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HJ 851-2017Water quality - Determination of methomyl and methomyl-oxime - High performance liquid chromatography (English PDF)

水质灭多威和灭多威肟的测定液相色谱法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

August 28, 2017

Implementation date

November 1, 2017

Scope

HJ 851-2017 is the English-translated version of 水质灭多威和灭多威肟的测定液相色谱法.

HJ 851-2017 — This standard specifies the determination of methotrexate and methotrexate in water by liquid chromatography. This standard applies to the determination of methomyl and methotrexate in surface water, groundwater, domestic sewage and industrial waste water.

When the injection volume was 50 µl, the detection limit of methomyl and methomyloxime was 1 µg/L, and the lower limit of determination was 4 µg/L.

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Document preview — HJ 851-2017

National Standard of the People's Republic of China

Classification: Z 16

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Normative reference documents
3 Principle of the method
4 Interference and elimination
5 Reagents and materials
6 Instruments and equipment
7 Samples
7.1 Sample collection and storage
7.2 Sample preparation
7.3 Preparation of blank samples
8 Analysis steps
8.1 Chromatographic reference conditions
8.2 Calibration curve establishment
8.3 Determination
8.4 Blank test
9 Results calculation and representation
9.1 Qualitative analysis
9.2 Quantitative analysis
10 Precision and accuracy
10.1 Precision
10.2 Accuracy
11 Quality assurance and quality control
11.1 Blank test
11.2 Initial calibration
11.3 Standard curve verification
11.4 Parallel samples
11.5 Matrix spikes
12 Waste treatment

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, the protection of human health, regulate the water Dudu Wei and methomyl oxime determination method, the development of this standard.

This standard specifies the determination of methotrexate and methotrexate in water by liquid chromatography.

This standard is the first release.

Appendix A to this standard is an informative appendix.

This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection and the Department of Science and Technology Standards.

The main drafting unit of this standard. Qingdao Environmental Monitoring Center Station and Qingdao University of Technology.

The main verification unit of this standard. Ministry of Agriculture, agricultural quality and safety supervision and inspection test center (Qingdao), Shandong Province Environmental Supervision Measuring center station, Jinan City Environmental Monitoring Center Station, Tai'an City Environmental Protection Monitoring Station, Liaoning North Environmental Testing Technology Co., Ltd.

Division and Qingdao in a monitoring Limited.

The environmental protection department of this standard approved on August 28, 2017.

This standard has been implemented since November 1, 2017.

This standard is explained by the Ministry of Environmental Protection.

Determination of water quality of methomyl and methotrexate by liquid chromatography Warning. methomyl and methomyloxime has some toxicity, the standard solution should be prepared in the operation of the fume hood, the operation should be in accordance with regulations it is required to wear protective equipment to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the determination of methotrexate and methotrexate in water by liquid chromatography.

This standard applies to the determination of methomyl and methotrexate in surface water, groundwater, domestic sewage and industrial waste water.

When the injection volume was 50 µl, the detection limit of methomyl and methomyloxime was 1 µg/L, and the lower limit of determination was 4 µg/L.

2 Normative reference documents

The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard.

Technical specification for surface water and wastewater monitoring Technical specification for groundwater environmental monitoring

3 Principle of the method

The methotrexate and methotrexate in water were injected directly by liquid chromatography with an ultraviolet detector. According to the reservation Qualitative and external standard method.

4 Interference and elimination

When the organic matter coexisting in the water sample interferes with the determination of the target compound can be determined by changing the chromatographic conditions, so that methomyl and methomyl Separate from the disturbance, or remove the water sample with n-hexane extraction to remove part of the interference, take the water phase for analysis.

5 Reagents and materials

Unless otherwise stated, analytical reagents conforming to national standards are used in the analysis. The test water is pure water containing no organic matter.

5.1 Hydrochloric acid. rho (HCl) = 1.18 g/ml.

5.2 hydrochloric acid solution. c (HCl) = 0.1 mol/L.

Accurately remove 3.1 ml of hydrochloric acid (5.1) in a small amount of water and dilute to 1 L.

5.3 sodium hydroxide (NaOH). excellent grade pure.

