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HJ 1018-2019: Water quality - Determination of sulfonylurea pesticides - High performance liquid chromatography
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Basic data

Standard ID HJ 1018-2019 (HJ1018-2019)
Description (Translated English) Water quality - Determination of sulfonylurea pesticides - High performance liquid chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Classification of International Standard 13.060
Word Count Estimation 20,279
Date of Issue 2019
Date of Implementation 2019-09-01
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1018-2019: Water quality - Determination of sulfonylurea pesticides - High performance liquid chromatography


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Water quality - Determination of sulfonylurea pesticides - High performance liquid chromatography National Environmental Protection Standard of the People's Republic Determination of water sulfonylurea pesticides High performance liquid chromatography Water quality-Determination of sulfonylurea pesticides-High Performance liquid chromatography 2019-04-13 released 2019-09-01 implementation Ministry of Ecology and Environment released

Content

Foreword...ii 1 Scope...1 2 Normative references...1 3 Principles of the method...1 4 Interference and elimination...1 5 Reagents and materials...1 6 Instruments and Equipment...2 7 samples... 2 8 Analysis steps...4 9 Calculation and representation of results...5 10 Precision and Accuracy...6 11 Quality Assurance and Quality Control...7 12 Waste Treatment...7 The detection limit and lower limit of determination of Appendix A (normative appendix) method...8 Appendix B (informative) method of precision and accuracy...9

Foreword

Protect the ecology for the implementation of the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control The environment, the protection of human health, the determination of sulfonylurea pesticides in water, the development of this standard. This standard specifies high performance liquid chromatography for the determination of sulfonylurea pesticides in water. This standard is the first release. Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix. This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment. This standard was drafted. Qingdao Environmental Monitoring Center Station and Qingdao Technological University. This standard is verified by. Agricultural Products Quality and Safety Supervision, Inspection and Testing Center (Qingdao), Weihai City Environment Protection monitoring station, Tai'an Environmental Protection Monitoring Station, Zibo Environmental Monitoring Station, Qingdao Hua Testing Technology Co., Ltd. and Mountain Dong Hengcheng Testing Technology Co., Ltd. This standard is approved by the Ministry of Ecology and Environment on April 13,.2019. This standard has been implemented since September 1,.2019. This standard is explained by the Ministry of Ecology and Environment. Water quality - Determination of sulfonylurea pesticides - High performance liquid chromatography Warning. The organic solvents and standard solutions used in the experiments have certain toxicity and volatility, reagent preparation and sample preparation. Cheng should be carried out in a fume hood, and protective equipment should be worn as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies high performance liquid chromatography for the determination of sulfonylurea pesticides in water. This standard applies to surface water, groundwater, domestic sewage and industrial wastewater in nicosulfuron, thifensulfuron, metsulfuron-methyl, sulfometurm Determination of 10 Sulfonylurea Pesticides such as Long, Etherbensulfuron, Chlorosulfuron, Amisulfuron, Bensulfuron, Pyrazosulfuron and Chlorsulfuron set. With direct injection, when the injection volume is 50 μl, the detection limit of the method is 0.006 mg/L to 0.009 mg/L, and the lower limit of determination is 0.024 mg/L to 0.036 mg/L; using liquid-liquid extraction or solid phase extraction, sampling 250 ml, the sample has a constant volume of 1.0 ml, and the sample is injected. When the volume is 20 μl, the detection limit is 0.05 μg/L to 0.09 μg/L, and the lower limit of determination is 0.20 μg/L to 0.36 μg/L. See the appendix for details. A.

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard. quasi. HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

The sample is separated by direct injection, liquid-liquid extraction or solid phase extraction, and separated by high performance liquid chromatography with a UV detector. According to the retention time qualitative, the external standard method is quantitative.

4 interference and elimination

4.1 When the water sample contains organic matter that interferes with the determination of the target compound, it can be purified by changing the chromatographic conditions or using a silica gel column. Except for some interference. 4.2 Under the conditions of this standard, bensulfuron-methyl with bensulfuron-methyl, ethersulfuron and metsulfuron-methyl, ethoxysulfuron and chlorsulfuron, 3,6-dichloro Peak concentration of -2-methoxybenzoic acid (dicamba) with metsulfuron-methyl, 4-(2,4-dichlorophenoxy)-butyric acid (2,4-DB) and chlorsulfuron-methyl Stacking, interference with the measurement.

