Search result: HJ 698-2014
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Water quality. Determination of chlorothalonil and deltamethrin. Gas chromatography method
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HJ 698-2014
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| Standard ID | HJ 698-2014 (HJ698-2014) | | Description (Translated English) | Water quality. Determination of chlorothalonil and deltamethrin. Gas chromatography method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 10,117 | | Date of Issue | 3/31/2014 | | Date of Implementation | 7/1/2014 | | Quoted Standard | HJ/T 91; HJ/T 164 | | Issuing agency(ies) | Ministry of Environmental Protection | | Summary | This Standard specifies the gas chromatographic determination of cyanide in water chlorothalonil and Australia chrysanthemum cool. This Standard applies to surface water, groundwater, industrial wastewater and domestic sewage in the determination of chlor |
HJ 698-2014
Water quality.Determination of chlorothalonil and deltamethrin.Gas chromatography method
National Environmental Protection Standard of the People's Republic
HJ 698-.2014
Determination of chlorothalonil and deltamethrin
Gas chromatography
Water quality-Determination of chlorothalonil and deltamethrin
- Gas chromatography method
2 0 1 4 - 0 3 - 3 1 released
2 0 1 4 - 0 7 - 0 1 implementation
Ministry of Environmental Protection released
Content
Preface II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 Interference and elimination 1
5 reagents and materials 1
6 Instruments and equipment 2
7 sample 2
8 Analysis steps. 2
9 Calculation and representation of results. 3
10 precision and accuracy. 4
11 Quality Assurance and Quality Control 5
12 Waste treatment.5
Foreword
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 protect the environment,
This standard is formulated to ensure human health and to regulate the determination method of chlorothalonil and deltamethrin in water.
This standard specifies gas chromatography for the determination of chlorothalonil and deltamethrin in water.
This standard is the first release.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Taizhou Environmental Monitoring Center Station.
This standard method verification unit. Jiangsu Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Suzhou Environmental Monitoring
Central Station, Wuxi Environmental Monitoring Center Station, Changzhou Environmental Monitoring Center and Taizhou Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on March 31,.2014.
This standard has been implemented since July 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of chlorothalonil and deltamethrin - Gas chromatography
Warning. The reagents and standard solutions used in this method are volatile toxic compounds. The preparation process should be in the fume hood.
Carry out; protective equipment should be worn as required to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the gas chromatographic method for the determination of chlorothalonil and deltamethrin in water.
This standard applies to the determination of chlorothalonil and deltamethrin in surface water, groundwater, industrial wastewater and domestic sewage.
When the sample amount is 100ml, the detection limit of this standard method is. chlorothalonil is 0.07μg/L, and deltamethrin is 0.40μg/L;
Lower limit of determination. chlorothalonil was 0.28 μg/L, and deltamethrin was 1.60 μg/L.
2 Normative references
The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this
standard.
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 chlorothalonil and deltamethrin in the sample were extracted with n-hexane, and the extract was dehydrated, concentrated, and made up to volume with anhydrous sodium sulfate.
Phase Chromatograph - Electron Capture Detector (ECD) separation, detection, qualitative according to retention time, external standard method for quantification.
4 interference and elimination
Due to its high sensitivity, the electron capture detector is prone to interference due to a large number of impurity peaks. When the target compound is detected,
Apply column 2 to aid in qualitative confirmation to eliminate interference.
5 reagents and materials
Unless otherwise stated, analytically pure reagents and distilled water in accordance with national standards were used for the analysis.
5.1 n-hexane. pesticide residue level.
5.2 chlorothalonil standard solution. ρ = 100mg/L, the solvent is petroleum ether.
5.3 Deltamethrin standard solution. ρ = 100mg/L, the solvent is petroleum ether.
5.4 Concentrated sulfuric acid (H2SO4)
5.5 anhydrous sodium sulfate (Na2SO4)
After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.
5.6 sodium chloride (NaCl)
After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.
5.7 Sodium sulfate solution. c (Na2SO4) = 1.0 mol/L.
Weigh 142 g of sodium sulfate (5.5) in a small amount of water and dilute to 1000 ml.
5.8 Nitrogen. purity ≥ 99.999%.
6 Instruments and equipment
6.1 Gas Chromatograph. With an electron capture detector.
6.2 Column 1. Quartz capillary column, 30m × 0.25mm, coated with 5% phenylmethylpolysiloxane, film thickness 0.25μm.
Or other equivalent capillary column.
6.3 Column 2. Quartz capillary column, 30m × 0.25mm, coated with 35% phenylmethylpolysiloxane, film thickness 0.25μm.
Or other equivalent capillary column.