5.4 Sodium hydroxide solution. c (NaOH) = 0.1 mol/L.

Accurately weighed 4.0 g of sodium hydroxide dissolved in a small amount of water, diluted to 1 L.

5.5 Acetonitrile (CH3CN). Liquid Chromatography Pure.

5.6 methomyl. purity >= 98%.

5.7 methomyloxime. purity >= 98%.

5.8 methomyl and methomyloxime mixed standard stock solution. rho = 100 µg/ml.

Were weighed 0.010 g (exact to 0.1 mg) methotrexate (5.6) and methotrexate (5.7), dissolved in acetonitrile (5.5) to 100 ml, frozen at 4 °C, protected from light, can be stored for 12 months, or directly to buy a certified standard solution.

5.9 Methomyl and methomyloxime mixed standard liquid. rho = 10.0 µg/ml.

2 Accurately remove 1.00 ml of methomyl and methotrexate standard stock solution (5.8) and dilute to 10 ml with water.

6 Instruments and equipment

6.1 Sampling vials. 100 ml brown glass jar with a mouth plug.

6.2 Liquid Chromatograph. with UV detector or diode array detector.

6.3 Columns. 5 µm ODS with a column length of 25 cm, an internal diameter of 4.6 mm, or other equivalent columns.

6.4 Micro Samplers. 10 µl, 50 µl and 100 µl.

6.5 Filtration. 0.22 µm Teflon or nylon microporous membrane.

6.6 Common laboratory equipment and equipment.

7 Samples

7.1 Sample collection and storage

Samples were collected according to the relevant regulations of HJ/T 91 and HJ/T 164. After sample collection, use hydrochloric acid solution (5.2) or sodium hydroxide solution (5.4) adjusted to pH 4 ~ 6, protected from light, within 8 d analysis is completed.

7.2 Sample preparation

The water sample was filtered through a 0.22 µm filter (6.5) and placed in a 2 ml vial and tested.

Note. For samples containing organic matter, take 10 ml of water samples, with 2 ml of n-hexane extraction, take the water phase for determination.

7.3 Preparation of blank samples

The sample was prepared in the same manner as in Sample Preparation Step (7.2).

8 Analysis steps

8.1 Chromatographic reference conditions

Mobile phase B. water flow rate. 1.0 ml/min; column temperature. 30 °C; detection wavelength. 232 nm; injection volume.

50 µl. The elution procedure is shown in Table 1.

Table 1 elution program

Time (min) A (%) B (%) Note. After elution time of 6 min for cleaning the column, the cleaning time can be adjusted according to the complexity of the actual sample.

8.2 Calibration curve establishment

3 to take appropriate amount of methomyl and methomyloxime mixed standard use of liquid (5.9), diluted with experimental water to prepare at least 5 concentration points of the standard series, the concentration of methomyl and methomyloxime were 5.0, 50.0, 100, 500 and 1000 µg/L, respectively degree). From the low concentration to high concentration in turn to the standard series of samples into the standard series of solutions of the target compound concentration for the abscissa, Corresponding to the peak height or peak area for the vertical axis, the establishment of calibration curve.

8.3 Determination

The sample to be tested (7.2) was subjected to the same conditions as the calibration curve.

8.4 Blank test

The blank sample to be measured (7.3) was measured under the same conditions as the sample.

9 Results calculation and representation

9.1 Qualitative analysis

According to the retention time of the target compound in the sample and the target compound in the standard series. If necessary, the use of standard samples Tim Addition, different wavelength absorption ratio or scanning ultraviolet absorption spectroscopy and other methods to assist the qualitative.

The standard chromatograms of methomyl and methomyl oxime are shown in Fig. 1 under the chromatographic reference conditions (8.1) specified in this standard.

1-methomyl oxime; 2-methomyl.

Figure 1 Standardized chromatogram of methomyl and methotrexate

9.2 Quantitative analysis

The mass concentration of the target compound in the water sample is calculated according to the following formula.

aA x-= (1)

Where. - mass concentration of the target compound in the water sample, µg/L;

A - the peak area or peak height of the target compound;

a - the intercept of the calibration curve;

b - the slope of the calibration curve;

f - the dilution factor of the water sample.

9.3 The result is shown when the determination is greater than or equal to 100 µg/L, the data retain the three significant digits; when the determination is less than 100 µg/L, the retention 4 to integer bits.

