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HJ 753-2015 English PDF

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HJ 753-2015: Water quality. Determination of chlorothalonil and pyrethroid insecticides. Gas chromatography mass spectrometry
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 753-2015429 Add to Cart 3 days Water quality. Determination of chlorothalonil and pyrethroid insecticides. Gas chromatography mass spectrometry Valid

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Basic data

Standard ID: HJ 753-2015 (HJ753-2015)
Description (Translated English): Water quality. Determination of chlorothalonil and pyrethroid insecticides. Gas chromatography mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 17,198
Date of Issue: 2015-08-21
Date of Implementation: 2015-10-01
Quoted Standard: HJ/T 91; HJ/T 164
Regulation (derived from): Ministry of Environment Announcement 2015 No.54
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the water chlorothalonil and eight kinds of liquid-liquid extraction pyrethroid pesticides or solid phase extraction/gas chromatography - mass spectrometry. This standard applies to the determination of chlorothalonil and pyrethroid pesticide compounds in surface water, groundwater, industrial wastewater and domestic sewage in. Liquid-liquid extraction and sampling of 1L, the method detection limit of 0.005 ~ 0.05��g/L, detection limit of 0.020 ~ 0.20��g/L; solid phase extraction sample volume of 500ml, the method detection limit of 0.005 to 0.08 ��g/L, detection limit of 0.020 ~ 0.32��g/L. See Appendix A.

HJ 753-2015: Water quality. Determination of chlorothalonil and pyrethroid insecticides. Gas chromatography mass spectrometry


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Water quality.Determination of chlorothalonil and pyrethroid insecticides.Gas chromatography mass spectrometry National Environmental Protection Standard of the People 's Republic of China Water quality - Determination of chlorothalonil and pyrethroid pesticide - Gas chromatography - mass spectrometry Water quality - Determination of chlorothalonil and pyrethroid insecticides - Gas Test mass spectrometry 2015-08-21 release 2015-10-01 implementation Ministry of Environmental Protection I directory Preface .ii 1 Scope of application 1 2 normative reference document 1 Principle of Method 1

4 reagents and materials

5 instruments and equipment

6 samples

7 Analysis Step 3 Calculation and presentation of results 9 Precision and Accuracy 6 10 Quality assurance and quality control 11 Waste treatment .7 12 Precautions .7 Appendix A (normative appendix) method detection limit and lower limit of measurement Appendix B (informative) Mass Spectrometry Reference Criteria 9 Appendix C (informative) method of precision and accuracy 10

Foreword

In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Water Pollution, Protection of human health, regulate the determination of chlorothalonil and pyrethroid pesticides in the determination of the method, the development of this standard. This standard specifies the chlorothalonil and pyrethroid pesticide gas chromatography-mass spectrometry. This standard is the first release. Appendix A to this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. National Environmental Analysis and Testing Center. The standard verification unit. Hunan Province Environmental Monitoring Center Station, Hubei Province Environmental Monitoring Center Station, Pearl River Basin Water Environment Monitoring Measuring center, Xiangtan City Environmental Protection Monitoring Station, Changsha City Environmental Monitoring Center Station and Zhuzhou City Environmental Monitoring Center Station. The Environmental Protection Department of this standard approves on August 21,.2015. This standard is implemented on October 1,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of chlorothalonil and pyrethroid pesticides - Gas chromatography - mass spectrometry Warning. The solvent, internal standard and standard samples used in the experiment are toxic and harmful compounds. The solution should be prepared. Wind cabinet, the operation should be required to wear protective equipment, to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the liquid-liquid extraction or solid-phase extraction/gas chromatography-mass spectrometry of chlorothalonil and eight pyrethroid pesticides Spectrum method. This standard applies to surface water, groundwater, industrial wastewater and domestic sewage chlorothalonil and pyrethroid pesticide compounds Determination of matter. The detection limit of the method was 0.005 μg/L to 0.05 μg/L, and the lower limit of determination was 0.020 Μg/L ~ 0.20 μg/L. When the sample volume was 500 ml, the detection limit was 0.005 μg/L ~ 0.08 μg/L. Limited to 0.020 μg/L to 0.32 μg/L. See Appendix A. for details.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Technical specification for surface water and wastewater monitoring Technical specification for groundwater environmental monitoring

3 Principle of the method

The liquid extract or solid phase extraction method was used to extract chlorothalonil and pyrethroid pesticide in water samples. The extract was dehydrated, Concentrated, purified, constant volume, separated by gas chromatography, mass spectrometry. According to the retention time, the fragment ion mass ratio and its abundance Degree of qualitative and internal standard method.

