix A.
(Informative)
The precision and accuracy of the method
Table A.1 Summary of Methods Precision (n = 6)
Compound name
content
(Mg/kg)
Laboratory relative standard
Quasi-deviation
(%)
Relative between laboratories
standard deviation
(%)
Repeatability r
(Mg/kg)
Reproducibility limit R
(Mg/kg)
PCB1242 0.218 7.9 ~ 12 1.7 0.056 0.059
PCB1242 1.09 3.8 ~ 9.0 2.7 0.20 0.22
PCB1242 5.46 4.5 ~ 8.7 2.9 0.90 0.98
Table A.2 Method Quasi-summary (n = 6)
Compound Name Sample Type
Scalar
(Mg/kg)
Spike recovery range
(%)
Spike recovery final value
(%)
PCB1242 Soil 0.218 85.5 ~ 89.5 87.4 ± 3.3
PCB1242 Lake sediments 1.09 85.9-93.5 90.3 ± 5.4
PCB1242 contaminated soil 5.46 89.3 ~ 96.7 92.9 ± 5.6
Appendix B
(Informative)
Standard sample Confirm the column chromatogram
Figure B.1 PCBs standard sample in the confirmation column chromatogram
PCB1242
PCB1248
PCB1254
PCB1260
PCB1221
Appendix C
(Informative)
Recommended Feature Recognition Peaks
Figures C.1 to C.5 are based on 100% polymethylsiloxane capillary column analysis results, under the same analytical conditions,
The same numbered peaks have the same retention time. According to Table C.1 recommended feature recognition peak select 5 to 10 into
Row quantitative calculation.
Figure C.1 PCB 1221 feature recognition peaks
Figure C.2 PCB 1242 feature recognition peaks
110.4
111.6
112.2
112.8
113.4
114.6
115.2
115.8
116.4
mV
10 12 14 16 18 20 22 24 26 min
Figure C.3 PCB 1248 Feature Recognition Peak
Figure C.4 PCB 1254 Feature Recognition Peaks
Figure C.5 PCB 1260 features identification peaks
Table C.1 Recommended Feature Recognition Peaks
Peak number
PCB
PCB
PCB
PCB
PCB
1 √
2 √
3 √
4 √ √
6 √ √
7 √ √
9 √ √
14 √ √ √
15 √ √ √
16 √ √ √
17 √ √ √
20 √ √ √
21 √ √ √
22 √
23 √
24 √ √ √
25 √ √
26 √ √
32 √ √ √
33 √ √ √
34 √ √ √
37 √ √
48 √ √ √
54 √ √ √
58 √ √ √
59 √ √
65 √
66 √ √
70 √
7...
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