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HJ 1054-2019 English PDF

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HJ 1054-2019: Soil and sediment -- Determination of dithiocarbamate pesticides -- Headspace gas chromatography
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HJ 1054-2019299 Add to Cart 3 days Soil and sediment -- Determination of dithiocarbamate pesticides -- Headspace gas chromatography Valid

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Basic data

Standard ID: HJ 1054-2019 (HJ1054-2019)
Description (Translated English): Soil and sediment -- Determination of dithiocarbamate pesticides -- Headspace gas chromatography
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z18
Classification of International Standard: 13.080
Word Count Estimation: 13,160
Date of Issue: 2019
Date of Implementation: 2020-04-24
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1054-2019: Soil and sediment -- Determination of dithiocarbamate pesticides -- Headspace gas 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.
(Soil and sediment Determination of total dithiocarbamate (salt) pesticides Headspace/gas chromatography) National Environmental Protection Standard of the People's Republic of China Soil and sediment dithiocarbamates (salts) Determination of total pesticides by headspace/gas chromatography Soil and sediment-Determination of dithiocarbamate pesticides -Headspace gas chromatography 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment

Contents

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Methodology ... 2 5 Interference and cancellation ... 2 6 Reagents and materials ... 2 7 Instruments and equipment ... 3 8 Sample ... 3 9 Analysis steps ... 4 10 Calculation and Representation of Results ... 5 11 Precision and accuracy ... 6 12 Quality Assurance and Quality Control ... 7 13 Waste disposal ... 7 Appendix A (informative) Precision and accuracy of the method ... 8

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination method for the total amount of dithiocarbamate (salt) pesticides in soil and sediment Law to formulate this standard. This standard specifies the headspace/gas phase color of total dithiocarbamate (salt) pesticides in soil and sediment. Spectrum method. Appendix A of this standard is an informative appendix. 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. Hainan Environmental Monitoring Center Station. Verification units of this standard. Chongqing Ecological Environment Monitoring Center, Hubei Province Environmental Monitoring Center Station, Hainan Entry-Exit Inspection Inspection and Quarantine Technology Center of the Quarantine Bureau, Haikou Environmental Protection Monitoring Station, Sanya Environmental Monitoring Station, and Haikou Disease Prevention and Control System center. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Determination of total dithiocarbamate (salt) pesticides in soil and sediment Headspace/gas chromatography Warning. The chemical reagents used in the experiment are toxic and corrosive, and should be worn and protected according to regulations when operating Appliances to avoid contact with skin and clothing.

1 Scope

This standard specifies the headspace/gas phase color of total dithiocarbamate (salt) pesticides in soil and sediment. Spectrum method. This standard applies to the determination of total dithiocarbamate (salt) pesticides in soils and sediments. Or carbon disulfide meter. This standard does not apply to the determination of samples of soils and sediments containing hydroxanthic acid and its salts. When the sample size is 2 g, the time limit is measured with mancozeb, the detection limit of the method is 0.05 mg/kg, and the lower limit of determination is 0.20 mg/kg When carbon disulfide was used, the detection limit of the method was 0.03 mg/kg, and the lower limit of determination was 0.12 mg/kg.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. GB 17378.3 Marine Monitoring Code Part 3. Sample Collection, Storage and Transportation GB 17378.5 Marine Monitoring Code Part 5. Sediment Analysis HJ 494 Water Quality Sampling Technical Guide HJ 495 Water Quality Sampling Scheme Design Technical Regulations HJ 613 Soil dry matter and moisture determination by gravimetric method HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 166 Technical Specifications for Soil Environmental Monitoring

3 terms and definitions

The following terms and definitions apply to this standard. 3.1 Total dithiocarbamate pesticides Refers to pesticides containing dithiocarbamoyl in the molecular structure under the conditions specified in this standard Fumei Zinc, Fumei Iron, Daisen United, Daisen Manganese, Daisen Zinc, Daisen Sodium, Propyl Zinc, etc.) Based on mancozeb or carbon disulfide.