4 reagents and materials

Unless otherwise stated, analytical analytical reagents and pure water that do not contain the target are used in the analysis. 4.1 dichloromethane (CH2Cl2). pesticide residues. 4.2 n-hexane (C6H14). pesticide residues. 4.3 methanol (CH3OH). pesticide residues. 4.4 chlorothalonil standard solution. ρ = 1 000 mg/L, the solvent is acetone, commercially available standard solution. 4.5 pyrethroid standard solution. ρ = 1 000 mg/L, including deltamethrin, fenvalerate, cypermethrin, cyhalothrin, Chrysanthemum, fenpropathrin, ketamine and allyrin, the solvent is acetone, commercially available standard solution. 4.6 internal standard stock solution I. ρ = 100 mg/L, including deuterated phenanthrene, deuterated pyrene and deuterium, the solvent is n-hexane. Can be purchased directly Certified standard solution can also be prepared with the standard material, diluted with n-hexane, 4 ℃ below the sealed light preservation. 4.7 internal standard stock solution II. ρ = 100 mg/L, including 13C-PCB209, the solvent is n-hexane. Can be purchased directly to prove the standard solution, Can also be prepared using standard materials, diluted with n-hexane, 4 ℃ below the sealed light preservation. 24.8 anhydrous sodium sulfate (Na2SO4). Burn at 400 ℃ for 4 h, cooled into the grinding glass bottle, placed in the dryer to save. 4.9 standard solution liquid. ρ = 10.0 ~ 100 mg/L. Respectively, remove 100 μl of chlorothalonil (4.4) and bifenthrin, fenpropathrin, ketamine, allylin standard solution (4.5), And then remove 1.00 ml of deltamethrin, fenvalerate, cypermethrin and cyhalothrin standard solution (4.5) to 10 ml Color volume bottle, with n-hexane (4.2) constant volume to the mark, mix. Is now available. 4.10 internal standard use of liquid. ρ = 10.0 ~ 20.0 mg/L. Remove the 1.00 ml internal standard stock solution I (4.6) and the 2.00 ml internal standard stock solution II (4.7) to 10 ml volumetric flask, respectively, With n-hexane (4.2) constant volume to the mark, mix. 4.11 n-hexane acetone solution. 95 5. 4.12 Magnesium silicate column. The filler is magnesium silicate, 500 mg, and the column volume is 6 ml. 4.13 solid phase extraction column. the filler is lipophilic divinyl benzene and hydrophilic N-vinyl pyrrolidone two kinds of monomer by a certain proportion of poly Synthetic macroporous copolymer or equivalent type of filler, 1 000 mg, column volume of 6 ml, commercially available. 4.14 Carrier gas. helium, purity ≥ 99.999%.

5 instruments and equipment

5.1 Sampling vials. 1 L or 2 L brown glass jar with a mouth plug. 5.2 Gas Chromatography Mass spectrometer. with capillary column and split/splitless inlet, programmable temperature, mass spectrometry with EI source. 5.3 Column. 5% phenyl-methylpolysiloxane with a column length of 30 m. The column was a fused silica with an inner diameter of 0.25 mm Capillary column with a film thickness of 0.25 μm. Or use other equivalent columns. 5.4 solid phase extraction device. solid phase extraction instrument, through the vacuum pump to adjust the flow rate. 5.5 Concentration device. rotary evaporator or KD concentrator, nitrogen blowing concentrator and other enrichment device. 5.6 separatory funnel. 2 L with polytetrafluoroethylene plug. 5.7 General laboratory equipment and equipment commonly used.

