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Ambient air. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method
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Basic data | Standard ID | HJ 902-2017 (HJ902-2017) | | Description (Translated English) | Ambient air. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 20,260 | | Date of Issue | 2017-12-14 | | Date of Implementation | 2018-03-01 | | Quoted Standard | HJ 194; HJ 691 | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 71 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies gas chromatography-mass spectrometry for the determination of polychlorinated biphenyls in ambient air. This standard applies to ambient air gas and particulate matter PCB 8, PCB 18, PCB 28, PCB 44, PCB 52, PCB 66, PCB 77, PCB 81, PCB 101, PCB 105, PCB 114, PCB 118, PCB 123, PCB 126, PCB 128, PCB 138, PCB 153, PCB 156, PCB 157, PCB 167, PCB 169, PCB 170, PCB 180, PCB 187, PCB 189, PCB 195, and PCB 206 total 27 types |
HJ 902-2017: Ambient air. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Ambient air - Determination of PCBs - Gas chromatography - mass spectrometry)
People's Republic of China national environmental protection standards
Ambient air - Determination of PCBs
Gas chromatography - mass spectrometry
Ambient air-Determination of polychlorinated biphenyls
-Gas chromatography/mass spectrometry method
2017-12-14 Published
2018-03-01 implementation
Ministry of Environmental Protection released
Directory
Preface ... i
1 Scope ... 1
2 Normative references ... 1
3 method principle ... 1
4 Interference and elimination ... 1
5 Reagents and materials ... 1
6 Instruments and Equipment ... 3
7 samples ... 5
8 Analysis step ... 6
9 Calculation and Expression of Results ... 8
10 Precision and accuracy ... 10
11 Quality Assurance and Quality Control ... 10
12 Waste treatment ... 11
Appendix A (Normative) Detection limit and lower limit of the method ... 12
Appendix B (informative) List of compounds ... 13
Appendix C (informative) Determination of the target compound reference parameters ... 15
Appendix D (informative) method of precision and accuracy ... 16
i Foreword
In order to implement the Law of the People's Republic of China on Environmental Protection and the Law of the People's Republic of China on Prevention and Control of Atmospheric Pollution,
Habitat to protect human health and regulate the ambient air Determination of PCBs, the development of this standard.
This standard specifies the determination of polychlorinated biphenyls in the air by gas chromatography - mass spectrometry.
Appendix A of this standard is a normative appendix, Appendix B ~ Appendix D is an informative annex.
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. Shenyang Environmental Monitoring Center Station.
This standard verification unit. Jiangsu Province Environmental Monitoring Center, Henan Province Environmental Monitoring Center, Liaoning Province, environmental monitoring experiments
Heart, Dalian Environmental Monitoring Center, Anshan Environmental Monitoring Center Station and Shenyang Environmental Protection Bureau Tiexi Branch Environmental Monitoring Station.
This standard MEP approved on December 14,.2017.
This standard since March 1,.2018 into effect.
This standard is interpreted by the MEP.
1 Ambient air - Determination of polychlorinated biphenyls - Gas chromatography - mass spectrometry
Warning. The solvents and reagents used in this method are toxic. The experimental procedure should be carried out in a fume hood.
Wear protective equipment as required and avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of polychlorinated biphenyls in the air by gas chromatography - mass spectrometry.
This standard applies to ambient air and particulate matter in the PCB 8, PCB 18, PCB 28, PCB 44, PCB 52,
PCB 66, PCB 77, PCB 81, PCB 101, PCB 105, PCB 114, PCB 118, PCB 123, PCB 126,
PCB 128, PCB 138, PCB 153, PCB 156, PCB 157, PCB 167, PCB 169, PCB 170, PCB 180,
PCB 187, PCB 189, PCB 195 and PCB 206 Determination of a total of 27 kinds of PCBs. See Appendix B for details.
When the sampling volume is 350 m3 (standard state), the volume of concentrated volume is 1.0 ml, this method measures 27 kinds of polychlorinated
The detection limit of benzene was 0.02 ng/m3 ~ 0.04 ng/m3, and the lower limit of determination was 0.08 ng/m3 ~ 0.16 ng/m3. See Appendix A for details.
2 Normative references
This standard references the following documents in the terms. For undated references, the effective version applies
This standard.
