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Ambient air. Determination of organochlorine pesticides. Gas chromatography/mass spectrometry method
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Basic data | Standard ID | HJ 900-2017 (HJ900-2017) | | Description (Translated English) | Ambient air. Determination of organochlorine pesticides. Gas chromatography/mass spectrometry method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 21,295 | | 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 organochlorine pesticides in the ambient air. This standard applies to ambient air gas and particulate matter hexachlorobenzene, alpha-hexanol, gamma-hexa-, beta- hexamethylene, delta- hexamethylene, heptachlor, aldrin, epoxy heptachlor-B , Gamma-chlordane, alpha-chlordane, endosulfan I, 4, 4""-DDE, dieldrin, endrin, 4, 4""-DDD, endosulfan II, 2, 4""- Determination of 23 Organochlorine Pesticides, DDT, 4, 4""-DDT, Enderaldehyde, Endosulfan Sulfate, Dimethoxy DDT, Ditrisone, and Mirex. See Appendix B for details. If verified, this standard also applies to the determination of other organochlorine pesticides. When the sampling volume is 350 m^(3) (standard state), the volume of concentrated volume is 1.0 |
HJ 900-2017: Ambient air. Determination of organochlorine pesticides. 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 organochlorine pesticides - Gas chromatography - mass spectrometry)
People's Republic of China national environmental protection standards
Ambient air - Determination of organochlorine pesticides
Gas chromatography - mass spectrometry
Ambient air-Determination of organochlorine pesticides
-Gas chromatography/mass spectrometry method
2017-12-14 Published
2018-03-01 implementation
Ministry of Environmental Protection released
i 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 ... 7
9 Calculation and Expression of Results ... 9
10 Precision and accuracy ... 10
11 Quality Assurance and Quality Control ... 11
12 Waste Treatment ... 11
Appendix A (Normative) Method Detection Limit and Determination of the lower limit ... 13
Appendix B (Informative) Compound List ... 14
Appendix C (Informative) Characteristics of organochlorine pesticides and ion-selective scanning procedures ...
Appendix D (informative) method of precision and accuracy ... 18
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, regulate the determination of organochlorine pesticides in the ambient air, the development of this standard.
This standard specifies the determination of organochlorine pesticides in ambient 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.
Ambient air - Determination of organochlorine pesticides - Gas chromatography - mass spectrometry
Warning. The solvents and reagents used in this method are toxic and experimental procedures should be performed in a fume cupboard
Always wear protective equipment to avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of organochlorine pesticides in ambient air by gas chromatography - mass spectrometry.
This standard applies to ambient air and particulate matter hexachlorobenzene, α-BHC, γ-BHC, β-BHC, δ-VI
Hexachlorocyclohexane, Aldrin, Epichlorohydrin B, γ-Chlordane, α-Chlordane, Endosulfan I, 4,4'-DDE, Dieldrin, Endrin,
4,4'-DDD, endosulfan II, 2,4'-DDT, 4,4'-DDT, endodaldehyde, endosulfan sulfate, methoxy DDT,
Moxa total of 23 kinds of organochlorine pesticides determination. See Appendix B for details. If verified, this standard also applies to other organic chlorine
Determination of pesticides.
When the sampling volume is 350 m3 (standard state), the volume of concentrated volume is 1.0 ml, and the selective ion scan (SIM)
Method, the detection limit of 23 organochlorine pesticides in this method was 0.03 ng/m3 ~ 0.07 ng/m3, the lower limit of determination
0.12 ng/m3 ~ 0.28 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 organochlorine pesticides in the ambient air and particulate matter into the filter and polyurethane foam
(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, choose to use sulfuric acid, magnesium silicate column and other purification methods to remove interference,
However, the purification of sulfuric acid can cause the decomposition of some organochlorine pesticides, as detailed in 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.
25.3 Ether (C4H10O). Chromatographic purity.
5.4 Dichloromethane (CH2Cl2). pesticide grade.
5.5 Anhydrous sodium sulfate (Na2SO4). before use in a muffle furnace 400 ℃ baking 4 h, after cooling, in a ground glass jar
Sealed and saved
5.6 Sodium chloride (NaCl). Bake in a muffle furnace at 400 ° C for 4 h before use, then cool and seal in a ground-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 acetone - n-hexane mixed solvent. 1 9, Pro use now with.
5.10 ether - n-hexane mixed solvent. 5 5, Pro use now.