4 Method principle

At a certain temperature, dithiocarbamate (salt) pesticides in the soil or sediment in the headspace bottle The reaction of tin in the inorganic acid medium generates carbon disulfide. When the carbon disulfide reaches the thermodynamic equilibrium in the gas-liquid-solid three-phase, Carbon disulfide in the gas phase is separated by gas chromatography and detected by an electron capture detector (ECD). According to the meter of carbon disulfide Calculate the total amount of dithiocarbamate (salt) pesticides.

5 Interference and cancellation

Carbon disulfide in the sample will positively interfere with the determination of dithiocarbamate (salt) pesticides. Subtract the measurement result from the unacidified sample.

6 Reagents and materials

Unless otherwise specified, analytical reagents that comply with national standards are used in the analysis. The experimental water is freshly prepared pure water or Carbon Disulfide Free. 6.1 Sulfuric acid (H2SO4). ρ = 1.84 g/ml, excellent purity. 6.2 stannous chloride (SnCl2 · 2H2O). 6.3 Sodium chloride (NaCl). excellent grade pure. Bake at 400 ° C for 4 h in a muffle furnace, cool in a desiccator to room temperature, and transfer to a sealed glass bottle for storage. 6.4 Disodium ethylenediamine tetraacetate (C10H14N2O8Na2 · 2H2O). 6.5 L-cysteine hydrochloride (C3H7NO2S · HCl · H2O). 6.6 Sodium hydroxide (NaOH). 6.7 Sodium hydroxide solution. c (NaOH) = 10 mol/L. Weigh 20 g of sodium hydroxide (6.6) in a small amount of experimental water and dilute to 50 ml. 6.8 Sulfuric acid solution. c (H2SO4) = 3 mol/L. Take 81 ml of sulfuric acid (6.1), slowly pour it into experimental water, and dilute to volume to 500 ml. 6.9 EDTA-cysteine alkaline solution. Weigh 12.5 g of disodium ethylenediamine tetraacetate (6.4) and 12.5 g of L-cysteine hydrochloride (6.5) and add 800 ml Dissolve and mix the experiment water with sodium hydroxide solution (6.7) to adjust the pH to 9.0 ~ 10.0. 6.10 stannous chloride-sulfuric acid solution. ρ (SnCl2 · 2H2O) = 15 g/L. Weigh 7.5 g of stannous chloride (6.2), slowly add to 500 ml of sulfuric acid solution (6.8), dissolve and mix. 6.11 Mancozeb (C4H6N2S4MnZn). purity ≥97.5%. 6.12 Mancozeb standard stock solution. ρ = 100 μg/ml. Accurately weigh 50 mg (accurate to 0.1 mg) mancozeb (6.11), transfer to a 500 ml brown volumetric flask, add EDTA-cysteine alkaline solution (6.9) is dissolved and made up to volume. For 2 months. 6.13 Standard solution of mancozeb. 0.20 μg/ml ～ 20.0 μg/ml. Take an appropriate amount of mancozeb standard stock solution (6.12) in a 10 ml brown volumetric flask, and use EDTA-cysteine base. Solution (6.9) at constant volume, formulated as 0.20 μg/ml, 0.60 μg/ml, 1.00 μg/ml, 2.00 μg/ml, 6.00 μg/ml, 10.0 μg/ml and 20.0 μg/ml standard use solutions, ready for use, not less than 5 concentration points. 6.14 Quartz sand (SiO2). particle size 270 μm to 830 μm (50 mesh to 20 mesh). Bake at 160 ° C for 2 h before use. 6.15 Nitrogen. Purity ≥99.999%.

