HJ 1071-2019 English PDF

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HJ 1071-2019: Water quality--Determination of glyphosate--High performance liquid chromatography
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Basic data

Standard ID: HJ 1071-2019 (HJ1071-2019)
Description (Translated English): Water quality--Determination of glyphosate--High performance liquid chromatography
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 11,180
Date of Issue: 2019
Date of Implementation: 2020-06-30
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1071-2019: Water quality--Determination of glyphosate--High performance liquid chromatography

---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.
Water quality--Determination of glyphosate--High performance liquid chromatography National Environmental Protection Standard of the People's Republic of China Water quality determination of glyphosate High performance liquid chromatography Water quality-Determination of glyphosate -High performance liquid chromatography 2019-12-31 released 2020-06-30 implementation Released by the Ministry of Ecology and Environment

Contents

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Methodology ... 1 4 Interference and cancellation ... 1 5 Reagents and materials ... 1 6 Instruments and equipment ... 2 7 Sample ... 3 8 Analysis steps ... 3 9 Results calculation and representation ... 4 10 Precision and accuracy ... 5 11 Quality Assurance and Quality Control ... 6 12 Waste disposal ... 7

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 Water Pollution Control", protect the ecology Environment, protect human health, standardize the determination method of glyphosate in water, and formulate this standard. This standard specifies the HPLC method for the determination of glyphosate in surface water, groundwater, domestic sewage and industrial wastewater. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Nanjing Institute of Environmental Sciences, Ministry of Ecology and Environment. This standard is verified by. Jiangsu Environmental Monitoring Center, Anhui Ecological Environment Monitoring Center, Nanjing Environmental Monitoring Center, Jiangsu Province Measurement center, Jiangsu Changzhou Environmental Monitoring Center, Jiangsu Wuxi Environmental Monitoring Center and Jiangsu Taizhou Environmental Monitoring Center. This standard was approved by the Ministry of Ecology and Environment on December 31,.2019. This standard will be implemented from June 30, 2020. This standard is explained by the Ministry of Ecology and Environment. Water quality-Determination of glyphosate-High performance liquid chromatography Warning. Some solvents and standards used in the experiment have certain toxicity. The reagent preparation and sample preparation process should be It should be carried out in a fume hood. Protective equipment should be worn during operation to avoid contact with skin and clothing.

1 Scope

This standard specifies HPLC for the determination of glyphosate in water. This standard applies to the determination of glyphosate in surface water, groundwater, domestic sewage and industrial wastewater. When the injection volume is 20 μl, the detection limit of the method is 2 μg/L, and the lower detection limit is 8 μg/L.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. HJ 91.1 Technical Specifications for Sewage Monitoring HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Method principle

Trisodium citrate dihydrate was added to the sample at a pH of 4-9, and the sample was purified by filtration or solid phase extraction and filtered with 9- 芴 The methyl chloroformate (FMOC-Cl) was subjected to derivatization reaction, and the generated fluorescent product was extracted and purified by dichloromethane to remove the derivatization. After the by-products are converted, they are separated and detected by high performance liquid chromatography with a fluorescence detector. Characterized by retention time and characteristic wavelength, external Standard quantification.

4 Interference and cancellation

The metal ions in the sample will form a stable complex with glyphosate and interfere with the determination of glyphosate. Hydrated trisodium citrate eliminates interference.