5 reagents and materials

Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis, and the experimental water was pure water containing no target. 5.1 Phosphoric acid. ρ(H3PO4) = 1.69 g/ml. 5.2 sodium thiosulfate (Na2S2O3). 5.3 Sodium chloride (NaCl). After burning at 400 ° C for 2 h, after cooling, it was sealed and stored in a ground glass bottle. 5.4 anhydrous sodium sulfate (Na2SO4). After burning at 400 ° C for 2 h, after cooling, it was sealed and stored in a ground glass bottle. 5.5 sodium hydroxide (NaOH). 5.6 Sodium hydroxide solution. c (NaOH) = 0.1 mol/L. Weigh 0.4 g of sodium hydroxide (5.5) dissolved in water and dilute to 100 ml with water. 5.7 Acetonitrile (CH3CN). Pure by liquid chromatography. 5.8 Methanol (CH3OH). pesticide residue grade. 5.9 Dichloromethane (CH2Cl2). pesticide residue grade. 5.10 Acetonitrile solution. 20 80. Mix 20 ml of acetonitrile (5.7) with 80 ml of water. 5.11 Standard stock solution of sulfonylurea pesticide. ρ=100 mg/L. Direct purchase of commercially available nicosulfuron, thifensulfuron, metsulfuron, mesulfuron, ethersulfuron, chlorsulfuron, ethamsulfuron, bensulfur Sulfuric acid, pyrazosulfuron-methyl, chlorsulfuron-methyl standard solution, according to the standard certificate requirements. 5.12 C18 solid phase extraction column. 1000 mg/6 ml. 5.13 Silica gel purification column. 1000 mg/6 ml. 5.14 Membrane. 0.45 μm PTFE membrane. 5.15 Nitrogen. purity ≥99.99%

6 Instruments and equipment

6.1 High Performance Liquid Chromatograph. UV detector or diode array detector. 6.2 Column. C18 reversed-phase column with a particle size of 5 μm, a column length of 25 cm, an internal diameter of 4.6 mm, or other equivalent columns. 6.3 Sampling bottle. 1000 ml brown thin-mouthed glass bottle with grinder or brown threaded glass bottle with Teflon liner. 6.4 Solid phase extraction device. automatic solid phase extraction instrument or other solid phase extraction device. 6.5 Concentration device. nitrogen blower, rotary evaporator, etc. 6.6 Separating funnel. 500 ml with Teflon stopper. 6.7 Microinjectors. 10 μl, 50 μl and 100 μl. 6.8 Common instruments and equipment used in general laboratories.

7 samples

7.1 Sample collection and preservation Sample collection was performed in accordance with the relevant regulations of HJ/T 91 and HJ/T 164. When collecting samples, the sample should be filled with sample bottles, not Leave liquid on the space. If the pH of the sample is not between 7 and 9, adjust the pH of the sample to 7~ with phosphoric acid (5.1) or sodium hydroxide solution (5.6). 9. For water samples containing residual chlorine, sodium thiosulfate (5.2) should be added to the water sample so that the concentration of sodium thiosulfate in the water sample is 80 mg/L. The collected samples should be stored at 4 °C or less, stored in the dark, and analyzed or extracted within 2 days. The extract should be refrigerated below 4 °C. Stored in the dark and analyzed within 8 days. 7.2 Preparation of samples 7.2.1 Direct injection The water sample was filtered through a filter (5.14) and placed in a 2 ml vial for testing. 7.2.2 Liquid-liquid extraction 7.2.2.1 Extraction Take 250 ml of water sample and place it in a 500 ml separatory funnel. Add 2.5 g of sodium chloride (5.3) and dissolve it with phosphoric acid (5.1). The pH is about 3. After adding 20 ml of dichloromethane (5.9), the mixture was vented, shaken for 2 min, and allowed to stand for 15 min. After that, the organic phase was collected in a triangular flask. Add 15 ml of dichloromethane (5.9) to the aqueous phase, repeat the extraction twice, and combine three times with organic Further, an appropriate amount of anhydrous sodium sulfate (5.4) was added for dehydration, and concentrated to 1 ml with a concentration apparatus (6.5) to be purified. For clean samples The product was directly concentrated to near dryness, and the volume was adjusted to 1.0 ml with an acetonitrile solution (5.10), and filtered through a filter (5.14) into a sample vial for testing. Note. Some sulfonylurea pesticides are unstable in acidity, and the sample should be extracted immediately after adjusting the pH to about 3. 7.2.2.2 Purification For complex water samples, the concentrated extract should be purified. Add 10 ml of dichloromethane (5.9) to the silica gel purification column (5.13), before the filler is to be exposed to air, transfer the concentrate to be purified (7.2.2.1) to the purification column and start collecting. Eluent. The concentrate bottle was washed with 5 ml of dichloromethane (5.9) and transferred to a purification column, which was repeated 2 times to collect all the eluents. Blow to near dryness with a nitrogen blower, dissolve with acetonitrile solution (5.10) and dilute to 1.0 ml, and filter into the sample vial with filter membrane (5.14). Measurement. 7.2.3 Solid phase extraction 7.2.3.1 Column activation The solid phase extraction column (5.12) was fixed on a solid phase extraction unit (6.4). 5 ml methanol (5.8) at a flow rate of about 2 ml/min Through the SPE column, add 10 ml of water to the column before the packing is exposed to air. When the water is about 2 ml left, close the valve. 7.2.3.2 Enrichment A 250 ml sample was placed in a triangular flask and the pH was adjusted to 3-6 with phosphoric acid (5.1). Passing activation at a flow rate of approximately 2 ml/min After the solid phase extraction column, after the sample is completely enriched, continue to pump for 5 min or purge with nitrogen (5.15) to dry the column. Then add Elution was carried out by adding 15 ml of methanol (5.8), and the eluate was collected in a concentrate bottle. The concentrated bottle was placed on a nitrogen gasifier (6.5) and concentrated to 60 ° C. Dry, dilute with acetonitrile solution (5.10) and dilute to 1.0 ml, filter into the sample vial with filter (5.14), and test. 7.3 Preparation of blank samples The test water was used instead of the sample, and the preparation of the blank sample was carried out in the same manner as in the sample preparation (7.2).