7 instruments and equipment

7.1 Gas chromatograph. with electronic capture detector (ECD, using 63Ni radiation source), with split/splitless inlet, Programmable heating. 7.2 Chromatographic column. Quartz capillary column. 30 m (length)  0.32 mm (inner diameter), the stationary phase is bonded silica or other High-efficiency capillary columns for light hydrocarbons and gas sulfides. 7.3 Automatic headspace sampler. headspace bottle (22 ml), seal (PTFE/siloxane material), cap (screw Cover or one-time use gland). 7.4 Constant temperature water bath oscillator. The oscillation frequency is 120 times/min. 7.5 Analytical balance. Sensitivity is 0.01 g and 0.1 mg. 7.6 Sampling bottle. Wide mouth brown ground glass bottle or brown screw mouth glass bottle with PTFE liner. 7.7 Instruments and equipment commonly used in general laboratories.

8 samples

8.1 Sample collection and storage Collection and preservation of soil samples in accordance with the relevant regulations of HJ/T 166; in accordance with GB 17378.3, GB 17378.5, The relevant regulations of HJ 494, HJ 495 and HJ/T 91 are used to collect and preserve sediment samples. The samples should be stored in clean sampling bottles (7.6), and protected from light, sealed and refrigerated during transportation. Such as temporarily Analysis, the samples should be stored under 4 ° C under cold storage for no more than 5 days. 8.2 Determination of moisture When weighing a sample, another sample is weighed for moisture determination. Determination of dry matter content in soil samples according to HJ 613 The water content of the sediment sample was measured in accordance with GB 17378.5. 8.3 Preparation of test specimens 8.3.1 Acid hydrolysis sample Remove stones and leaves from fresh samples and mix. Weigh 2 g (accurate to 0.01 g) sample and 3 g (fine Make sure that 0.1 g of sodium chloride (6.3) is added to a 22 ml headspace bottle, and 1.0 ml of EDTA-cysteine alkaline solution (6.9) is accurately added. And 7.0 ml of stannous chloride-sulfuric acid solution (6.10), immediately sealed. 120 ° C on a 80 ° C thermostatic water bath shaker (7.4) After 90 minutes of frequency/min oscillation, the analysis was completed within 24 hours. 8.3.2 Unacidified sample Remove stones and leaves from fresh samples and mix. Weigh 2 g (accurate to 0.01 g) sample and 3 g (fine Add 0.1 g of sodium chloride (6.3) to a 22 ml headspace bottle, add 8.0 ml of experimental water, and immediately seal it to 120 times. The analysis was completed within 24 hours after shaking at room temperature for 10 minutes. 8.4 Preparation of blank samples Quartz sand (6.14) was used in place of the sample, and blank samples were prepared in the same steps as in sample preparation (8.3).

