HJ 587-2010 English PDF

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HJ 587-2010: Water quality. Determination of Atrazine. High performance liquid chromatography
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
HJ 587-2010	239	Add to Cart	3 days	Water quality. Determination of Atrazine. High performance liquid chromatography	Valid

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Basic data

Standard ID: HJ 587-2010 (HJ587-2010)
Description (Translated English): Water quality. Determination of Atrazine. High performance liquid chromatography
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 9,944
Date of Issue: 2010-09-20
Date of Implementation: 2010-12-01
Regulation (derived from): Department of Environmental Protection Notice No. 68 of 2010
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the determination of atrazine by HPLC. This standard applies to surface water and groundwater in the determination of atrazine. When the sample volume is 100ml samples, the method detection limit is 0. 08��g/L, detection limit is 0. 32��g/L.

HJ 587-2010: Water quality. Determination of Atrazine. High performance liquid chromatography

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Water quality.Determination of Atrazine.High performance liquid chromatography National Environmental Protection Standard of the People's Republic Determination of water quality atrazine by high performance liquid chromatography Water quality-Determination of Atrazine-High performance liquid Gas chromatography Released on.2010-09-20 2010-12-01 Implementation Ministry of Environmental Protection released Ministry of Environmental Protection announcement No. 68 of.2010 In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve the "environmental air benzene series" Five standards, such as solid adsorption/thermal desorption-gas chromatography, are considered as national environmental protection standards and are released. The standard name and number are as follows. I. Determination of Benzene in Ambient Air Solid Adsorption/Thermal Desorption-Gas Chromatography (HJ 583-2010); 2. Determination of Benzene in Ambient Air Activated Carbon Adsorption/Carbon Disulfide Desorption - Gas Chromatography (HJ 584-2010); 3. Determination of free chlorine and total chlorine in water, N,N-diethyl-1,4-phenylenediamine titration method (HJ 585-2010); 4. Determination of free chlorine and total chlorine in water - N,N-diethyl-1,4-phenylenediamine spectrophotometric method (HJ 586-2010); The above standards have been implemented since December 1,.2010 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection. From the date of implementation of the above standards, the following four national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished. The name and number are as follows. I. Determination of Air Quality, Toluene, Xylene and Styrene by Gas Chromatography (GB/T 14677-93); 2. Determination of Air Quality Styrene by Gas Chromatography (GB/T 14670-93); 3. Determination of free chlorine and total chlorine in water. N,N-diethyl-1,4-phenylenediamine titration method (GB 11897-89); 4. Determination of free chlorine and total chlorine in water quality N,N-Diethyl-1,4-phenylenediamine spectrophotometric method (GB 11898-89). Special announcement. September 20,.2010

Content

Foreword..iv 1 Scope..1 2 Method principle..1 3 interference and elimination.1 4 Reagents and materials.1 5 instruments and equipment.1 6 samples. 2 7 Analysis steps..2 8 Results calculation and representation..3 9 precision and accuracy..3 10 Quality Assurance and Quality Control.4 Iv

Foreword

To protect the environment and protect the human body 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 Prevention and Control To develop and standardize the monitoring methods for atrazine in water. This standard specifies high performance liquid chromatography for the determination of atrazine in water. This standard was first developed. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Shanghai Environmental Monitoring Center. This standard is verified by. Jiangsu Environmental Monitoring Center, Zhejiang Environmental Monitoring Center, Shanghai Environmental Monitoring Center, Nanjing Environment Monitoring Center Station, Shanghai Municipal Center for Disease Control and Prevention. This standard was approved by the Ministry of Environmental Protection on September 20,.2010. This standard has been implemented since December 1,.2010. This standard is explained by the Ministry of Environmental Protection. Determination of water quality atrazine by high performance liquid chromatography

1 Scope of application

This standard specifies high performance liquid chromatography for the determination of atrazine in water. This standard applies to the determination of atrazine in surface water and groundwater. When the sample volume is 100 ml, the detection limit of this method is 0.08 μg/L, and the lower limit of determination is 0.32 μg/L.