8 Analysis steps

8.1 Chromatographic Reference Conditions Mobile phase A. acetonitrile, mobile phase B. aqueous phosphoric acid solution (0.02% phosphoric acid); flow rate. 1.0 ml/min; detection wavelength. 230 nm; Injection volume. direct injection was 50.0 μl, liquid-liquid extraction and solid phase extraction were 20.0 μl; column temperature. 40 ° C; gradient elution procedure is shown in Table 1. Table 1 Gradient elution procedure Time (min) mobile phase A (%) mobile phase B (%) 10~22 35 65 27～32 40 60 35～45 45 55 50～55 90 10 60~70 20 80 Note. 50 min ~ 55 min is used to clean the column, the cleaning time can be adjusted according to the complexity of the actual sample. 60 Min~70 min is the equilibrium time of the column. 8.2 Establishment of calibration curve 8.2.1 Direct injection Take appropriate amount of sulfonylurea pesticide standard stock solution (5.11), and prepare a standard series of at least 5 concentration points by dilution with water. The mass concentrations of the components were 0.050 mg/L, 0.100 mg/L, 0.500 mg/L, 2.00 mg/L, and 10.0 mg/L, respectively (this is the reference concentration). The sample is injected sequentially from a low concentration to a high concentration, and the mass concentration of the target compound in the standard series solution is plotted on the abscissa, corresponding peak height or peak. The area is the ordinate and a calibration curve is established. 8.2.2 Liquid-liquid extraction and solid phase extraction Take appropriate amount of sulfonylurea pesticide standard stock solution (5.11), and prepare at least 5 concentrations by gradual dilution with acetonitrile solution (5.10). The standard series of points, the mass concentration of each component is 0.100 mg/L, 0.500 mg/L, 2.00 mg/L, 5.00 mg/L, 10.0 mg/L (This is the reference concentration). The sample is injected sequentially from a low concentration to a high concentration, and the mass concentration of the target compound in the standard series solution is plotted on the abscissa. The corresponding peak height or peak area is the ordinate, and a calibration curve is established. 8.3 Determination The measurement of the sample (7.2) was carried out under the same conditions as the establishment of the calibration curve (8.2). 8.4 Blank test The blank sample (7.3) was measured under the same conditions as the sample measurement (8.3).