9 Analysis steps

9.1 Instrument reference conditions 9.1.1 Headspace Sampler Reference Conditions Heating equilibrium temperature. 65 ℃; Heating equilibration time. 15 min; Sampling needle temperature. 90 ℃; Transmission line temperature. 115 ℃; Pressure time. 2 min; injection time. 0.04 min; needle removal time. 0.5 min. 9.1.2 Reference conditions for gas chromatography Inlet temperature. 210 ° C; carrier gas (6.15) flow rate. 2.0 ml/min (constant flow mode); injection mode. split flow Sample (split ratio 5. 1); heating program. initial column temperature was maintained at 60 ° C for 2 min, and the temperature was increased to 10 ° C/min at 10 ° C/min for 2 min, The temperature was increased from 15 ° C/min to.200 ° C for 4 minutes; detector temperature. 280 ° C; flow of makeup gas (6.15). 30 ml/min. 9.2 Establishment of working curve Add 2 g (accurate to 0.01 g) quartz sand (6.14), 3 g (accurate to 0.1 g) chlorine to 7 headspace bottles in this order. Sodium chloride (6.3), 7.0 ml of stannous chloride-sulfuric acid solution (6.10), and 1.0 ml of standard use solution (6.13) with different concentrations, Immediately seal and prepare mancozeb containing 0.20 μg, 0.60 μg, 1.00 μg, 2.00 μg, 6.00 μg, 10.0 μg and 20.0 μg standard series. Place the prepared standard series samples on an 80 ° C thermostatic water bath shaker (7.4) at 120 times/min. After 90 minutes of frequency oscillation, according to the instrument's reference conditions (9.1), sample injection and analysis were performed from low concentration to high concentration, and the peak surface was recorded Product or peak height. Take the content of mancozeb in the standard series solution (μg) as the abscissa, and its corresponding peak area or peak height as Vertical coordinate, establish working curve. 9.3 Standard sample chromatogram Under the recommended instrument reference conditions (9.1) of this standard, the reference chromatogram of manganese zinc acidolysis to form carbon disulfide is shown in figure 1. Figure 1 Standard chromatogram of manganese zinc acidolysis to form carbon disulfide 9.4 Sample determination Place the prepared acidolysis sample (8.3.1) and the non-acidification sample (8.3.2) on the automatic headspace sampler (7.3). The measurement of the sample is carried out according to the same instrument conditions as the working curve (9.2). 9.5 Blank test Follow the same procedure as for sample measurement (9.4) to measure the blank sample (8.4). 10 Calculation and representation of results 10.1 Qualitative analysis Characterized by the retention time of the reaction of mancozeb to form carbon disulfide. Before sample analysis, a retention time window t ± 3s should be established. t is the average retention time of the target compound at each concentration level during the initial calibration, and s is the target at each concentration level during the initial calibration Standard deviation of compound retention time. When analyzing a sample, the target compound should peak within the retention time window. 10.2 Calculation of results The total amount of dithiocarbamate (salt) pesticides in soil is calculated according to formula (1). dmwm mm  011 (1) In the formula. 1w-total amount of dithiocarbamate (salt) pesticides in soil (calculated as mancozeb), mg/kg; 1m-the mass of mancozeb in the acid hydrolysis sample obtained from the working curve, μg; 0m-mass of carbon disulfide converted to mancozeb in the unacidified sample obtained from the working curve, μg; m-sample volume (wet weight), g; dmw-dry matter content in soil sample,%. The total amount of dithiocarbamate (salt) pesticides in the sediment is calculated according to formula (2). )1( OHw'm mm   (2) In the formula. 2w-total dithiocarbamate (salt) pesticides in sediment (calculated as mancozeb), mg/kg 2m-mass of mancozeb in the acid hydrolysis sample obtained from the working curve, μg; 3m-Mass of carbon disulfide converted to mancozeb in the unacidified sample obtained from the working curve, μg; 'm-sample volume (wet weight), g; OHw 2-moisture content of sediment sample,%. The total amount of dithiocarbamate (salt) pesticides in soil or sediment is counted by carbon disulfide and calculated according to formula (3) Count. wwcs  574.0 (3) In the formula. csw-total dithiocarbamate (salt) pesticides in soil or sediment (calculated as carbon disulfide), mg/kg; 0.574--Coefficient converted to manganese zinc into carbon disulfide; w-total amount of dithiocarbamate (salt) pesticides in soil (1w) or sediment (2w) Manganese zinc meter), mg/kg. 10.3 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 three significant digits are retained. 