6 samples

6.1 Collection and storage of samples The collection and storage of water samples are carried out in accordance with the relevant provisions of HJ/T 91 and HJ/T 164. Samples were taken with a sampling vial (5.1) The samples were stored at 4 ° C and the extraction was completed within 7 days. 6.2 Preparation of the sample 6.2.1 Liquid-liquid extraction method 6.2.1.1 Extraction Accurately measure 1 000 ml of water in a 2 L separatory funnel (5.6). Add 30 ml of dichloromethane (4.1) and shake for 5 min (Note the gas), put it aside for 5 min, to be two-phase stratification, collecting the lower organic phase. Repeat the above operation twice. Combined extract, The extract was dehydrated by anhydrous sodium sulfate (4.8). During the concentration of the extract, the conversion solvent was n-hexane and concentrated to about 1 ml, To be purified. Note 1. When using methylene chloride extraction attention to deflation; if the extraction of emulsification phenomenon, can be salting out, stirring, centrifugal, frozen or glass Cotton filter and other methods to break the milk. 36.2.1.2 Purification Groundwater and background interference low surface water and other samples of the extract can be purified without direct analysis. The extract was purified using a magnesium silicate column (4.12). eluting with 10 ml of n-hexane acetone solution (4.11) and 10 ml N-Hexane (4.2) pre-leaching, column bed to leave the liquid; the concentrate was transferred to the purification column, with about 2 ml of n-hexane (4.2) Wash the collection bottle and wash the solution together with the column; elute with 10 ml of n-hexane acetone solution (4.11) and collect the eluate in a concentrated flask in. 6.2.1.3 Concentration Concentrate with a concentrator (5.5) and set to 1.0 ml with n-hexane, add 10.0 μl of internal standard (4,10), transfer Into a sample vial for GC-MS analysis. 6.2.2 solid phase extraction method 6.2.2.1 Activation of solid phase extraction column Followed by 10 ml of dichloromethane (4.1), 10 ml of methanol (4.3), 10 ml of water pre-leaching column, to ensure that the bed in a wet And active state standby. 6.2.2.2 enrichment of water samples Accurately measure the water sample 500 ml, to 5 ~ 10 ml/min flow rate of enrichment, water enrichment, rinse with 10 ml of water The inner wall of the vial is enriched and then blown with high purity nitrogen to dry the extract column. If the sample is extracted using an automatic solid phase extraction (SPE) Should be in accordance with their own instructions to operate the instrument. Note 2. Water samples with high suspended solids are not suitable for solid phase extraction. 6.2.2.3 Sample elution and concentration The sample was washed with 12 ml of dichloromethane (4.1) and washed with a solid phase extraction column, dried over anhydrous sodium sulfate (4.8) In the receiving tube. After concentration with a nitrogen bubbler (5.5), the conversion solvent was n-hexane and continued to concentrate to 1.0 ml, Μl internal standard using liquid (4.10), transferred to the sample vial for GC-MS analysis. Note 3. If the chromatographic analysis can not be carried out in time, it should be stored at 4 ° C and stored within 40 days. 6.3 Preparation of blank samples Substantially the same procedure as in sample preparation (6.2.1 or 6.2.2) was used instead of the sample to prepare a blank sample.