9 Calculation and representation of results

9.1 Qualitative analysis Qualitative according to the retention time of the target compound in the sample and the target compound in the standard series, standard addition method, no Assisted by methods such as absorption ratio at the same wavelength or scanning ultraviolet absorption spectroscopy. If necessary, liquid chromatography-tandem mass spectrometry should be used for The standard compound is confirmed. The standard chromatograms of the 10 sulfonylurea pesticides are shown in Figure 1 under the chromatographic reference conditions (8.1) specified in this standard. 1-nicotsulfuron-methyl; 2-thiensulfuron-methyl; 3-methylsulfuron-methyl; 4-sulfuron-methyl; 5-ethersulfuron-methyl; 6-chlorosulfuron; 7-amibensulfuron; 8-bensulfuron-methyl; 9-pyrimsulfuron-methyl; 10-chlorosulfuron-methyl. Figure 1 Standard chromatogram of sulfonylurea pesticides (ρ = 0.500 mg/L) 9.2 Quantitative analysis 9.2.1 Direct injection The mass concentration ρi (mg/L) of the target compound in the sample is calculated according to the formula (1). (1) Where. ρi--the mass concentration of the target compound i in the sample, mg/L; Ai--the peak area or peak height of the target compound i; A--the intercept of the target compound i calibration curve; B--the slope of the target compound i calibration curve; D-- dilution factor. 9.2.2 Liquid-liquid extraction and solid phase extraction The mass concentration ρi (μg/L) of the target compound in the sample is calculated according to the formula (2). 10DVρ 1si  (2) 0 5 10 15 20 25 30 35 40 Min 8 9 10 colors aAi i  = Where. ρi - the mass concentration of the target compound i in the sample, μg/L; Ρis--calculate the mass concentration of target compound i in the sample from the calibration curve, mg/L; V1--the volume of the volume after preparation of the sample, ml; V--sampling volume, ml; D--dilution factor. 9.3 Result representation The number of decimal places in the measurement result is consistent with the method detection limit, and up to 3 significant digits are reserved. 10 Precision and accuracy 10.1 Precision 6 laboratories used direct injection to 10 sulfonylurea pesticides with concentrations of 0.020 mg/L, 0.500 mg/L, 8.00 mg/L The wastewater spiked samples were tested six times. the relative standard deviations in the laboratory were. 0.9% to 19%, 0.2% to 13%, 0.1%~13%; the relative standard deviations between laboratories are. 6.2%~20%, 5.1%~8.2%, 6.8%~9.1%; repetitive limit r respectively It is. 0.004 mg/L~0.006 mg/L, 0.063 mg/L~0.084 mg/L, 0.89 mg/L~1.3 mg/L; the reproducibility limit R is 0.005 Mg/L~0.012 mg/L, 0.11 mg/L~0.13 mg/L, 1.7 mg/L~2.2 mg/L. 6 laboratory liquid-liquid extraction of 10 sulfonylurea pesticides with surface concentrations of 0.200 μg/L, 2.00 μg/L, and 32.0 μg/L The spiked samples were tested six times. the relative standard deviations in the laboratory were. 2.7%~20%, 1.8%~20%, 1.4%~16%; The relative standard deviations between laboratories were. 12%~21%, 11%~23%, 14%~22%; the repeatability limits r were. 0.05 μg/L~0.07 Gg/L, 0.30 μg/L~0.56 μg/L, 4.7 μg/L~7.8 μg/L; reproducibility limit R. 0.07 μg/L~0.11 μg/L, 0.69 μg/L~1.2 Gg/L, 12 μg/L~19 μg/L. 6 laboratory liquid-liquid extraction of 10 sulfonylurea pesticides with a concentration of 2.00 μg/L of domestic sewage and 32.0 μg/L of industrial wastewater The spiked samples were subjected to 6 replicate measurements. the relative standard deviations in the laboratory were. 2.7% to 19%, 1.2% to 21%; The relative standard deviations were. 6.5%~21%, 11%~20%; the repeatability limits r were. 0.36 μg/L~1.0 μg/L, 4.2 μg/L~11 Gg/L; Reproducibility limits R are. 0.57 μg/L to 1.2 μg/L, and 11 μg/L to 17 μg/L. 6 laboratory solid phase extractions for 