5.11 ether - n-hexane mixed solvent. 6 94, Pro use now with.
5.12 ether - n-hexane mixed solvent. 15 85, Pro use now.
5.13 Sodium chloride solution. ρ = 50 g/L.
Weigh 50.0 g of sodium chloride (5.6) in a beaker, dissolved in water and set the volume to 1000 ml, mix, Pro use now.
5.14 Endrin and 4,4'-DDT standard solution. ρ = 1.0 mg/L.
Buy a commercially available standard solution directly and dilute with n-hexane (5.2).
5.15 pairs of 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.
5.16 Analysis Alternative stock solution. ρ =.2000 μg/ml.
Weigh p-terphenyl-D14 (5.15) about 0.1 g, accurate to 0.1 mg, in a 50 ml volumetric flask, with a small amount of dichloromethane
After dissolving alkane (5.4), dilute with n-hexane (5.2) and mix well.
5.17 Analysis of intermediate solution. ρ = 40.0 μg/ml.
Pipette 500 μl of stock solution (5.16) into a 25 ml volumetric flask and dilute with n-hexane (5.2) and mix well.
5.18 Analysis Alternatives Solution. ρ = 2.00 μg/ml.
Pipette 100 μl of stock solution (5.16) into 100 ml volumetric flask, dilute to volume with n-hexane (5.2), mix
uniform.
5.19 Endosulfan I-D4 or 4,4'-DDT-D8 stock solution. ρ = 100 μg/ml.
Sampling alternatives, other isotopic markers may also be used. Direct purchase of certified public standard solution, the solvent is isooctane.
5.20 Sample Alternatives Intermediate solution. ρ = 20.0 μg/ml.
Take 1.00 ml aliquots of stock solution (5.19) in a 5 ml volumetric flask and dilute to volume with n-hexane (5.2) and mix well.
5.21 sampling alternative solution. ρ = 2.00 μg/ml.
Take 1.00 ml of sample substitute intermediate solution (5.20) in a 10 ml volumetric flask, dilute with n-hexane (5.2) and mix well.
5.22 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.
5.23 Internal standard intermediate solution. ρ = 75.0 μg/ml.
Take 1.00 ml internal standard stock solution (5.22) in a 10 ml volumetric flask, dilute with n-hexane (5.2) and mix well.
5.24 Internal standard solution. ρ = 15.0 μg/ml.
3 Take 2.00 ml internal standard solution (5.23) in a 10 ml volumetric flask and dilute with n-hexane (5.2) and mix well.
5.25 standard stock solution. ρ =.2000 μg/ml.
Direct purchase of the market a certified standard solution, including α-BHC, γ-BHC, β-BHC, δ-BHC, heptachlor,
Aldrin, epichlorohydrin B, gamma-chlordane, alpha-chlordane, endosulfan I, 4,4'-DDE, dieldrin, endrin, 4,4'-DDD,
Endosulfan II, 4,4'-DDT, isoderaldehyde, endosulfan sulfate, methylated DDT and docetaxel, a total of 20 kinds of organochlorine pesticides mixed
Combined solution. Hexachlorobenzene, 2,4'-DDT and mirex as single standard solutions at a concentration of.2000 μg/ml. Can also be prepared 23 kinds of organic
Chlorine pesticide mixed solution.
5.26 standard intermediate solution. ρ = 40.0 μg/ml.
Pipette 1.00 ml of organochlorine pesticide standard stock solution (5.25) in a 50 ml volumetric flask with n-hexane (5.2)
Mix well.
5.27 standard solution. ρ = 1.0 μg/ml.
Pipette 250 μl of the assay intermediate (5.17), 500 μl of the sample intermediate (5.20) and 250 μl
Standard intermediate solution (5.26) in 10 ml volumetric flask, with n-hexane (5.2) volume, mix.
5.28 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.
5.29 Dopentafluorophenylphosphine (DFTPP) Use solution. ρ = 4.0 μg/ml.
Pipette 1.00 ml of decafluorotriphenylphosphine (5.28) in a 25 ml volumetric flask, dilute with dichloromethane (5.4) and mix well.
Note. All solutions (5.14 ~ 5.29) are transferred to a screw-capped glass bottle with Teflon liner, refrigerated at 4 ° C and sealed against light
save.