7 Analysis steps

7.1 Instrument reference analysis conditions 7.1.1 Gas Chromatographic Reference Conditions Inlet temperature. 280 ° C, splitless injection; carrier gas flow rate. 1.0 ml/min; injection volume. 1.0 μl; Oven temperature. 70 ° C (2 min) 30 ° C/min 220 ° C (3 min) 5 ° C/min 280 ° C (5 min) 20 ° C/min 300 ° C (5 min). Note 4. Determination of chlorothalonil, gas chromatography chamber liner should be put or put a very small amount of glass wool. 7.1.2 Mass Spectral Reference Conditions Four-stage bar temperature. 150 ° C; ion source temperature. 230 ° C; transmission line temperature. 300 ° C; ionization energy. 70 eV. Data acquisition method. Select ion scan. The peak order of the target compound, the retention time and the main selection of ions Refer to Appendix B for reference conditions. 7.2 Calibration 47.2.1 Instrument performance check The mass spectrometer system is tuned with perfluorotributylamine prior to use. Before the sample analysis and every 24 h, need to inject 1.0 Μl decafluorotriphenylphosphine (DFTPP, 50 μg/ml), the entire system to check the instrument. The critical ion abundance of DFTPP should Meet the requirements of Table 1. Table 1 DFTPP critical ion and ion abundance standards Mass ion (m/z) abundance standard mass ion (m/z) abundance standard 51% of the peak of 30% -60% of the base peak of 5% -9% 68% less than 69% of the peak of 275% of the peak of 10% -30% 70 less than 69 peaks of 2% 365 greater than 1% of peak 127 base peaks of 40% -60% 441 are present and less than 443 peaks 197 is less than 1% of the base peak 442 is greater than 40% of the base peak 198 base, abundance of 100% 443 442 peak of 17% -23% 7.2.2 Preparation of standard series Take 5 10 ml brown volumetric flasks and add 10.0, 50.0, 100,.200, 500 μl of standard solution (4.9) With n-hexane volume to the mark, and then add 100 μl internal standard liquid (4.10), mix. Prepared into five different concentrations Standard series (CS) See Table 2. Table 2 Preparation of standard solutions of chlorothalonil and pyrethroid pesticide standard series Standard Series CS-1 CS-2 CS-3 CS-4 CS-5 Standard solution using liquid volume (μl) 10.0 50.0 100.200 500 Fixed volume (ml) 10.0 10.0 10.0 10.0 10.0 Internal volume of liquid used (μl) 100 100 100 100 100 Chlorothalonil, allyl ester, ketamine, bifenthrin and fenpropathrin concentration (ng/ml) 10.0 50.0 100.200 500 Cyhalothrin, cypermethrin, deltamethrin and deltamethrin concentration (ng/ml) 100 500 1 000 2 000 5 000 7.2.3 Establishment of calibration curve The GC-MS determination was carried out sequentially from low to high concentrations according to the instrumentation analysis conditions (7.1). To the standard series The ratio of the mass concentration of the target to the mass concentration of the internal standard is the abscissa, and the peak area of the corresponding peak and the peak area of the internal standard The product of the ratio and the concentration of the internal standard is the ordinate, and the internal standard calibration curve is established. 7.3 Determination of samples The determination was made according to the same instrumentation analysis conditions (7.1) as the standard curve for drawing. If the concentration of the substance to be measured in the sample Beyond the calibration curve range, need to be re-measured after dilution. 7.4 blank test The blank sample (6.3) was measured according to the same instrumentation analysis conditions (7.1) as the standard curve. 58 Calculation and presentation of results 8.1 Qualitative analysis According to the target retention time, fragment ion mass ratio and its abundance ratio qualitative. For each target, the subject should be used The quasi-solution (or standard series) is subjected to multiple injections to establish a retention time window with a retention time window of ± 3 times the average retention time Of the standard deviation, the retention time of the target in the sample should be within the window of the retention time. The target is the auxiliary ion in the sample The relative aberration of the relative abundance of the quantitative ions and the relative abundance obtained by the nearest calibration standard should be less than 30%. Chlorothalonil And pyrethroid pesticide total ion chromatogram shown in Figure 1. 1 deuterated phenanthrene, 2 probiotics, 3 allylene, 4 deuterated pyrene, 5 deuterated, 6 bifenthrin, 7 quinisol, 8 fenpropathrin, Ester 1, 10 cyhalothrin 2, 11 cypermethrin 1, 12 cypermethrin 2, 13 cypermethrin 3, 14 cypermethrin 4, 15 13C-PCB209, 16 Fenvalerate 1, 17 fenvalerate 2, 18 deltamethrin 1, 19 deltamethrin 2 Figure 1 Total ion chromatogram of chlorothalonil and pyrethroid pesticide 8.2 Quantitative analysis Auxiliary ion quantification is allowed when the quantitation ions of the target in the sample are interfering. The concentration of the target in the sample (Μg/L), calculated according to formula (1). (1) Where. the mass concentration of chlorothalonil or pyrethroid in ρ-sample, μg/L; Ρ1 - concentration of chlorothalonil or pyrethroid in the sample calculated according to the internal standard calibration curve, μg/L; V1 - the volume of the sample, ml; V-water sample volume, ml; F-dilution factor. 8.3 results show When the determination result is greater than 1.00 μg/L, the data retains three significant digits. When the result is less than or equal to 1.00 μg/L, Bacteria clear, allyl permethrin, pyrethroid, bifenthrin and fenpropathrin data were retained at three decimal places, cyhalothrin, cyano cyanide Fρρ 1  V1 Pyrethrins and deltamethrin data were retained for two decimal places.