HJ 194 Manual Air Quality Monitoring Technical Specifications
HJ 691 Environmental airborne semi-volatile organic compounds sampling techniques
3 method principle
A large flow sampler is used to collect the filters and polyurethane foam from the PCBs in ambient air and particulate matter
(PUF), extracted with ether-n-hexane mixed solvent, the extract was concentrated, purified, and separated by gas chromatography-mass spectrometry
Detection, retention time and characterization of ion abundance ratio qualitative, internal standard method.
4 Interference and elimination
Other organic matter in the sample may interfere with the determination, the choice of sulfuric acid, magnesium silicate chromatography column or a composite silica gel column
Methods to remove interference, see 7.3.3.
5 Reagents and materials
Unless otherwise specified, the analysis of analytical reagents are used in line with national standards of analytical chemistry, experimental water is freshly prepared
Pure water.
5.1 acetone (C3H6O). pesticide grade.
5.2 n-hexane (C6H14). pesticide residues.
5.3 ether (C4H10O). Chromatography.
5.4 Dichloromethane (CH2Cl2). pesticide grade.
25.5 Anhydrous Sodium Sulfate (Na2SO4). Bake at 400 ℃ in muffle furnace for 4 hours before use, after cooling,
Sealed in the preservation.
5.6 Sodium chloride (NaCl). Bake in a muffle furnace at 400 ° C for 4 h before use, cool and seal in a milled glass jar
save.
5.7 sulfuric acid (H2SO4). ρ = 1.84 g/cm3, excellent grade pure.
5.8 ether - n-hexane mixed solvent. 1 9, Pro use now.
5.9 Diethyl ether - n-hexane mixed solvent. 6 94, Pro use now.
5.10 Sodium chloride solution. ρ = 50 g/L.
Weigh 50.0 g of sodium chloride (5.6) in a beaker, add water to dissolve and dilute to 1000 ml, mix well, use now with.
5.11 p-terphenyl - D14. purity of 98% or more.
Alternatives are analyzed, and other deuterated species or analogues not found in the sample can be used. Can be purchased directly from the market with a permit standard
Solution.
5.12 Analysis Alternative stock solution. ρ =.2000 μg/ml.
Weigh p-terphenyl-D14 (5.11) about 0.1 g, accurate to 0.1 mg in 50 ml volumetric flask, with a small amount of dichloromethane
After dissolving alkane (5.4), dilute with n-hexane (5.2) and mix well.
5.13 Analysis Substitute intermediate solution. ρ = 40.0 μg/ml.
Pipette 500 μl of stock solution (5.12) into a 25 ml volumetric flask and dilute to volume with n-hexane (5.2) and mix well.
5.14 Analysis Alternatives to use. ρ = 2.00 μg/ml.
Pipette 100 μl of stock solution (5.12) into a 100 ml volumetric flask and dilute with n-hexane (5.2) and mix well.
5.15 decablol (DCBP). purity of 99% or more.
Sampling alternatives, other deuterations or analogues not found in the sample can also be used. Can be purchased directly from the market with a permit standard
Solution.
5.16 Sampling alternatives stock solution. ρ =.2000 μg/ml.
Weigh deca-biphenyl (5.15) about 0.1 g, accurate to 0.1 mg in a 50 ml volumetric flask with a small amount of methylene chloride (5.4)
After dissolving, dilute with n-hexane (5.2) and mix well.
5.17 sampling alternative intermediate solution. ρ = 100 μg/ml.
Pipette 500 μl of stock solution (5.16) into a 10 ml volumetric flask and dilute to volume with n-hexane (5.2) and mix well.
5.18 sampling alternative solution. ρ = 2.00 μg/ml.
Pipette 500 μl of sample replacement intermediate solution (5.17) into a 25 ml volumetric flask and dilute to volume with n-hexane (5.2) and mix well.
5.19 Internal standard stock solution. ρ = 750 μg/ml.
Direct purchase of a certified public standard solution, with Philippine-D10, 䓛 -D12 or other deuterium-substituted PAHs.
5.20 Internal standard intermediate solution. ρ = 75.0 μg/ml.
Pipette 1.00 ml internal standard stock solution (5.19) in a 10 ml volumetric flask, dilute to volume with n-hexane (5.2) and mix well.