5.30 Magnesium silicate solid phase extraction column. 1000 mg/6 ml.
5.31 Magnesium silicate. 150 μm to 250 μm (100 mesh to 60 mesh). Activate at 130 ° C for at least 18 h before use and allow to dry
After cooling in the desiccator, transfer to a glass bottle and seal.
5.32 Quartz/glass fiber filter. According to the sampling head to select the appropriate specifications, 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.
5.33 Polyurethane Foam (PUF). polyether type, with a density of 22 mg/cm3 ~ 25 mg/cm3, cut to grow 70 mm, straight
Cylindrical diameter of 45 mm to 65 mm (length, diameter as determined by the specifications of the glass sampling cartridge). Use hot water before use
Scald, and then repeatedly rub into warm water, drained, rinsed with acetone (5.1) three times and placed in a Soxhlet extractor (6.4)
Followed by acetone (5.1), ether - n-hexane mixed solvent (5.8) reflux extraction 16 h, replace 2 times to 3 times fresh B
Ether - n-hexane mixed solvent (5.8) reflux extraction, removed after the nitrogen (5.34) stream drying (also can be true at room temperature
Air dry 2 h ~ 3 h), into the glass sample tube (6.3.2) sealed in a suitable container.
5.34 Nitrogen. Purity ≥99.999%.
5.35 Helium. Purity ≥ 99.999%.
5.36 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.
46.2 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, and the stationary phase is 35% phenyl 65% dimethylpolysiloxane column,
Or other equivalent low-loss columns.
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.
With filters and sorbents, 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 tube stainless steel mesh support, the adsorption tube
The material is PUF (5.33). Sampling tube sealed with a silicone rubber seal 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.
56.5 Glass Column. 350 mm long, 15 mm to 20 mm id, glass column with Teflon piston on the bottom.
6.6 Concentration device. Rotary evaporator, nitrogen purifier or other performance-equivalent equipment.
6.7 solid phase extraction device.
6.8 separatory funnel. 60 ml.
6.9 General laboratory equipment commonly used.
7 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 Substitute Solution (5.21) to the PUF before site collection, place for 1 h, and then install
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 the glass sampling cylinder out of the sampling cartridge sleeve, wrap it with aluminum foil, and put it into a storage box to seal it.
7.1.2 Site blank samples
Bring the sealed blank glass sampling cartridge and filter to the sampling site and add 125 μl sampling replacements to the PUF
With liquid (5.21), place 1 h to dry the solvent, installed in the sampling head without sampling, and then remove the sampling cartridge and the filter,
Store in the same way as the sample and 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
(5.18), add 300ml ~ 500ml diethyl 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 anhydrous sodium sulfate (5.5) to sodium sulfate particles free-flowing, placed 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
Standard requirements of quality control, but also the use of 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
65 ml of sodium chloride solution (5.13), 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 (5.24) is transferred to the vial for analysis.
This purification method does not apply to dieldrin, endrin, endosulfan I, endosulfan II, endodialdehyde, endrin and methoxy
DDT determination.
7.3.3.2 Magnesium silicate solid phase extraction column purification
Take solid phase extraction column (5.30), followed by 10 ml of acetone (5.1), 10 ml of n-hexane (5.2) pre-leaching, discard the flow
Liquid.
Keep the liquid level just above the bed and transfer the sample extract concentrate (7.3.2) or sulfuric acid concentrate (7.3.3.1) to
In the column, the effluent is received, the sample bottle is washed twice with 1 ml of n-hexane (5.2), the wash liquid is transferred to the SPE column,
With 10 ml acetone - n-hexane mixed solvent (5.9) elution, control the flow rate of less than 2 ml/min, continue to receive the eluent. wash
Dispense 7.3.2 concentrated volume to 1.0 ml, add 10.0 μl of internal standard solution (5.24), transferred to the vial to be analyzed.
7.3.3.3 Magnesium silicate column purification
The bottom of the glass column (6.5) is filled with glass wool (5.36) and 20 g of magnesium silicate (5.31) is wet-filled with n-hexane (5.2)
Exhaust air bubbles, add 1 cm ~ 2 cm anhydrous sodium sulfate (5.5) on the top. Pre-rinse with 60 ml n-hexane (5.2) and keep
The liquid level is slightly above the bed, the extraction concentrate (7.3.2) is transferred to the column and the sample bottle is washed with 1 ml of n-hexane (5.2)
2 times, were transferred to the column, discard the effluent.
