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HJ 1072-2019: Water quality--Determination of pyridine--Headspace / gas chromatography
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Water quality--Determination of pyridine--Headspace / gas chromatography
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HJ 1072-2019
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Basic data | Standard ID | HJ 1072-2019 (HJ1072-2019) | | Description (Translated English) | Water quality--Determination of pyridine--Headspace / gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 10,113 | | Date of Issue | 2019 | | Date of Implementation | 2020-06-30 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1072-2019: Water quality--Determination of pyridine--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.
Water quality--Determination of pyridine--Headspace/gas chromatography
National Environmental Protection Standard of the People's Republic of China
Water quality--Determination of pyridine--Headspace/gas chromatography
Water quality-Determination of pyridine
-Headspace/gas 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 Reagents and materials ... 1
5 Instruments and equipment ... 2
6 Sample ... 2
7 Analysis steps ... 3
8 Calculation and Representation of Results ... 3
9 Precision and accuracy ... 4
10 Quality Assurance and Quality Control ... 5
11 Waste disposal ... 5
12 Notes ... 5
Appendix A (informative) Instrument reference conditions for auxiliary qualitative columns ... 6
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 pyridine in water, and formulate this standard.
This standard specifies headspace/gas chromatography for the determination of pyridine in surface water, groundwater, domestic sewage and industrial wastewater.
Compared with "Gas Chromatography for the Determination of Water Quality Pyridine" (GB/T 14672-1993), the main differences between this standard are as follows.
-The name was changed to "headspace/gas chromatography for the determination of pyridine in water";
-Added normative references;
-Added description of method principle;
-The chromatographic column was changed from a packed column to a capillary column, and the manual headspace sample was changed to a fully automatic headspace sampler;
-Quantitative by standard curve external standard method;
-Added quality control and quality assurance;
-Added waste disposal and precautions.
Since the date of implementation of this standard, the "Pyridine of Water Quality" approved and issued by the former State Environmental Protection Administration on September 18,.1993
Determination of Gas Chromatography (GB/T 14672-1993) in the corresponding environmental quality standards and pollutant emission (control) standards
Execution will stop during the implementation.
Appendix A of this standard is an informative appendix.
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. China Shipbuilding Industry Corporation 718 Research Institute.
This standard is verified by. Hebei Province Environmental Monitoring Center Station, Shijiazhuang City Environmental Monitoring Station, Anyang City Environmental Monitoring Station,
Baoding Environmental Monitoring Station, China Shipbuilding Chemicals Testing Center and Beijing Huaxue North Testing Technology Co., Ltd.
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 pyridine--Headspace/gas chromatography
Warning. The solvents and standard samples used in the experiment are toxic and harmful compounds. Their reagent preparation and sample preparation process
It should be carried out in a fume hood, and protective equipment should be worn during operation to avoid contact with skin and clothing.
1 Scope
This standard specifies headspace/gas chromatography for the determination of pyridine in water.
This standard applies to the determination of pyridine in surface water, groundwater, domestic sewage and industrial wastewater.
When the sampling volume is 10.0 ml, the detection limit of the method is 0.03 mg/L, and the lower limit of determination is 0.12 mg/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
Place the sample in a sealed headspace bottle. Under certain conditions, the pyridine in the sample in the headspace bottle volatilizes to the headspace.
Vapor pressure is generated and thermodynamic equilibrium is reached in the gas-liquid two-phase. Take a part of the gas sample and separate it by gas chromatography, hydrogen flame
Detection by ionization detector. Qualitative according to retention time, quantified by standard curve external standard method.
4 Reagents and materials
Unless otherwise stated, analytical reagents that comply with national standards are used in the analysis. The experimental water is double distilled water or pure
Water prepared by water equipment must be blank checked before use to confirm that it does not contain the target compound and its retention time is within the target compound.
No interfering chromatographic peaks appeared in the interval.
4.1 Sulfuric acid (H2SO4). ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
4.2 Sodium hydroxide (NaOH).
4.3 Sodium chloride (NaCl). excellent grade pure.
Burn at 500 ° C to 550 ° C for 2 h, cool to room temperature, and store in a desiccator for later use.
4.4 Sodium thiosulfate (Na2S2O3).
4.5 Methanol (CH3OH). chromatographically pure.
4.6 Pyridine (C5H5N). purity ≥99.5%.
4.7 Sulfuric acid solution. 1 1.
4.8 Sodium hydroxide solution. c (NaOH) = 10 mol/L.
4.9 Standard stock solution. ρ≈1000 mg/L.
Add a suitable amount of methanol (4.5) to a 100 ml volumetric flask, and then weigh 100 mg (accurate to 0.1 mg) of pyridine (4.6)
Add to volumetric flask, make up to volume with methanol (4.5), and mix. Refrigerate below 4 ° C, sealed and protected from light, can be stored
3 months, return to room temperature before use. Or purchase a certified standard solution directly.
4.10 Standard use solution. ρ = 10.0 mg/L.
Dilute the standard stock solution (4.9) with water and prepare immediately before use.