5 Reagents and materials

Unless otherwise specified, analytical reagents that meet national standards are used in the analysis. Out of deionized water. 5.1 Acetonitrile (CH3CN). chromatographically pure. 5.2 Methanol (CH3OH). chromatographically pure. 5.3 Dichloromethane (CH2Cl2). chromatographically pure. 5.4 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 5.5 Phosphoric acid. ρ (H3PO4) = 1.69 g/ml, excellent purity. 5.6 Sodium hydroxide (NaOH). 5.7 Hydrochloric acid solution. 1 1. Measure 50 ml of hydrochloric acid (5.4) and slowly add to 50 ml of water. 5.8 Sodium hydroxide solution. c (NaOH) = 0.1 mol/L. Weigh 0.4 g of sodium hydroxide (5.6) in a small amount of water and make up to 100 ml. 5.9 Phosphoric acid solution. φ (H3PO4) = 0.2%. Take 2.0 ml of phosphoric acid (5.5) into a 1000 ml volumetric flask, dilute with water to the mark, and mix. 5.10 Trisodium citrate dihydrate (Na3C6H5O7 · 2H2O). 5.11 Sodium tetraborate decahydrate (Na2B4O7 · 10H2O). 5.12 Sodium tetraborate solution. c (Na2B4O7) = 0.05 mol/L. Weigh 1.91 g of sodium tetraborate decahydrate (5.11) in a small amount of water and make up to 100 ml. 5.13 9-fluorenyl methyl chloroformate (C15H11ClO2) standard. purity not lower than 99.0%, refrigerated below 4 ° C, protected from light. 5.14 9-fluorenyl methyl chloroformate acetonitrile solution. ρ (C15H11ClO2) = 1000 mg/L. Weigh 50 mg of 9-fluorenyl methyl chloroformate standard (5.13), dissolve with a small amount of acetonitrile (5.1), and transfer to a 50 ml container. In a measuring flask, dilute to the mark with acetonitrile (5.1) and mix. Refrigerate and protect from light below 4 ℃, the shelf life is 3 months. 5.15 Glyphosate (C3H8NO5P) Standard. The purity is not less than 99.0%, and refrigerated under 4 ° C, protected from light. 5.16 Glyphosate standard stock solution. ρ (C3H8NO5P) = 1000 mg/L. Accurately weigh 50.0 mg of glyphosate standard (5.15), dissolve in a small amount of water, transfer to a 50 ml volumetric flask, and dilute with water Release the volume to the mark and mix well. Refrigerate below 4 ° C, protect from light, shelf life is 6 months, or purchase certified standard solution directly. 5.17 Standard glyphosate solution. ρ (C3H8NO5P) = 10.0 mg/L. Take an appropriate amount of glyphosate standard stock solution (5.16), dilute with water, and prepare a glyphosate standard at a concentration of 10.0 mg/L. With liquid. Refrigerate and protect from light below 4 ℃, the shelf life is 2 months. 5.18 Filter membrane. 0.45 µm, hydrophilic polypropylene, glass fiber, hydrophilic PTFE or other equivalent materials.

6 Instruments and equipment

6.1 High Performance Liquid Chromatograph (HPLC). with fluorescence detector. 6.2 Column. Octadecyl bonded silica (C18) with 5 μm particle size, 250 mm column length, and 4.6 mm inner diameter Phase chromatography column, or other similar performance column. 6.3 Solid-phase extraction column. an extraction column packed with a copolymer of divinylbenzene and N-vinylpyrrolidone or octadecyl silica gel, Or equivalent extraction column, 500 mg/6 ml. 6.4 Polyethylene plastic (PE) tube. 10 ml. 6.5 Horizontal oscillator. 6.6 Vortex oscillator. 6.7 Brown sampling bottle. 250 ml or 500 ml screw-cap glass or ground bottle with Teflon liner. 6.8 Brown vial. 2.0 ml screw cap glass bottle with Teflon liner. 6.9 Instruments and equipment commonly used in general laboratories.

7 samples

7.1 Sample collection and storage Collect the samples in accordance with the relevant regulations of HJ 91.1, HJ/T 91 and HJ/T 164. Collect the sample with a brown sampling bottle (6.7) and collect the sample in a full bottle. If the pH of the collected sample is not between 4-9, use Adjust the pH to 4-9 with hydrochloric acid solution (5.7) or sodium hydroxide solution (5.8). Keep refrigerated and protected from light below 4 ℃, within 7 days Complete sample analysis. 7.2 Preparation of test specimens 7.2.1 Purification by solid phase extraction Activate the solid phase extraction column (6.3) with 6 ml of methanol (5.2) and 6 ml of water in order to ensure that the column head is infiltrated. measure For a 10 ml sample, add 29.3 mg of trisodium citrate dihydrate (5.10) and mix well at about 3 ml/min (about 1 drop/second). The flow rate was passed through a solid-phase extraction column, and the purified sample was collected and derivatized. Note 1. For samples with good cleanliness and no obvious interference to the determination of target compounds, trisodium citrate dihydrate can be added (5.10) After filtering directly through the filter membrane (5.18), it will be derived. Note 2. If the sample concentration is high, first dilute the sample, add trisodium citrate dihydrate (5.10), and then perform solid phase extraction purification, wait for the Raw. 7.2.2 Derivatization reaction Take 2.00 ml of the purified sample into a polyethylene plastic (PE) tube (6.4) and add 0.50 ml of sodium tetraborate solution (5.12), 1.00 ml of 9-fluorenyl methyl chloroformate acetonitrile solution (5.14), mix thoroughly and place on a horizontal shaker (6.5) Derived at 40 ° C for 1 h. 7.2.3 Liquid-liquid extraction purification Add 5 ml of dichloromethane (5.3) to the derivatized sample and vortex on a vortex shaker (6.6) for 2 min. Take the aqueous layer and filter it through a filter membrane (5.18). Collect 1 ml of the filtrate in a brown sample bottle (6.8) for testing. 7.3 Preparation of blank samples Use experimental water to replace the sample, and follow the same steps as the sample preparation (7.2) to prepare a laboratory blank sample.