10 Precision and accuracy

10.1 Precision

6 laboratories were charged with blank water, surface water and domestic sewage with a concentration of 10.0 µg/L, 100 µg/L, 800 µg/L samples were subjected to six repeated determinations. the relative standard deviations in the laboratory were. 0.8% ~ 7.3%, 0.3% ~ 4.3%, 0.1% ~ 2.9%, respectively. The relative standard deviations were 6.0% ~ 9.1%, 4.3% ~ 6.5%, 7.8% ~ 8.2%, respectively the reproducibility limit r is. 2 ~ 3 µg/L, 13 ~ 19 µg/L, 176 ~ 184, and the reproducibility limit r is. 1 µg/L, 6 ~ 7 µg/L, 18 ~ 36 µg/L µg/L; the relative standard deviations in the laboratory were. 1.4% ~ 12%, 0.4% ~ 5.0%, 0.1% ~ 1.9%; laboratory the relative standard deviations were. 3.0% ~ 9.9%, 4.2% ~ 6.7%, 6.2% ~ 7.9%, the repeatability r was 1 ~ 2 µg/L, 6 ~ 8 µg/L, 16 ~ 24 µg/L; reproducibility R. 2 ~ 3 µg/L, 13 ~ 20 µg/L, 141 ~ 181 µg/L.

The concentration of methicillin was 125 µg/L, 296 µg/L, 741 µg/L and the concentration of methomyloxoxom was 106 µg/L, µg/L, 249 µg/L of industrial wastewater samples were subjected to six repeated determinations. the relative standard deviations in the laboratory were.

1.3% ~ 8.4%, 0.1% ~ 4.2%, 0.2% ~ 2.8%; the relative standard deviation between the laboratory were. 10%, 3.4%, 6.1% L = 37 µg/L, 32 µg/L, 130 µg/L, and the expression of rituximab in the range of 15 µg/L, 15 µg/L, 29 µg/L, the relative standard deviations in the laboratory were 0.6% ~ 11%, 0.3% ~ 3.6%, 0.5% ~ 8.3%, respectively. The relative standard deviation the reproducibility limit r was. 28 µg/L, 10 µg/L, 29 µg/L, 44 µg/L, 71 µg/L.

10.2 Accuracy

6 laboratories were charged with blank water, surface water and domestic sewage with a concentration of 10.0 µg/L, 100 µg/L, 800 µg/L samples were analyzed and determined. the recoveries of methomyl were. 82.0% ~ 113%, 91.4% ~ 112%, 84.1% ~ the recoveries were 99.3% ± 18.0% ~ 102% ± 17.0%, 98.7% ± 8.4% ~ 101% ± 12.0% 98.6% ± 14.4% ~ 99.1% ± 16.2%. The recoveries of Madduoxime were 82.5% ~ 115%, 93.2% ~ 113%, 90.4% ~ 100% ± 19.8% ~ 106% ± 6.6%, 99.0% ± 10.6% ~ 101% ± 8.2%, and the recoveries were 100% 100% ± 13.2% ~ 101% ± 16.4%.

The concentration of methomyladol was 21 µg/L,.199 µg/L, 646 µg/L and the concentration of methomyloxoxom was 6 µg/L, 43 µg/L, 142 µg/L of industrial wastewater samples were labeled with methomyl and methotrexate 100 µg/L were measured by spiked determination.

The recoveries were 94.3% ~ 112%, 80.6% ~ 106% and 84.2 ~ 117%, respectively. The final recoveries were. 102% ± 14.4% 95.9% ± 18.2%, 95.3% ± 22.4%, respectively. The recoveries of spiradoxime were 93.3% ~ 109%, 92.7% ~ 115%, 92.8% ~ the final recoveries were 101% ± 13.0%, 104% ± 18.0% and 100% ± 13.6% respectively.

Details of precision and accuracy are given in Appendix A.

11 Quality assurance and quality control

11.1 Blank test

Every 20 samples or per batch (less than 20 samples) should be at least one lab blank, blank in the end of methomyl and methomyl of the concentration should be lower than the method detection limit.

11.2 Initial calibration

The correlation coefficient of the calibration curve is >=0.995.