The column was eluted with.200 ml ether-n-hexane mixed solvent (5.11) at a rate of 2 ml/min to 5 ml/min
Receive effluent as a first-stage eluent. Continue with.200 ml ether - hexane mixed solvent (5.12) eluting the column, then
Receive effluent as a second-stage eluate. The column was eluted with.200 ml of ether-n-hexane mixed solvent (5.10) to receive the flow
Effluent as a third-level eluent. If not received grading, you can directly use.200 ml acetone - n-hexane mixed solvent (5.9)
Eluting the column and receiving the eluate. Eluate 7.3.2 concentrated volume to 1.0 ml, add 10.0 μl of internal standard solution (5.24),
Transfer to vial for analysis.
The first eluent contains all of the PCBs except for endosulfan, dieldrin, endrin and their degradation products,
Other pesticides at this level; dieldrin, endosulfan I, endrin distributed in the first or second level, may also co-exist at two levels;
Endosulfan II, endrin, endosulfan sulfate are mainly distributed in the third-stage eluate; the endodildehyde distribution in the second and third
Grade eluent.
Note. Due to the solid phase extraction column and column specifications, the amount of magnesium silicate, the amount of eluent may be different at all levels of the eluate of organic chlorine
There are differences in the elution efficiency of pesticides, the laboratory before the use of conditions required to conduct experiments; as long as this standard can meet the quality control
Requirements, but also the use of 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.
78 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 (5.35), Flow rate. 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. 9 min; electron multiplying voltage. consistent with tuning voltage;
The remaining parameters refer to the instruction manual of the instrument.
8.1.3 Select the ion scan (SIM) program
Take 250 μl of the analyte intermediate solution (5.17), 500 μl of the sample alternative intermediate solution (5.20), 250 μl of
Chlorine pesticide intermediate solution (5.26), add 10.0 μl internal standard stock solution (5.22), according to the instrument reference conditions (8.1)
Scan analysis, according to the retention time to determine the selected ion program, see Table C.1.
8.2 Instrument Performance Check
Prior to initial calibration, 1.0 μl of DFTPP use solution (5.29) was injected into the GC-MS and the full scan
DFTPP key ion abundances should meet the criteria set forth in Table 1, or 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%
After passing the DFTPP key ion abundance, 1.0 μl of endrin and 4,4'-DDT mixture (5.14) were injected
In addition to the detection of the above compounds, if chromatographic - mass spectrometry, isomerised aldehyde, endrin and 4,4'-DDE were also detected,
4,4'-DDD, which indicates that endrin and 4,4'-DDT decomposition, if the degradation of a single compound ≥ 20% or both
The sum of the degradation is ≥30%, and the inlet and column heads need to be maintained. Systematic inspection of organochlorine pesticides after school
quasi.
8.3 Calibration
88.3.1 Determination of standard series
Pipette a certain amount of organochlorine pesticide standard solution (5.27), with n-hexane (5.2) diluted standard series, the standard
The series concentrations were 50.0 μg/L, 100 μg/L,.200 μg/L, 300 μg/L, 500 μg/L,
Add 10.0 μl of internal standard solution (5.24). According to the instrument reference conditions (8.1) for analysis, to obtain different concentrations of standard solution
Liquid mass spectrometry, record the target compound, internal standard, replacement retention time and quantitative ion peak area. Organochlorine pesticide selection
Selected Ion Scan (SIM) The total ion current is shown in Figure 2.
1-α-BHC; 2-HCB; 3-β-BHC; 4-γ-BHC; Heptachlor; 8-
Aldrin 9-Ephedrine B 10-γ-Chlordane 11-Endosulfan I-D4 (Sampling Alternative) 12-Endosulfan I 13-α-Chlordane 14-4,4 '-DDE;
15-Dieldrin; 16-p-terphenyl-D14 (Analytical Substitutes); 17-Endrin; 18- Endosulfan II; 19-4,4'-DDD; 20-2,4'-DDT;
Endosulfan sulfate; 23-4,4'-DDT-D8 (sample replacement); 24- 4,4'-DDT; 25-
䓛 -D12 (internal standard); 27-methoxy DDT; 28-mirex.
Figure 2 Organochlorine pesticide selective ion scan (SIM) total ion chromatogram (5% phenyl 95% dimethylpolysiloxane column)
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. If the relative standard deviation ≤ 20%, use the average relative
Response factor calculation results.
The relative response factor (iRRF) is calculated according to equation ...
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