5.21 Internal standard solution. ρ = 15.0 μg/ml.
Pipette 2.00 ml of the internal standard intermediate solution (5.20) in a 10 ml volumetric flask, dilute to volume with n-hexane (5.2) and mix well.
5.22 standard stock solution. ρ = 10.0 μg/ml.
Direct purchase of 28 licensed PCBs certified standard solution containing IUPAC component number PCB 8,
PCB 18, PCB 28, PCB 44, PCB 52, PCB 66, PCB 77, PCB 81, PCB 101, PCB 105, PCB 114,
3PCB 118, PCB 123, PCB 126, PCB 128, PCB 138, PCB 153, PCB 156, PCB 157, PCB 167,
PCB 169, PCB 170, PCB 180, PCB 187, PCB 189, PCB 195, PCB 206, and DCBP, see attached
Record B. 4 ℃ below the sealed storage, or reference standard solution preservation conditions.
5.23 standard solution. ρ = 1.00 μg/ml.
Pipette 1.00 ml standard stock solution (5.22) and 250 μl analysis alternative intermediate solution (5.13), respectively, in 10 ml
In a volumetric flask, dilute with n-hexane (5.2) and mix well.
5.24 Dodecafluorotriphenylphosphine (DFTPP) stock solution. ρ = 100 μg/ml.
Can be purchased directly from the market certified standard solution can also be prepared with standard materials, the solvent is methylene chloride.
5.25 Dopentafluorophenylphosphine (DFTPP) solution. ρ = 4.0 μg/ml.
Pipette 1.00 ml of decafluorotriphenylphosphine (5.24) in a 25 ml volumetric flask, dilute with dichloromethane (5.4) and mix well.
Note. All solutions (5.12 ~ 5.25) are transferred to a screw-capped glass bottle with Teflon liner, refrigerated at 4 ℃, sealed dark
save.
5.26 composite silica gel column
The bottom of the column filled with glass wool (5.32), from the bottom were filled with anhydrous sodium sulfate 4 g, silica gel 0.9 g, 2% KOH
Silica gel 3 g, silica gel 0.9 g, 44% silica gel 4.5 g, 22% silica gel 6 g, silica gel 0.9 g, 10% silver nitrate silica gel 3 g,
The top is anhydrous sodium sulfate 6 g. Can also be purchased directly commodity column.
5.27 Magnesium silicate. 150 μm ~ 250 μm (100 mesh ~ 60 mesh), activated at 130 ℃ for 18 h before use,
After cooling in the desiccator, transfer to a glass bottle and seal it for preservation.
5.28 Quartz/glass fiber filter. according to the sampling head to select the appropriate size, the filter on the 0.3 μ m standard particle retention efficiency
Not less than 99%. Before use in the muffle furnace 400 ℃ heating 5 h above, after cooling, stored in the filter box, to ensure that the filter at
Sampling before and after not contaminated, and in the sample before the flat state.
5.29 Polyurethane Foam (PUF). polyether type, with a density of 22 mg/cm3 ~ 25 mg/cm3, cut and grown 70 mm, straight
Cylindrical diameter of 45 mm to 65 mm (length, diameter as determined by the specifications of the glass sampling cartridge). Use heat before use
Water scald, and then repeatedly rub into warm water, drained, with acetone (5.1) three times, into the Soxhlet extractor
(6.4), followed by reflux extraction with acetone (5.1), ether-n-hexane mixed solvent (5.8) for 16 h,
Times fresh diethyl ether - n-hexane mixed solvent (5.8) reflux extraction, removed after the nitrogen (5.30) flow drying (also available
Vacuum dried at room temperature for 2 h ~ 3 h), into the glass sample tube (6.3.2) sealed in a suitable container.
5.30 Nitrogen. Purity ≥99.999%.
5.31 Helium. Purity ≥99.999%.
5.32 glass wool. Before use with dichloromethane (5.4) reflux extraction 2 h ~ 4 h, dried and sealed.
6 instruments and equipment
6.1 Gas Chromatography - Mass Spectrometer. Split/Splitless Inlet, Temperature Programmable, Electron Impact Ionization Source.
6.2 Column. Low Loss Quartz Capillary Column, 30 m (length) × 0.25 mm (ID) × 0.25 μm (film thickness),
The stationary phase is 5% phenyl 95% dimethylpolysiloxane, or other equivalent low-loss chromatography column.