4.11 Carrier gas. High-purity nitrogen with a purity of ≥99.999%.
4.12 Combustion gas. high-purity hydrogen, with a purity of ≥99.999%.
4.13 Gas-assisting gas. air, dehydrated by silica gel, and activated carbon to remove organic matter.
5 Instruments and equipment
5.1 Sampling bottle. a 40 ml brown screw-top glass bottle with a silicone rubber-teflon liner screw cap.
5.2 Gas chromatograph. with split/splitless inlet and hydrogen flame ionization detector (FID), chromatographic data processing tool
Work stop.
5.3 Column I. Specifications are 30 m (column length) × 0.32 mm (inner diameter) × 0.5 μm (film thickness), 100% polyethylene glycol
Stationary capillary columns, or other equivalent capillary columns.
5.4 Column II. 30 m (column length) × 0.25 mm (inner diameter) × 1.4 μm (film thickness), 6% nitrile propionyl
94% dimethylpolysiloxane stationary phase capillary column, or other equivalent capillary column.
5.5 Automatic headspace sampler. The temperature control accuracy is ± 1 ° C.
5.6 Headspace bottle. Headspace bottle (22 ml), polytetrafluoroethylene (PTFE)/silicone gasket, cap (screw cap or
Glands), or glass headspace vials that are compatible with automatic headspace samplers.
5.7 Pipette. 1 ml to 10 ml.
5.8 Analytical balance. 0.1 mg accuracy.
5.9 General laboratory instruments and equipment.
6 samples
6.1 Sample collection
Collect the samples in accordance with the relevant regulations of HJ 91.1, HJ/T 91 and HJ/T 164.
Before sampling, determine the pH value of the sample. According to the pH measurement result, use a sulfuric acid solution (4.7) or sodium hydroxide solution.
(4.8) Adjust the pH to 6-8. When collecting samples, allow the sample to overflow in the vial without leaving space on the liquid. When sampling
Minimize or reduce exposure of the sample to air. All samples were taken in duplicate. If there is residual chlorine in the sample,
Add 1000 mg of sodium thiosulfate (4.4) to a 1000 ml sample.
Follow the same steps as for sample collection, place a portion of experimental water in a sample bottle in the laboratory, seal it, and bring it
At the sampling site, return the sample to the laboratory and save it at the same time.
6.2 Sample preservation
Analyze samples as soon as they are returned to the laboratory. If it can't be analyzed in time, it should be refrigerated below 4 ℃, sealed and protected from light.
The analysis was completed within 3 days. The sample storage area should be free of volatile organic compounds, and the sample should be returned to room temperature before the sample is measured.
6.3 Preparation of test specimens
Add 3 g of sodium chloride (4.3) to the headspace bottle (5.6), add 10.0 ml of sample, immediately cap and seal, shake
Uniform, to be tested.
6.4 Preparation of laboratory blank samples
Use experimental water to replace the sample, and follow the same steps as in sample preparation (6.3) to prepare a laboratory blank sample.
6.5 Preparation of full procedure blank sample
Follow the same procedure for sample preparation (6.3) to prepare a blank sample for the entire procedure.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Headspace Sampler Reference Conditions
Heating equilibrium temperature. 70 ℃; Heating equilibration time. 30 min; Sample valve temperature. 100 ℃; Transmission line temperature. 110 ℃;
Injection volume. 1.0 ml; pressure equilibration time. 1 min; injection time. 0.2 min.
7.1.2 Gas chromatograph reference conditions
Inlet temperature..200 ° C; Detector temperature. 230 ° C; Column temperature. 70 ° C; Column flow rate. 3.0 ml/min;
Combustion gas (4.12) flow rate. 40 ml/min; assisted gas (4.13) flow rate. 350 ml/min; makeup gas flow rate. 30 ml/min;
The split ratio is 10. 1.
7.2 Drawing of standard curve
Add 3 g of sodium chloride (4.3) to each of the 5 headspace bottles, and add 9.80 ml, 9.50 ml, 9.00 ml,
8.00 ml and 5.00 ml water, then 0.20 ml, 0.50 ml, 1.00 ml, 2.00 ml, and 5.00 ml pyridine
Quasi-use solution (4.10), formulated into a pyridine mass concentration of 0.20 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L
And the standard series of 5.00 mg/L, immediately cap and seal, and mix well. According to the instrument reference conditions (7.1), from low concentration to high concentration
Sampling analysis was performed sequentially, and the retention time and response value of pyridine were recorded. Pyridine concentration as the abscissa and its corresponding response value
Create a standard curve for the ordinate.
7.3 Determination of sample
The measurement of the sample (6.3) was performed under the same conditions as the standard curve. If the concentration of pyridine in the sample exceeds the standard curve
The range should be determined after dilution.
7.4 Determination of laboratory blank samples
The measurement of the laboratory blank sample (6.4) is performed in the same procedure as the sample measurement (7.3).
8 Results calculation and representation
8.1 Qualitative analysis
Qualitative based on the retention time of the target in the sample and the target in the standard series. Before sample analysis, when establishing retention
The window t ± 3S. t is the average retention time of pyridine at each concentration level during initial calibration, and S is pyridine at each concentration level during initial calibration
Standard deviation of pyridine retention time. During sample analysis, the target should peak within the retention time window.