8 Analysis steps

8.1 Reference conditions for liquid chromatography Mobile phase A. acetonitrile (5.1), mobile phase B. phosphoric acid solution (5.9), the gradient elution procedure is shown in Table 1; Flow rate. 1.0 ml/min; column temperature. 30 ° C; injection volume. 20 μl; Excitation wavelength. 254 nm; Emission wavelength. 302 nm as the detection wavelength and 315 nm as the auxiliary qualitative wavelength. Table 1 Gradient elution procedure Time (min) Mobile phase A (%) Mobile phase B (%) Note. 15 minutes to 20 minutes are used to clean the column. The cleaning time can be adjusted according to the complexity of the actual sample. 20 min ～ 25 min is the equilibration time of the column. 8.2 Establishment of working curve Take an appropriate amount of glyphosate standard use solution (5.17) and dilute with water to prepare a standard series of at least 5 concentration points, The mass concentration of glyphosate is 0 μg/L, 10 μg/L, 20 μg/L, 50 μg/L, 100 μg/L,.200 μg/L, 500 μg/L (This is the reference concentration). Perform derivatization reaction according to step 7.2.2, liquid-liquid extraction and purification according to step 7.2.3, and then according to the instrument reference conditions (8.1) Inject the standard series solution from low concentration to high concentration, take the concentration of glyphosate as the abscissa, and the corresponding chromatographic peak area Or the peak height is the ordinate to establish a working curve. 8.3 Sample determination The measurement of the sample (7.2) is carried out according to the same instrument conditions as the establishment of the working curve (8.2). 8.4 Blank test The blank sample (7.3) was measured under the same instrument 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, if necessary, standard addition method, fluorescence at different wavelengths can be used Intensity ratio and other methods assist qualitative analysis. Under the reference conditions of liquid chromatography recommended in this standard (8.1), the standard color of the derivative corresponding to the 100 g/L glyphosate solution The spectrum is shown in Figure 1. Figure 1 Standard chromatogram of glyphosate derivative 9.2 Quantitative analysis The glyphosate in the sample was quantified by external standard method, and the mass concentration of glyphosate was calculated according to formula (1). ρ = ρ × D (1) In the formula. ρ-mass concentration of glyphosate in the sample, μg/L; ρ1--the concentration of glyphosate calculated from the working curve, μg/L; D--The dilution factor of the sample. 9.3 Representation of results The number of digits after the decimal point in the measurement result is the same as the detection limit of the method. A maximum of 3 significant digits are retained. 10 Precision and accuracy 10.1 Precision Six laboratories performed six replicate determinations of surface water samples with glyphosate spiked concentrations of 10 µg/L and 100 µg/L. The relative standard deviations in the laboratory are 2.2% ~ 9.2%, 2.5% ~ 8.5%, and the relative standard deviations between laboratories are 6.8%, 6.3%; repeatability limits are 2 µg/L and 14 µg/L; reproducibility limits are 2 µg/L and 22 µg/L. Six laboratories performed 6 repeated determinations of groundwater samples with spiked concentrations of 10 µg/L and 100 µg/L. The relative standard deviations in the laboratories are 3.3% to 9.8% and 1.3% to 3.8%; the relative standard deviations in the laboratories are 5.1%, 4.8%; repeatability limits are 2 µg/L and 9 µg/L; reproducibility limits are 2 µg/L and 16 µg/L. Six laboratories performed 6 repeated determinations of glyphosate spiked domestic sewage samples at 10 µg/L and 100 µg/L. The relative standard deviations in the laboratory were 3.2% to 7.6% and 2.7% to 7.4%; the relative standard deviations between the