6.4 Concentration device. Rotary evaporation device or equivalent equipment such as KD concentrator and concentrator.
6.5 Oscillator.
6.6 Separating funnel. 100 ml, 250 ml.
6.7 Microinjector. 10 μl, 50 μl, 100 μl.
6.8 Drying column. glass column with a length of 250mm and an inner diameter of 20mm, and the glass piston is not coated with lubricating oil. At the lower end of the column, put
A small amount of glass wool or glass fiber filter paper was added to 10 g of anhydrous sodium sulfate (5.5). Or use other types of drying equipment.
6.9 Box type electric furnace.
6.10 Common instruments and equipment used in general laboratories.
7 samples
7.1 Acquisition and preservation
Samples were taken with reference to the relevant regulations of HJ/T 91 and HJ/T 164.
Samples were collected using a 500 ml hard ground glass bottle or a brown threaded glass bottle with a Teflon septum.
The sample is stored at 2 ° C ~ 5 ° C, the extraction is completed within 7 days, the extract can be stored for 40 days.
7.2 Preparation of samples
7.2.1 Measure 100.0ml sample into a 250ml separatory funnel, add 10g sodium chloride (5.6), dissolve, add 10ml
Hexane (5.1), shaken and vented, placed on a shaker and shaken vigorously for 5 min, allowed to stand for 10 min, layered, and extracted with n-hexane.
The solution was transferred to a 100 ml separatory funnel.
7.2.2 Repeat the extraction once and combine the n-hexane extract.
Note 1. For samples with complex composition, if the emulsification phenomenon is serious during the extraction process, mechanical separation should be used to complete the two-phase separation.
It can be broken by agitation, centrifugation, filtration with glass wool, etc., or it can be broken by freezing.
7.2.3 Purification. Add 5 ml of concentrated sulfuric acid to the extract, vortex the mixture, let stand for 1 minute, and discard the sulfuric acid layer. repeatedly
Wash to sulfuric acid layer is colorless, discard the sulfuric acid layer; wash n-hexane with appropriate amount of sodium sulfate solution (5.7), repeat washing to the water phase
Neutral, discard the water phase.
Note 2. For cleaner groundwater and surface water samples, the purification step can be omitted.
7.2.4 Dehydrate the n-hexane extract through a drying column (or other type of drying equipment) and wash it with a small amount of n-hexane.
The separatory funnel was 2-3 times, and the washing liquid was dehydrated through a drying column, and all the dehydrated n-hexane was collected and concentrated to a concentration until
5.0ml, to be tested.
7.3 Preparation of blank samples
A sample of 100.0 ml of distilled water was used instead of the sample, and a blank sample was prepared in accordance with the same procedure as in the preparation of the sample (7.2).
8 Analysis steps
8.1 Recommended chromatographic conditions
Inlet temperature. 250 ° C, column flow rate. 1.0 ml/min;
Oven. 30/min 30/min 50 min min 290 min⎯⎯⎯→ ⎯⎯⎯→°C °C°C(1).200°C(8) °C(10);
Split injection, split ratio 5.1; injection volume. 1.0 μl.
Detector temperature. 320 °C.
8.2 Drawing a calibration curve
Take 6 10ml volumetric flasks, add appropriate amount of n-hexane (5.1), add 0.0μl, 1.0μl, 2.0μl, 5.0μl, respectively.
10.0 μl, 20.0 μl chlorothalonil standard solution (5.2) and 0.0 μl, 5.0 μl, 10.0 μl, 25.0 μl, 50.0 μl, 100.0 μl cyanide
The standard solution of pyrethroid (5.3) was fixed to volume with n-hexane (5.1), and the concentration of chlorothalonil was 0.0 mg/L.
0.010mg/L, 0.020mg/L, 0.050mg/L, 0.100mg/L, 0.200mg/L, the mass concentration of deltamethrin is
0.0 mg/L, 0.050 mg/L, 0.10 mg/L, 0.25 mg/L, 0.50 mg/L, 1.00 mg/L standard series. Standard solution
The series concentration (mg/L) is the abscissa, and the corresponding peak response value (peak area or peak height) is plotted on the ordinate.
curve.
8.3 Determination of samples
Use a micro-syringe to take 1.0 μl of the sample to be tested (7.2) into the gas chromatograph, in the same chromatographic strip as the calibration curve.
Determine the retention time and peak area (or peak height) of the chromatographic peak.
8.4 Blank test
While the sample is being analyzed, a blank test should be performed. Take 1.0μl blank sample (7.3) into the gas chromatograph, press
8.3 Determine the same steps for analysis.
9 Calculation and representation of results
9.1 Qualitative analysis
Take a certain amount of chlorothalonil and deltamethrin standard solution, diluted to 20.0μg/L and 100.0μg/L with n-hexane (5.1),
Take 1.0 μl of the injection and separate it with column 1 to characterize the retention time of the peaks of chlorothalonil and deltamethrin. Chlorothalonil,
The standard chromatogram of deltamethrin is shown in Figure 1.