When it is detected on column I (5.3) but cannot be confirmed, column II (5.4) can be used for auxiliary characterization. color
Refer to Appendix A for the reference conditions for the determination of column II and the standard chromatogram of pyridine in water.
Under the measurement conditions specified in this standard, the standard reference chromatogram of pyridine in water is shown in Figure 1.
1-methanol; 2-pyridine
Figure 1 Standard chromatogram of pyridine (5.00 mg/L)
8.2 Calculation of results
The mass concentration of pyridine in the sample is calculated according to formula (1).
(1)
Where. -mass concentration of pyridine in the sample, mg/L;
i-the mass concentration of pyridine in the sample obtained from the standard curve, mg/L;
D-- sample dilution.
8.3 Representation of results
The number of digits after the decimal point of the measurement result is the same as the detection limit of the method. A maximum of 3 significant digits are retained.
9 Precision and accuracy
9.1 Precision
Six laboratories performed 6 replicates of blank spiked samples at concentrations of 0.20 mg/L, 1.00 mg/L and 4.50 mg/L
Determination. The relative standard deviations in the laboratory were 4.2% to 8.1%, 2.0% to 9.2%, and 2.6% to 6.7%, respectively.
The standard deviations are 4.5%, 2.6%, and 2.8%, respectively; the repeatability limits are 0.04 mg/L, 0.17 mg/L, and 0.61 mg/L, respectively;
Reproducibility limits were 0.04 mg/L, 0.17 mg/L, and 0.66 mg/L.
The six laboratories separately tested two different spiked concentrations of 0.60 mg/L (surface water) and 2.00 mg/L (industrial wastewater).
Six repeated determinations of the same type of samples. the relative standard deviations in the laboratory were 1.9% to 11% and 2.1% to 6.5%;
Interlaboratory relative standard deviations were 4.6% and 2.8%, respectively; repeatability limits were 0.10 mg/L and 0.24 mg/L, respectively; reproducibility
The limits were 0.12 mg/L and 0.27 mg/L, respectively.
9.2 Accuracy
The six laboratories separately tested the two different concentrations of 0.60 mg/L (surface water) and 2.00 mg/L (industrial wastewater).
Six determinations of the same type of sample were performed. the spiked recoveries ranged from 92.8% to 105% and 95.1% to 102%, respectively;
The final recoveries were 97.0% ± 8.8% and 98.0% ± 5.8%, respectively.
Di
10 Quality Assurance and Quality Control
10.1 Laboratory blank
Every 20 samples or each batch of samples (less than 20/batch) should be made at least 1 laboratory blank, the blank test results should be low
Due to method detection limit.
10.2 Full Program Blank
Every 20 samples or each batch of samples (less than 20/batch) should be made at least 1 full program blank, the full program blank determination results
Results should be below the method detection limit.
10.3 Calibration
The standard curve contains at least 5 non-zero concentration points, and the correlation coefficient is ≥0.995. Every 20 samples or batches (less
20), the middle concentration point of a standard curve should be measured, and the relative error between the measurement result and the standard concentration value should be within ± 15%
between. Otherwise, find the cause and redraw the standard curve.
10.4 Parallel samples
Analyze at least 1 parallel sample for every 20 samples or batches (less than 20 samples/batch), single parallel sample measurement results
The relative deviation is ≤20%.
10.5 Matrix Spiking
Analyze at least one matrix spiked sample for every 20 samples or batches (less than 20/batch), matrix spiked recovery
It should be between 80% and 110%.
11 Waste treatment
Wastes generated during the experiment should be sorted and disposed of accordingly, and properly identified, and entrusted to a qualified unit for treatment.
12 Notes
12.1 During sample collection, sample storage and pretreatment, avoid contact with plastics and other organics.
12.2 When measuring samples with high salt content, the amount of sodium chloride (4.3) can be reduced to avoid salt precipitation in the sample
This causes a change in the gas-liquid two-phase volume in the headspace vial. The amount of sodium chloride (4.3) added to the sample and the standard solution should be the same
To.
12.3 When analyzing complex samples, in order to ensure that the high boiling point components of the previous sample do not affect the determination of the analyzed sample, the
After each sample, the high-boiling components in the sample are blown out by rapid heating, and then the next sample is analyzed.
Appendix A
(Informative appendix)
Instrument reference conditions for auxiliary qualitative columns
A.1 Reference conditions for auxiliary qualitative gas chromatography
Inlet temperature..200 ℃;
Detector temperature. 230 ℃;
Column temperature. 90 ℃;
Carrier gas. nitrogen;
Column flow rate. 3.0 ml/min;
Hydrogen flow rate. 40 ml/min;
Air flow rate. 350 ml/min;
Makeup gas flow rate. 30 ml/min;
The split ratio is 10. 1.
A.2 Standard chromatogram of auxiliary qualitative column (column II)
The reference standard chromatogram of pyridine in water on an auxiliary qualitative chromatographic column (column II) is shown in Figure A.1.
1-methanol; 2-pyridine
Figure A.1 Chromatogram of a pyridine standard sample (Column II)
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