10 sulfonylurea pesticides with surface concentrations of 0.200 μg/L, 2.00 μg/L, and 32.0 μg/L The spiked samples were tested in 6 replicates. the relative standard deviations in the laboratory were. 0.9% to 21%, 1.3% to 17%, and 0.6% to 20%; The relative standard deviations between laboratories were. 9.9%~17%, 12%~25%, 9.0%~18%; the repeatability limits r were. 0.04 μg/L~0.07 Gg/L, 0.20 μg/L~0.42 μg/L, 3.8 μg/L~8.1 μg/L; reproducibility limits R. 0.06 μg/L~0.09 μg/L, 0.63 μg/L~1.2 Gg/L, 9.2 μg/L~15 μg/L. 10.2 Accuracy The concentration of sulfonylurea-containing pesticides in 6 laboratories was (0~0.093) mg/L, (0~2.01) mg/L, (0~24.2). The industrial wastewater of mg/L was spiked with 0.500 mg/L and analyzed by 6 replicates. the average of 10 sulfonylurea pesticides The recoveries ranged from 97.4% to 104%, 90.5% to 107%, and 83.1% to 103%. The final values of the spiked recovery are. 97.4%±13.6%~104%±14.0%, 90.5%±23.2%~107%±19.8%, 83.1%±18.6%~103%±25.8%. 6 laboratory liquid-liquid extractions were performed on surface water samples with spiked concentrations of 0.200 μg/L, 2.00 μg/L, and 32.0 μg/L. The repeated analysis showed that the average spiked recoveries of 10 sulfonylurea pesticides ranged from 80.5% to 86.8% and 84.2% to 95.6%, respectively. 78.4%~91.1%; the final recoveries of the spiked recovery are. 80.5%±24.0%~86.8%±25.0%, 80.5%±24.0%~95.6%±25.8%, 78.4% ± 22.4% ~ 91.1% ± 30.0%. 6 laboratory liquid-liquid extraction pairs of domestic sewage samples with a concentration of 2.00 μg/L, the concentration of sulfonylurea-containing pesticides was (0~71.3) μg/L industrial wastewater spiked with 32.0 μg/L sample was analyzed by 6 replicates. 10 sulfonylurea pesticides The average spike recovery rates ranged from. 76.4% to 101%, 81.9% to 92.6%; the final values of the spiked recovery were. 78.9%±27.0%~101%±26.6%, 81.9%±11.0%~92.6%±28.0%. 6 laboratory solid phase extractions were performed on surface water samples with spiked concentrations of 0.200 μg/L, 2.00 μg/L, and 32.0 μg/L. The repeated analysis showed that the average recoveries of the 10 sulfonylureas ranged from 78.2% to 89.4% and 81.4% to 92.9%. 80.3%~88.8%. The final recoveries of the spiked recovery were. 78.2%±20.2%~89.4%±24.6%, 81.7%±39.0%~92.9%±27.0%, 80.3% ± 27.6% ~ 88.8% ± 17.8%. See Appendix B for precision and accuracy results. 11 Quality Assurance and Quality Control 11.1 Blank test At least one laboratory blank should be made for every 20 samples or batches (≤20 samples/batch), and the results should be lower than the method detection. limit. 11.2 Calibration The correlation coefficient of the calibration curve is ≥0.995. Every 10 samples or batches (≤10 samples/batch) should be measured in a calibration curve For the intermediate concentration point standard solution, the relative error between the measurement result and the concentration at this point should be within ±15%. 11.3 Parallel samples A parallel sample should be made for every 20 samples or batches (≤ 20 samples/batch). For direct injection, the relative bias of parallel samples The difference is ≤ 30%. For liquid-liquid extraction and solid phase extraction, the relative deviation of the parallel samples is ≤ 35%. 11.4 Matrix addition A matrix plus standard should be made for every 20 samples or batches (≤ 20 samples/batch). For direct injection, the substrate is labeled back The yield should be between 70% and 130%. For liquid-liquid extraction and solid-phase extraction, the recovery of matrix spikes should be between 60% and 130%. 12 Waste treatment The organic waste liquid generated in the experiment should be collected and stored in a centralized manner, and the corresponding signs should be marked and entrusted to qualified units for processing.