6.3 Sampling device
6.3.1 Large flow sampler. to meet the HJ 691 requirements, with automatic accumulation of sampling volume, automatically convert the standard sampling volume
Function, and automatic timer, power off again and automatically compensate for voltage fluctuations, changes in resistance caused by changes in flow function.
4 With the filter and adsorbent installed, the sampler load flow should be 250 L/min for high flow rates,
The operating point flow rate is 225 L/min; for oversized flow sampling, the sampler load flow should be able to reach 900 L/min,
For the point of flow of 800 L/min.
6.3.2 Sampling head. to meet the HJ 691 requirements, by the filter holder and the sampling sleeve sleeve of two parts, as shown in Figure 1. Sampling head
The material selection of PTFE or stainless steel and other non-adsorption of organic materials. Filter clip includes filter ring, filter and filter
Film stent. Sampling tube Sleeve equipped with a glass sampling cylinder, the bottom of the sampling cylinder supported by a stainless steel mesh, the adsorption cartridge
The material is PUF (5.29). Sampling tube with silicone rubber seal fixed between the filter holder and the suction pump.
1-gas flow inlet; 2-filter holder; 3- sampling sleeve
Barrel; 4-gas outlet; 5-filter ring; 6-
Silicone rubber ring; 7-filter; 8- stainless steel mesh;
9-filter holder; 10-glass sampling cartridge.
Figure 1 sampling head schematic
Soxhlet extractor. 500 ml or 1000 ml. Other performance extraction devices may also be used.
6.5 Glass column. 300 mm long, 15 mm to 20 mm ID, glass column with Teflon piston on the bottom.
6.6 Concentration device. Rotary evaporation apparatus, nitrogen blowing concentrator or other performance-equivalent equipment.
6.7 solid phase extraction device.
6.8 separatory funnel. 60 ml.
6.9 General laboratory equipment commonly used.
57 samples
7.1 Sample Collection
7.1.1 Ambient air samples
According to HJ 194 and HJ 691, sampling points should be laid for the determination of meteorological parameters and sample collection.
Add 125 μl Sampling Reagent Solution (5.18) to the PUF before sampling in the field and place for 1 h before installing
Filter clips, sampling cartridge sleeve, connected to the sampler, adjust the sampling flow, start sampling. Remove the filter after sampling, sampling
Fold the dust inwards, fold out the glass sampling tube, wrap it with aluminum foil, and put it into a storage box to seal it.
7.1.2 Site blank samples
Bring sealed sealed blank sampling cartridges and filters to the sampling site and add 125 μl Sampling Reagent to PUF
(5.18), place 1 h to evaporate the solvent, installed in the sampling head without sampling, and then remove the sampling tube and filter, and
Samples are stored in the same way and shipped back to the lab with the sample.
7.2 Sample preservation
Samples were stored at room temperature protected from light, extracted within 24 h; otherwise, they should be stored in the dark below 4 ℃ and extracted within 7 d.
The sample extract is refrigerated at below 4 ° C and analyzed within 40 days.
7.3 Sample Preparation
7.3.1 Sample Extraction
Transfer the filter and glass sampling cartridge to a Soxhlet extractor (6.4), add 125 μl of assayed replacement fluid to the PUF
(5.14), add 300ml ~ 500ml ether - n-hexane mixed solvent (5.8) reflux extraction more than 16 h, every hour back
Flow 3 times to 4 times. After the extraction is completed, the mixture is cooled to room temperature, the bottom bottle is taken out, the extraction cup interface is washed, and the cleaning solution is transferred to the end
bottle. Add a little anhydrous sodium sulfate (5.5) to the sodium sulfate particles free-flowing, place 30 min dehydration and drying.
Note. If using automatic Soxhlet extraction, with ether - n-hexane mixed solvent (5.8) reflux extraction of not less than 40 cycles. As long as you can achieve this
Standards require quality control requirements, but also other sample extraction methods.
7.3.2 Sample concentration
The sample extract was transferred to a concentration apparatus, concentrated at below 45 ℃, the solvent was replaced by n-hexane, concentrated to 1 ml
about. If using sulfuric acid purification (7.3.3.1), concentrated to about 10 ml.