11.3 Standard curve verification

5 per 20 samples or per batch (less than 20 samples) should be measured with a calibration curve in the middle of the standard solution, the results and the relative deviation of the concentration of the curve should be <= 15%. Otherwise, a new calibration curve should be established.

11.4 Parallel samples

Every 10 samples or each batch (less than 10 samples) should be a parallel sample, parallel to the relative deviation of <= 15%.

11.5 Matrix spikes

Every 20 samples or each batch (less than 20 samples) should be a matrix plus standard sample, the matrix spike recovery rate should be controlled at 80% ~ Within 120% of the range.

12 Waste treatment

The organic waste generated in the experiment should be collected and kept collectively and entrusted with qualified units for processing.

6 Appendix A

(Informative)

Method of precision and accuracy Tables A.1 and A.2 give the precision and accuracy of the method, respectively.

Table A.1 The precision of the method

Sample type compound average value (Mg/L) Relative standards in the laboratory deviation(%) Inter-laboratory relative standard deviation(%) Repetitive limit r (Mg/L) Reproducibility R (Mg/L) Blank water Methomyl 10 1.1 to 5.0 8.3 1 3 99 1.0 to 3.6 4.3 6 13 793 0.2 to 1.2 8.2 18 182 Methomyl oxime 10 1.9 to 4.2 8.7 1 3 99 1.1 to 4.1 5.4 8 17 801 0.3 to 1.7 6.7 24 153 Surface water Methomyl 10 0.8 to 7.3 9.1 1 3 100 0.6 to 3.8 6.5 6 19 791 0.1 to 2.9 7.8 36 176 Methomyl oxime 11 2.2 ~ 12 3.0 2 2 101 0.8 to 3.9 4.2 6 13 813 0.1 to 1.3 6.2 16 141 life Sewage Methomyl 10 1.0 to 7.1 6.0 1 2 101 0.3 to 4.3 6.1 7 18 794 0.4 ~ 2.2 8.2 28 184 Methomyl oxime 10 1.4 to 4.1 9.9 1 3 100 0.4 ~ 5.0 6.7 8 20 806 0.1 to 1.9 7.9 22 181 industry Waste water Methomyl 125 1.3 to 8.4 10 15 37 296 0.1 to 4.2 3.4 15 32 741 0.2 to 2.8 6.1 29 130 Methomyl oxime 106 0.6 ~ 11 7.9 16 28 145 0.3 to 3.6 10.6 10 44 249 0.5 to 8.3 9.4 29 71

7 Table A.2 Method of accuracy Sample type compound Sample concentration (Mg/L) Spiked concentration (Mg/L) Spiked recovery rate range(%) the final value of the recoveries 2 ± S (%) Blank water Methomyl 0 10.0 90.4 ~ 113 102 ± 17.0 0 100 96.8 to 104 98.7 ± 8.4 0 800 91.2 ~ 114 99.0 ± 16.2 Methomyl oxime 0 10.0 89.6 ~ 115 103 ± 18.0 0 100 93.2 to 106 99.0 ± 10.6 0 800 92.4 ~ 112 100 ± 13.2 Surface water Methomyl 0 10.0 82.0 ~ 107 99.3 ± 18.0 0 100 91.4 to 110 99.7 ± 13.0 0 800 88.7 to 110 98.6 ± 14.4 Methomyl oxime 0 10.0 102 to 112 106 ± 6.6 0 100 97.1 to 107 101 ± 8.2 0 800 96.3 ~ 111 101 ± 10.8 life Sewage Methomyl 0 10.0 93.7 to 110 101 ± 12.4 0 100 96.7 to 112 101 ± 12.0 0 800 84.1 to 108 99.1 ± 16.2 Methomyl oxime 0 10.0 82.5 ~ 111 100 ± 19.8 0 100 94.2 to 113 100 ± 13.4 0 800 90.4 to 114 101 ± 16.4 industry Waste water Methomyl 21 100 94.3 ~ 112 102 ± 14.4 199 100 80.6 ~ 106 95.9 ± 18.2 646 100 84.2 ~ 117 95.3 ± 22.4 Methomyl oxime 6 100 93.3 ~ 109 101 ± 13.0 43 100 92.7 ~ 115 104 ± 18.0 142 100 92.8 ~ 111 100 ± 13.6

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

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