Appendix A

(normative appendix) Method detection limit and lower limit of determination Table A.1 gives the method detection limits and lower limit of determination for 10 sulfonylurea pesticides. Table A.1 Detection limits and lower limit of determination of the method Pesticide name English name CAS number Direct injection liquid-liquid extraction solid phase extraction The detection limit (mg/L) Lower limit of measurement (mg/L) The detection limit (μg/L) Lower limit of measurement (μg/L) The detection limit (μg/L) Lower limit of measurement (μg/L)

1 Nicosulfuron

Nicosul- Furon -09-4 0.009 0.036 0.05 0.20 0.05 0.20

2 thifensulfuron

Thifensul- Furonmethyl -27-3 0.009 0.036 0.05 0.20 0.07 0.28

3 metsulfuron

Metsulfuron- Methyl -64-6 0.006 0.024 0.06 0.24 0.09 0.36

4 sulfometuron

Sulfome- Turonmethyl -97-2 0.006 0.024 0.06 0.24 0.07 0.28

5 ether sulfonate

Triasul- Furon -50-5 0.009 0.036 0.06 0.24 0.09 0.36

6 chlorsulfuron

Chlorsul- Furon -72-3 0.006 0.024 0.07 0.28 0.09 0.36

7 acesulfame

Ethametsul- Furonmethyl -06-8 0.009 0.036 0.09 0.36 0.08 0.32 8 bensulfuron-methyl Bensulfuron- Methyl -99-6 0.009 0.036 0.09 0.36 0.06 0.24

9 pyrazosulfuron

Pyrazosul- Furonethyl -74-6 0.006 0.024 0.06 0.24 0.06 0.24 10 chlorsulfuron Chlorimuron -ethyl -32-4 0.006 0.024 0.06 0.24 0.09 0.36

Appendix B

(informative appendix) Method precision and accuracy Tables B.1 to B.6 show the precision and accuracy of the 10 sulfonylurea pesticides, respectively. Table B.1 Precision of direct injection of industrial wastewater Serial number of pesticide name Standard concentration (mg/L) Mean value (mg/L) Experimental room relative standard deviation(%) Interlaboratory standard deviation(%) Reproducibility limit r(mg/L) Reproducibility limit R(mg/L)

1 Nicosulfuron

0.020 0.019 1.7～16 16 0.005 0.009 0.500 0.518 0.4～13 5.1 0.084 0.11 8.00 7.55 0.8～11 6.8 1.1 1.8

2 thifensulfuron

0.020 0.019 0.9～19 8.1 0.004 0.006 0.500 0.509 0.3~9.5 7.3 0.065 0.12 8.00 7.54 0.8～11 8.8 1.1 2.1

3 metsulfuron

0.020 0.020 1.4～14 11 0.004 0.020 0.500 0.513 0.4～9.2 7.3 0.064 0.12 8.00 7.54 0.8～10 9.1 1.1 2.2

4 sulfometuron

0.020 0.020 1.5～14 16 0.005 0.020 0.500 0.507 0.4～9.0 6.9 0.065 0.12 8.00 7.48 0.7～10 7.1 0.89 1.7

5 ether sulfonate

0.020 0.020 2.6～16 11 0.006 0.020 0.500 0.519 0.3～10 6.3 0.074 0.12 8.00 7.85 0.7～12 7.6 1.3 2.1

6 chlorsulfuron

0.020 0.019 1.7～15 11 0.004 0.019 0.500 0.511 0.2～9.1 7.8 0.063 0.13 8.00 7.56 0.8～10 9.0 0.94 2.1

7 acesulfame

0.020 0.019 1.9～16 6.2 0.004 0.019 0.500 0.510 0.2～9.4 7.5 0.068 0.13 8.00 7.82 0.1～13 8.8 1.1 2.2 8 bensulfuron-methyl 0.020 0.020 1.1～11 10 0.004 0.020 0.500 0.505 0.2～8.9 8.2 0.065 0.13 8.00 7.53 0.7～13 7.6 1.1 1.9

9 pyrazosulfuron

0.020 0.020 1.9～16 11 0.006 0.020 0.500 0.509 0.4～9.2 7.6 0.063 0.13 8.00 7.82 0.3~12 7.5 1.0 1.9 10 chlorsulfuron 0.020 0.020 1.6～16 20 0.004 0.021 0.500 0.523 0.7～8.7 7.5 0.066 0.13 8.00 7.41 1.1～12 8.9 1.3 2.2 Table B.2 Precision of liquid-liquid extraction Serial number pesticide name sample type Standard concentration (μg/L) Mean value (μg/L) Experimental indoor phase Standard deviation (%) Interlaboratory phase Standard deviation (%) Reproducibility limit r(μg/L) Reproducibility limit R (μg/L)

1 Nicosulfuron

Surface water 0.200 0.17 3.9~16 15 0.05 0.08 2.00 1.66 5.2~15 19 0.38 0.95 32.0 27.7 1.6～10 18 4.7 15 Domestic sewage 2.00 1.64 9.5~15 20 0.61 1.1 Industrial wastewater 32.0 25.9 3.5～20 11 8.2 11 2 thi...

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