7.3.3 Sample Purification
7.3.3.1 sulfuric acid purification
The sample extract concentrate (7.3.2) was transferred to a separatory funnel (6.8), add 5 ml sulfuric acid (5.7), gently
Shake and deflate, shaking 1 min, after standing layered layer of sulfuric acid removed. Repeat the above procedure until the sulfuric acid layer is colorless. Add organic phase
5 ml sodium chloride solution (5.10), mix well, leave the aqueous phase after standing stratification, and add anhydrous sodium sulfate (5.5) to the organic phase
Dehydration, according to 7.3.2 concentrated to 1 ml or less, to be purified. If no further purification, set the volume to 1.0 ml, add 10.0 μl within
The standard solution (5.21) is transferred to the vial for analysis.
7.3.3.2 Magnesium silicate column purification
The bottom of the glass column (6.5) is filled with glass wool (5.32) and 20 g of magnesium silicate (5.27) is wet-filled with n-hexane (5.2)
6 Exhaust the bubbles and add 1 cm ~ 2 cm anhydrous sodium sulfate (5.5) to the top. Pre-rinse with 60 ml n-hexane (5.2) and keep
The liquid level is slightly above the column bed and the sample extract concentrate (7.3.2) or sulfuric acid-concentrated concentrate (7.3.3.1) is transferred to a chromatographic
The column was washed twice with 1 ml of n-hexane (5.2) and transferred to the column. The effluent was discarded.
The column was eluted with.200 ml of ether-n-hexane mixed solvent (5.9) at an elution rate of 2 ml/min to 5 ml/min
Receive eluate. Eluate 7.3.2 concentrated volume to 1.0 ml, add 10.0 μl of internal standard solution (5.21), transferred to the sample
Bottle to be analyzed.
7.3.3.3 Compound silica gel column purification
Take a mixture of silica gel column (5.26), pre-rinse with 100 ml of n-hexane (5.2). Keep the liquid level slightly higher than the bed, will be like
The product extract concentrate (7.3.2) was transferred to the column and the vial was washed twice with 1 ml of n-hexane (5.2) and transferred to the column
Within, discard the effluent.
Add.200 ml of n-hexane (5.2) for elution, control the flow rate of 2.5 ml/min or so and collect the eluent. Eluent according to 7.3.2
Concentrate to 1.0 ml, add 10.0 μl of internal standard solution (5.21) and transfer to vial for analysis.
Note. by the column size, the amount of adsorbent and other effects, the amount of eluent may be different, the laboratory before the need to carry out the conditions of the real
Inspection; as long as the quality control requirements of this standard can be achieved, you can also use other sample purification methods.
7.4 Preparation of blank samples
7.4.1 Site blank
On-site blank samples (7.1.2) In-situ blank samples were prepared according to the same procedure as Preparation of samples (7.3).
7.4.2 Laboratory blank
The same batch of sampling cartridges and filters according to the preparation of the sample (7.3) the same procedure for the preparation of laboratory blank samples.
8 Analysis steps
8.1 Instrument reference conditions
8.1.1 GC reference conditions
Inlet. 250 ℃; Injection mode. Splitless injection, shunt at 0.75 min, split ratio 60.1; Injection volume. 2.0 μl;
Column temperature. 50 ℃ for 1 min, 25 ℃/min heating to 180 ℃, holding 2 min, 5 ℃/min heating to 280 ℃,
Hold for 5 min; Carrier gas. Helium (5.31), Flow. 1.0 ml/min.
8.1.2 Reference conditions for mass spectrometry
Transmission line. 280 ℃; Ion source. 250 ℃; Ion source electron energy. 70 eV; Scanning mode. Selected ion scan
(SIM) or full scan (SCAN); solvent delay time. 8 min; electron multiplying voltage. consistent with tuning voltage;
The remaining parameters refer to the instruction manual of the instrument.
8.2 Instrument Performance Check
Prior to initial calibration, 1.0 μl of DFTPP solution (5.25) was injected into the GC-MS for full scan
DFTPP key ion abundances should meet the criteria set forth in Table 1; otherwise some parameters of the mass spectrometer need to be adjusted or cleaned
source of ion.