Figure 1 Standard chromatogram of chlorothalonil and deltamethrin (column 1)
If the target compound is detected, use column 2 to aid in qualitative confirmation, see Figure 2.
Figure 2 Assisted qualitative chromatogram of chlorothalonil and deltamethrin (column 2)
9.2 Quantitative analysis
The concentration (μg/L) of chlorothalonil and deltamethrin in the sample was calculated according to formula (1).
10V
Ρρ = × × (1)
In the formula.
Ρ-- chlorothalonil, deltamethrin mass concentration, μg/L;
1-1-- Calculate the concentration of chlorothalonil and deltamethrin in the sample to be tested according to the calibration curve, mg/L;
V 1--water sample volume, ml;
V2--sample volume, ml.
9.3 Result representation
When the measurement result is less than 1.00 μg/L, it is retained to two decimal places; when the measurement result is greater than or equal to 1.00 μg/L,
Keep three significant digits.
10 Precision and accuracy
10.1 Precision
Six laboratories were tested for uniform samples with chlorothalonil concentrations of 0.500 μg/L, 2.00 μg/L, and 10.0 μg/L, respectively.
The relative standard deviations in the experimental room were. 6.1%~9.0%, 1.2%~7.4%, 1.5%~5.3%;
The deviations were. 5.4%, 4.7%, 2.9%; the repeatability limits were. 0.11μg/L, 0.27μg/L, 1.1μg/L; reproducibility
The limits are. 0.12 μg/L, 0.35 μg/L, and 1.3 μg/L.
Uniform samples of deltamethrin concentrations of 2.50 μg/L, 10.0 μg/L, and 50.0 μg/L were tested in 6 laboratories.
The relative standard deviations in the laboratory are. 4.5%~7.8%, 2.6%~6.7%, 3.1%~4.7%;
The standard deviations were. 4.4%, 4.2%, 2.4%; the repeatability limits were. 0.37 μg/L, 1.4 μg/L, 5.6 μg/L; reproducibility
The limits are. 0.43 μg/L, 1.8 μg/L, and 6.1 μg/L.
10.2 Accuracy
Six laboratories conducted calibration standards containing chlorothalonil concentrations of 0.500 μg/L, 2.00 μg/L, and 10.0 μg/L.
For the measurement, the relative errors are. -6.2%~0.0%, -5.1%~3.9%, -3.0%~3.0%. Relative error final value
It is. -2.7% ± 5.0%, 1.6% ± 7.2%, 0.3% ± 5.2%.
Six laboratories carried out chlorpyrifos addition to the surface water, domestic sewage and industrial wastewater samples, and added the scalar amount.
Do not. 0.050μg, 0.200μg, 1.00μg, the standard addition recovery rate is. the standard recovery is 82.0%~92.0%,
89.0%~95.5%, 89.0%~97.3%, and the final recoveries were 88.0%±8.4%, 92.8%±4.5%, and 93.4%±6.1%.
Six laboratories conducted certified standards for deltamethrin concentrations of 2.50 μg/L, 10.0 μg/L, and 50.0 μg/L, respectively.
For the measurement, the relative errors are. -4.6%~7.2%, -4.8%~3.9%, -4.9%~1.4%, and the relative errors are the final values.
0.2% ± 11%, -1.4% ± 6.8%, -1.9% ± 5.1%.
Six laboratories tested the deltamethrin spikes on surface water, domestic sewage and industrial wastewater samples, and added scalar quantities.
They were. 0.250μg, 1.00μg, 5.00μg, and the recoveries were 92.5%~111%, 90.3%~97.4%, respectively.
93.8%~101%, the final recoveries of the spiked recovery were 101%±17.5%, 94.3%±6.0%, and 97.0%±5.4%, respectively.
11 Quality Assurance and Quality Control
11.1 At least one laboratory blank should be made for each batch of samples. The blank value should be lower than the method detection limit. Otherwise, the cause should be ascertained.
11.2 The correlation coefficient of the calibration curve should be ≥0.995, otherwise the calibration curve should be redrawn.
11.3 Continuous calibration. For every 20 samples measured, a standard solution of the concentration of the middle point of the calibration curve shall be determined.
The relative error of the concentration of the calibration curve at this point should be ≤ 20%. Otherwise, the calibration curve needs to be redrawn.
11.4 At least 10% of parallel samples should be measured for each batch of samples. When the number of samples is less than 10, at least one parallel double should be determined.
kind. When the measurement result is within 10 times the detection limit (including the detection limit of 10 times), the relative deviation of the results of the parallel double sample determination should be
≤50%; When the measurement result is greater than 10 times the detection limit, the relative deviation of the parallel double sample measurement results should be ≤ 20%.
11.5 At least one spiked sample shall be determined for each batch of samples. The recovery rate of the spiked sample shall be between 70% and 130%.
12 Waste treatment
The organic waste generated by the experiment should be stored in a centralized manner and entrusted to a qualified unit for processing.
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