9 precision and accuracy

9.1 precision 9.1.1 Liquid-liquid extraction method Six laboratories were tested for chlorothalonil, allylene, fenpropathrin, bifenthrin, ketamine concentration of 0.010 μg/L, 0.10 μg/L, 1.00 μg/L, cyhalothrin, cypermethrin, fenvalerate, deltamethrin concentration of 0.10 μg/L, 1.00 Μg/L, 10.0 μg/L of the uniform samples were measured. The relative standard deviations in the laboratory were 4.2% ~ 21%, 1.3% ~ 18% 1.7% ~ 17%; the relative standard deviation between the laboratory is. 5.8% ~ 17%, 2.9% ~ 11%, 4.3% ~ 10%; repeatability limit (r) Respectively. 0.003 μg/L ~ 0.037 μg/L, 0.019 μg/L to 0.320 μg/L, 0.240 μg/L to 3.30 μg/L, the reproducibility limit (R) Respectively. 0.004 μg/L ~ 0.055 μg/L, 0.022 μg/L to 0.380 μg/L, 0.280 μg/L to 3.10 μg/L, respectively. 9.1.2 Solid phase extraction The six laboratories were tested for chlorothalonil, permethrin, fenpropathrin, bifenthrin, amphetamycin at 0.020 μg/L, 0.20 Μg/L, 2.00 μg/L, cyhalothrin, cypermethrin, fenvalerate, deltamethrin concentration of 0.20 μg/L, 2.00 μg/L, 20.0 μg/L of the uniform samples were measured. The relative standard deviations in the laboratory were 2.0% ~ 13%, 2.1% ~ 17% 3.1% ~ 16%; the relative standard deviation between the laboratory is. 5.4% ~ 14%, 3.4% ~ 17%, 4.6% ~ 15%; repeatability limit (r) (0.20 μg/L to 0.045 μg/L, 0.021 μg/L to 0.450 μg/L, 0.320 μg/L to 4.50 μg/L, respectively) Respectively. 0.004 μg/L ~ 0.070 μg/L, 0.043 μg/L to 0.930 μg/L, 0.520 μg/L to 8.20 μg/L. 9.2 Accuracy 9.2.1 Liquid-liquid extraction method Six laboratories containing chlorothalonil, permethrin, fenpropathrin, bifenthrin, and the concentration of permethrin was 0.100 μg/L Cyhalothrin, cypermethrin, deltamethrin, deltamethrin at a concentration of 1.00 μg/L were tested by spiked assay set. The recoveries ranged from 79.5% to 110% and the standard deviations were 2.6% to 12%, respectively. 9.2.2 Solid phase extraction Six laboratories containing chlorothalonil, allyrin, fenpropathrin, bifenthrin, and amphetamycin concentrations of 0.200 μg/L Cyhalothrin, cypermethrin, deltamethrin and deltamethrin at a concentration of 2.00 μg/L were measured by spiked assay set. The recoveries ranged from 78.3% to 94.5% and the standard deviations were in the range of 2.9% to 11%. Refer to Appendix C for precision and accuracy results. 10 quality assurance and quality control 10.1 blank test Each batch of samples (with 20 samples for a batch) should be at least one lab blank experiment, all blank test results Of the target compound concentration should be less than the detection limit, if the target compound detection, should identi......
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