Table 1 DFTPP key ion abundance criteria
Mass ion m/z abundance standard mass ion m/z abundance standard
51 Base peak 30% ~ 60%.199 Base peak 5% ~ 9%
68 2% of less than 69 peaks 275% of the base peak 10% to 30%
70 Less than 69 2% of peak 365 365% of base peak 1%
40% to 60% of Base Peaks 441 are present and less than 443 Peaks
197 Less than 1% of base peak 442 Greater than 40% of base peak
198 base peak with an abundance of 100% 443 442 17% ~ 23%
8.3 Calibration
8.3.1 Determination of standard series
Pipette a certain amount of PCB standard solution (5.23), with n-hexane (5.2) diluted standard series, standard solution
The concentration of liquid was 25.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L, 300 μg/L and 500 μg/L,
Add 10.0 μl of internal standard solution (5.21) to the standard solution. According to the instrument reference conditions (8.1) for analysis, to obtain different concentrations
Degree standard solution of the mass spectrum, record the target compound, internal standard, replacement retention time and quantitative ion peak area. Polychlorine
Biphenyl Selective Ion Scan (SIM) The total ion chromatogram is shown in Figure 2.
8.3.2 Calculation of the average relative response factor
According to formula (1) and formula (2), the relative response factor of the standard series of target compounds for quantitative ions and the average relative
Response factor, and calculate the relative standard deviation of the relative response factor.
Relative response factor (
iRRF) according to formula (1) calculation.
sis
iss
i A
RRF
(1)
Average relative response factor (
iRRF) according to formula (2) calculation.
RRF
RRF
1 (2)
Where.
iRRF - relative response factor;
sA - Quantum ion peak area of target compound in standard solution;
is - concentration of the internal standard, μg/L;
isA - peak area of internal standard quantitation ion;
s - Concentration of target compound in standard solution, μg/L;
iRRF - Mean relative response factor.
88.3.3 drawing of the standard curve
The target compound concentration and internal standard concentration ratio as the abscissa, the target compound and internal standard ion peak area ratio
The value is ordinate, using the least squares method to draw the standard curve.
8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00 min
Time - >
Abundance
22,23
1-PCB 8; 2-PCB 18; 3-phenanthrene-D10 (internal standard); 4-PCB 28; 5-PCB 52; 6-PCB 44; 7-PCB 66;
8-PCB 101; 9-PCB 81; 10-p-terphenyl-D14 (Analytical Substitutes); 11-PCB 77; 12-PCB 123; 13-PCB
118, 14-PCB 114, 15-PCB 153, 16-PCB 105, 17-PCB 138, 18-PCB 126, 19-PCB 187,
20-PCB 128, 21-PCB 167, 22-䓛-D12 (internal standard), 23-PCB 156, 24-PCB 157, 25-PCB 180,
26-PCB 169; 27-PCB 170; 28-PCB 189; 29-PCB 195; 30-PCB 206;
Like substitute).
Figure 2. Total ion chromatogram of PCBs with ion-selective scanning (SIM)
8.4 Determination of the sample
The measurement of the sample is performed according to the same instrument conditions as those of the standard series, and the peak area of the quantitative ion and the retention time are recorded
between.
When the sample concentration exceeds the linear range of the standard curve, add 10.0 μl of internal standard solution (5.21) per ml
N-hexane solution was diluted appropriately, and then measured.
8.5 Blank test
The blank sample (7.4) was measured according to the same instrument conditions as the sample.
9 results calculated and expressed
9.1 Qualitative analysis
Select the ion scan or full scan mode to collect data, according to the relative retention time of the target compound in the sample
(RRT), auxiliary qualitative ion and quantitative ion peak area ratio (Q) qualitative. The relative retention of the target compound in the sample
The difference between the relative retention time of the compound and the midpoint of the standard curve is controlled within ± 0.03. The target compound in the sample
Of the auxiliary qualitative and quantitative ion peak area ratio (Q) and the standard series of intermediate point of the compound Q value control
Within ± 30%.
According to formula (3) calculate the relative retention time (RRT).
9is
RT
RT
RRT (3)
Where.
iRT - retention time of the target compound, min;
isRT - Internal standard retention time, min.
According to the formula (4) calculate the auxiliary qualitative ion and quantitative ion peak area ratio (Q).
0
Q (4)
Where.
qA - Auxiliary Qualitative Ion peak area;
tA - Quantitative ion peak area.
9.2 Quantitative method
According to the quantitative ion peak area, using internal standard method.
9.3 Results Calculation
The mass concentration of PCBs () in ambient air is calculated according to equation (5) and calculated using the average relative...
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