2 Principle of the method

The method extracts atrazine in water with dichloromethane, and the extract is dried over anhydrous sodium sulfate, and concentrated to near dryness with methanol in a concentrator. The volume was measured by a high performance liquid chromatograph with a UV detector. Characterize by retention time and quantify by external standard method.

3 interference and elimination

There may be co-existing organic matter interference measurements on the UV detector in the water sample, and the Atrazine and interference can be made by changing the chromatographic conditions. Separate the object or select a diode array detector for qualitative confirmation.

4 reagents and materials

Unless otherwise stated, analytically pure reagents and distilled water containing no organic materials were used in the analysis. 4.1 Methanol, HPLC grade. 4.2 Dichloromethane, pesticide residue grade. 4.3 Atrazine standard stock solution, ρ = 100 μg/ml. Accurately weigh 0.010 0 g of atrazine standard sample, dissolve it with a small amount of dichloromethane, and then determine the volume to 100 ml with methanol. Standard stock solution for Atrazine. Store in a refrigerator at 4 ° C for half a year. 4.4 Atrazine standard use solution, ρ = 10.0 μg/ml. Take Atrazine standard stock solution (4.3) 1.00 ml in a 10.0 ml volumetric flask, make up to volume with methanol, mix well, and prepare for standard use. Solution. Store in a refrigerator at 4 ° C for half a year. 4.5 Anhydrous sodium sulfate. burned at 400 ° C for 4 h, cooled and sealed in a glass bottle. 4.6 Sodium chloride. ignite at 400 ° C for 4 h, cool and store in a glass bottle.

5 Instruments and equipment

Unless otherwise stated, the analysis used a Class A glass gauge in accordance with national standards. 5.1 High Performance Liquid Chromatograph. A tunable wavelength UV detector or diode array detector. 5.2 Column. Packing is 5.0 μm ODS, column length is.200 mm, inner diameter is 4.6 mm reversed phase column or other similar performance column. 5.3 Oscillator. Adjustable speed. 5.4 Concentration device. Rotary evaporation device or equivalent equipment such as KD concentrator and concentrator. 5.5 separatory funnel. 250 ml. 5.6 Common instruments in general laboratories.

6 samples

6.1 Acquisition and preservation Samples should be collected in brown glass containers. The water sample should be filled with the sample bottle and sealed, placed in a refrigerator at 4 ° C to protect from light. After sampling The sample should be extracted within 7 days. 6.2 Preparation of samples A 100 ml sample was weighed into a 250 ml separatory funnel using a graduated cylinder, and shaken by adding 5 g of sodium chloride (4.6). With 20 ml of dichloromethane (4.2) Two extractions, 10 ml each, were shaken well for 5 min on an oscillator (5.3). Note the manual shaking and deflation. After standing and layering, there will be The machine phase was passed through a funnel containing anhydrous sodium sulfate (4.5) to a concentrated bottle, taking care to rinse thoroughly with anhydrous sodium sulfate. Combine two dichlorocarbs Alkane extract. Concentrate to near dryness with a concentrator (5.4) and dilute to 1.00 ml with methanol (4.1) for analysis. The sample is stored in a refrigerator at 4 ° C In the middle, the analysis was completed within 40 days. Note. When the sample is concentrated during the concentration process, it should be immediately fixed to volume when it is concentrated to near dryness, otherwise Atrazine will have a large loss.