11 Precision and accuracy 11.1 Precision Six laboratories added blank stones with manganese zinc content of 0.30 mg/kg, 1.00 mg/kg, and 9.00 mg/kg, respectively. British sand spiked samples were measured in 6 replicates. Relative standard deviations in the laboratory were 1.4% to 4.1%, 1.1% to 3.8% And 0.9% to 2.6%; the relative standard deviations between laboratories were 6.8%, 9.9%, and 8.2%; the repeatability limits were 0.02 mg/kg, 0.08 mg/kg, and 0.48 mg/kg; the reproducibility limits are 0.06 mg/kg, 0.28 mg/kg, and 2.0 mg/kg, respectively. Six laboratories added sandy soils with manganese zinc content of 0.30 mg/kg, 1.00 mg/kg, 9.00 mg/kg Soil, loam soil and clay soil samples were measured in 6 replicates. Relative standard deviations in the laboratory are 1.6% to 8.6%, 1.8% to 4.8%, and 1.1% to 5.1%; the relative standard deviations between laboratories were 9.0%, 9.6%, and 5.6%, respectively; Repeatability limits are 0.04 mg/kg, 0.08 mg/kg, and 0.80 mg/kg, respectively; reproducibility limits are 0.08 mg/kg, 0.27 mg/kg and 1.6 mg/kg. Six laboratories spike lake-type sediments and rivers with manganese zinc content of 1.00 mg/kg and 9.00 mg/kg, respectively. Flow pattern sediment samples were measured in 6 replicates. Relative standard deviations in the laboratory were 1.8% ～ 4.0% and 1.3% ～ 5.8%; relative standard deviations between laboratories were 11% and 6.8%; repeatability limits were 0.07 mg/kg and 1.1 mg/kg, respectively; Reproducibility limits were 0.32 mg/kg and 1.9 mg/kg, respectively. Refer to Appendix A for summary data of the method precision using the mancozeb and carbon disulfide meters. 11.2 Accuracy Six laboratories for sand-type manganese zinc supplemented with sand content of 0.30 mg/kg, 1.00 mg/kg and 9.00 mg/kg Soil, loam-type soil, clay-type soil samples and mancozeb were spiked at 1.00 mg/kg Soil samples were tested in 6 replicates. The spiked recovery ranges are. 87% ~ 113%, 82% ~ 107%, 91% ~ 106% And 87% ~ 107%, the final recoveries are. 101% ± 18%, 96% ± 18%, 101% ± 12%, and 100% ± 15%. Six laboratories spike lake-type sediments and rivers with manganese zinc content of 1.00 mg/kg and 9.00 mg/kg, respectively. Flow pattern sediment samples were measured in 6 replicates. Spike recovery rates range from 81% to 110% and 85% to 103%, respectively. Final recovery rate. 99% ± 22%, 94% ± 12%. See Appendix A for a summary of the accuracy of the mancozeb and carbon disulfide meters. 12 Quality Assurance and Quality Control 12.1 Blank test Analyze at least one laboratory blank every 20 samples or batches (less than 20 samples/batch). Laboratory blank test The results should be below the method detection limit. 12.2 Calibration The correlation coefficient of the working curve is ≥ 0.995, otherwise the working curve is re-established. Every 20 samples or batch (less (20 samples/batch) to perform a calibration of the middle concentration point of the working curve, the relative error of the measured value of the calibration point should be ± 15% Within. 12.3 Parallel samples Every 20 samples or each batch (less than 20 samples/batch) should analyze at least one parallel sample, the results of parallel sample analysis The relative deviation should be ≤30%. 12.4 Matrix Spiking Every 20 samples or each batch (less than 20 samples/batch) should analyze at least one matrix plus standard sample, and matrix plus standard back The yield should be between 70% and 130%. 13 Waste treatment The used reference materials and waste acids should be collected centrally and entrusted to a qualified unit for disposal.

Appendix A

(Informative appendix) Method precision and accuracy Table A.1 Summary of method precision Compound matrix type Spiked concentration (Mg/kg) average value (Mg/kg) Laboratory phase Standard deviation (%) Interphase Standard deviation (%) Repeatability limit r (mg/kg) Reproducibility limit R (Mg/kg) Dithio Carbamate Acid ester (Salt) category Pesticides Mancozeb Zinc meter) Blank quartz sand 0.30 0.30 1.4 ~ 4.1 6.8 0.02 0.06 1.00 0.98 1.1 ~ 3.8 9.9 0.08 0.28 9.00 8.54 0.9 ~ 2.6 8.2 0.48 2.0 Sandy soil 0.30 0.30 1.6 ~ 8.6 9.0 0.04 0.08 Loam soil 1.00 0.96 1.8 ~ 4.8 9.6 0.08 0.27 Clay soil 9.00 9.11 1.1 ~ 5.1 5.6 0.80 1.6 Lake reservoir sediment 1.00 0.99 1.8 ~ 4.0 11 0.07 0.32 River sediment 9.00 8.45 1.3 ~ 5.8 6.8 1.1 1.9 ......
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