laboratories were 6.1%, 8.4%; repeatability limits are 2 µg/L and 14 µg/L; reproducibility limits are 2 µg/L and 26 µg/L. min Six laboratories spiked industrial wastewater (glyphosate production) at concentrations of 10 µg/L, 100 µg/L, and 1000 µg/L Wastewater total discharge port) samples were tested 6 times repeatedly. the relative standard deviations in the laboratory were 2.4% ～ 9.5%, 3.5% ～ 7.8%, 1.6% to 8.4%; relative standard deviations between laboratories were 7.6%, 4.8%, and 8.4%; repeatability limits were 2 µg/L, 15 µg/L, 143 µg/L; reproducibility limits are 3 µg/L, 19 µg/L, and 265 µg/L. The six laboratories separately treated industrial wastewater containing glyphosate at an average concentration of 15 µg/L (the outlet of the glyphosate production wastewater workshop). Six replicates were spiked at 10 µg/L and 100 µg/L. the relative standard deviations in the laboratory were 0.8% to 9.8%, 2.2% ～ 4.7%, 0.9% ～ 6.5%; the relative standard deviations among laboratories are 8.4%, 4.3%, and 6.9%, respectively; They are 2 µg/L, 3 µg/L, 12 µg/L; the reproducibility limits are 4 µg/L, 4 µg/L, and 24 µg/L. 10.2 Accuracy Six laboratories analyzed and measured surface water samples with spiked concentrations of 10 µg/L and 100 µg/L. spiking The recoveries were 91.5% ～ 106%, 92.9% ～ 109%, and the final recoveries were 97.4% ± 13.0%, 98.7%. ± 12.4%. Six laboratories have analyzed and measured glyphosate groundwater samples with spiked concentrations of 10 µg/L and 100 µg/L. The recoveries were 89.4% to 103%, 92.9% to 107%, and the final recoveries were 98.7% ± 10.2% and 100%. ± 9.6%. Six laboratories analyzed and analyzed glyphosate for domestic sewage samples with spiked concentrations of 10 µg/L and 100 µg/L. The standard recovery rates are 88.5% to 105%, 85.0% to 108%, and the final recovery rates are 97.7% ± 12.0%, 97.6%. ± 16.6%. Six laboratories spiked industrial wastewater (glyphosate production) at concentrations of 10 µg/L, 100 µg/L, and 1000 µg/L The total waste water outlet) samples were analyzed and determined. the spiked recovery rates were 84.6% to 105%, 92.3% to 106%, and 89.7% to 111%, the final recoveries were 96.6% ± 14.4%, 98.9% ± 9.4%, 97.9% ± 16.8%. The six laboratories separately treated industrial wastewater containing glyphosate at an average concentration of 15 µg/L (the outlet of the glyphosate production wastewater workshop). Analyzed and spiked at 10 µg/L and 100 µg/L. The recoveries were 87.0% ～ 108%, 87.7% ～ 107%, The final recoveries were 97.7% ± 15.4% and 95.8% ± 13.4%. 11 Quality Assurance and Quality Control 11.1 Blank test At least one blank test shall be performed every 20 samples or each batch (less than 20 samples/batch). Legal detection limit. 11.2 Calibration Before analyzing samples, a working curve covering at least 5 concentration points in the sample concentration range should be established. The number of relationships should be ≥0.995. Every 20 samples or each batch (less than 20 samples/batch), a standard series intermediate concentration should be determined Point, the relative error between the measurement result and the concentration of this point in the working curve should be within ± 20%. Otherwise, a new work song should be created line. 11.3 Parallel samples Every 20 samples or each batch (less than 20 samples/batch) should take one parallel sample, and the relative deviation of parallel samples should be ≤20%. 11.4 Matrix Spiking Every 20 samples or each batch (less than 20 samples/batch) should be analyzed with a matrix plus standard sample. The yield should be between 70% and 130%. 12 Waste treatment The waste generated during the experiment should be collected in a centralized manner, be labeled accordingly, and be entrusted to a qualified unit for processing. ......

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