7 Analysis steps

7.1 Reference chromatographic conditions 7.1.1 Column. Reversed phase ODS column; 4.6 mm ×.200 mm, 5 μm 7.1.2 Mobile phase. methanol. water = 70.30 (volume fraction) 7.1.3 Flow rate. 0.8 ml/min 7.1.4 UV detection wavelength. 225 nm 7.1.5 Column temperature. 40 ° C 7.1.6 Injection volume. 10.0 μl 7.2 Calibration 7.2.1 Preparation of the standard series Take different amounts of Atrazine standard use solution (4.4), dilute with methanol (4.1), and make a concentration of 0.030, 0.050, 0.100, The standard series of 0.500 and 1.00 μg/ml are stored in brown vials and stored in a refrigerator at 4 °C. 7.2.2 Initial standard curve Transfer 10 μl of the standard concentration of 5 concentrations through the autosampler or sample loop, and inject into the liquid chromatograph to obtain different concentrations. The chromatogram of Atrazine. The chromatographic response is plotted on the ordinate and the concentration of atrazine is plotted on the abscissa. standard curve line The correlation coefficient is R≥0.999. 7.3 Sample Analysis It will be prepared according to the preparation of the 6.2 sample and according to the 7.1 chromatographic conditions. 7.4 Blank test While analyzing the sample, a blank test should be performed, that is, distilled water is used instead of the water sample. Blank samples should undergo all of the sample preparation and determination step. Check for contamination during the analysis.

8 Calculation and representation of results

8.1 Standard chromatogram Under the chromatographic conditions (7.1) specified in this standard, the standard chromatogram of atrazine is shown in Figure 1. Normalized 0 2 4 6 min 1--Atrazine (5.282 min). Figure 1 Atrazine standard chromatogram 8.2 Qualitative analysis The retention time of the sample is compared to the retention time of the standard solution. Used as a qualitative retention time window width to measure the day The actual retention time change is the baseline. 8.3 Quantitative analysis Calculate the concentration in the sample according to equation (1) using the external standard curve method. m V ρ ⋅= ⋅ (1) Where. ρ--the mass concentration of atrazine in the water sample, μg/L; M--the mass concentration of atrazine was found from the calibration curve, μg/ml; tV - the volume after concentration of the extract concentrate, ml; sV - the volume of the extracted water sample, ml.

9 Precision and accuracy

9.1 precision Five laboratory-based blank spiked samples containing atrazine concentrations of 1.0 μg/L and 5.0 μg/L were measured in five laboratories. The relative standard deviations in the experimental room were. 3.0% to 15%, 1.7% to 5.9%; The relative standard deviations between laboratories were. 8.2%, 3.9%; The repeatability limit is. 0.20 μg/L, 0.49 μg/L; Reproducibility limits are. 0.20 μg/L, 0.94 μg/L. 9.2 Accuracy Five laboratories tested uniform samples containing atrazine at a concentration of 2.0 μg/L. The relative error is. −16% to 1.0%; The final value of the relative error is. −9.5% ± 13%. The actual samples were spiked and analyzed in 3 laboratories, and the scalar weights were 1.0 μg and 5.0 μg, respectively. The recoveries of spiked standards were. 81.3%~92.1%, 85.9%~104%; The final recoveries were 88.1%±12% and 94.6%±18%. 10 Quality Assurance and Quality Control 10.1 Blank test There must be a full blank for each batch (20) of samples analyzed. All blank test results should be below the method detection limit. 10.2 Adding a standard 10.2.1 Each batch (20 samples) must have a blank plus standard for each sample; the component recovery rate is 70% to 120%. 10.2.2 Each sample (20 samples) must have one sample plus standard sample, and the component recovery rate is 70% to 120%. 10.3 Parallel samples There must be a parallel sample for each batch of samples (20 samples), and the relative error of the parallel samples is within 10%. 10.4 Calibration Standard Points 10.4.1 Use a standard solution of intermediate concentration for routine calibration before each analysis. The relative error of the measured value of the calibration point should be within 10%. The initial calibration curve is available for use. Otherwise, find the cause and take action; if you can't find the root cause of the problem after taking the action, you should redraw it. Calibration curve. 10.4.2 20 samples per interval or 1 batch (this batch is less than 20 samples) must be calibrated with a standard solution to recalibrate Leave time and window. ......

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