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HJ 1017-2019: Water quality - Determination of benzidine - High performance liquid chromatography
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Water quality - Determination of benzidine - High performance liquid chromatography
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HJ 1017-2019
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Basic data | Standard ID | HJ 1017-2019 (HJ1017-2019) | | Description (Translated English) | Water quality - Determination of benzidine - High performance liquid chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 10,114 | | Date of Issue | 2019 | | Date of Implementation | 2019-09-01 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1017-2019: Water quality - Determination of benzidine - High performance liquid chromatography
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Water quality - Determination of benzidine - High performance liquid chromatography
National Environmental Protection Standard of the People's Republic
Determination of water quality benzidine
High performance liquid chromatography
Water quality-Determination of benzidine
-High performance liquid chromatography
2019-04-13 released.2019-09-01 implementation
Department of Ecology and Environment
Content
Foreword...ii
1 Scope...1
2 Normative references...1
3 Principles of the method...1
4 Reagents and materials...1
5 Instruments and Equipment...2
6 samples...3
7 Analysis steps...4
8 Calculation and representation of results...4
9 Precision and Accuracy...5
10 Quality Assurance and Quality Control...6
11 Waste treatment...6
Foreword
Protect the ecology for the implementation of 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
The environment, the protection of human health, the determination of the determination of benzidine in water, the development of this standard.
This standard specifies high performance liquid chromatography for the determination of benzidine in surface water, groundwater, domestic sewage and industrial wastewater.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Qingdao Environmental Monitoring Center Station.
This standard is verified by. Shandong Provincial Environmental Monitoring Center Station, Agricultural and Rural Department, Agricultural Products Quality and Safety Supervision and Testing
Heart (Qingdao), Weihai Environmental Protection Monitoring Station, Liaoning North Environmental Testing Technology Co., Ltd., Qingdao Hua Testing Technology
Co., Ltd. and National Urban Water Supply Monitoring Network Qingdao Monitoring Station.
This standard is approved by the Ministry of Ecology and Environment on April 13,.2019.
This standard has been implemented since September 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
Water quality - Determination of benzidine - High performance liquid chromatography
Warning. The organic solvent used in the experiment has certain toxicity and volatility. The standard substance has strong carcinogenicity and reagents.
Preparation and sample preparation should be carried out in a fume hood, and protective equipment should be worn as required to avoid contact with the skin and
Clothing.
1 Scope of application
This standard specifies high performance liquid chromatography for the determination of benzidine in water.
This standard applies to the determination of benzidine in surface water, groundwater, domestic sewage and industrial wastewater.
When the sampling volume is 150 ml, the sample volume is 2.0 ml, and the injection volume is 40 μl, the method detection limit is
0.006 μg/L, the lower limit of determination is 0.024 μg/L.
2 Normative references
This standard refers to the following documents or their terms. 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 sample is passed through a cation exchange solid phase extraction column, the benzidine is adsorbed, and the benzidine is locked to the solid phase extraction with an acetic acid solution.
On the column, the impurities are removed by washing with methanol, and then eluted with ammonia methanol solution. The eluent is concentrated and concentrated to have fluorescence.
High performance liquid chromatography separation detection of the detector. According to the retention time qualitative, the external standard method is quantitative.
4 reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated.
water.
4.1 Hydrochloric acid. ρ(HCl) = 1.19 g/ml.
4.2 Glacial acetic acid. ρ(CH3COOH) = 1.05 g/ml.
4.3 Ammonia. ρ(NH3·H2O)=0.91 g/ml, excellent grade.
4.4 Sodium hydroxide (NaOH).
4.5 sodium thiosulfate (Na2S2O3).
4.6 Ammonium acetate (CH3COONH4). chromatographically pure.
4.7 benzidine. w ≥ 99.6%.
4.8 Methanol (CH3OH). Pure by liquid chromatography.
4.9 Ethanol (CH3CH2OH).
4.10 Acetonitrile (CH3CN). Pure by liquid chromatography.
4.11 Hydrochloric acid solution. 1 1.
4.12 Aqueous methanol solution. 1 1.
4.13 Ammonium acetate solution. c (CH3COONH4) = 0.01 mol/L.
Weigh 0.77 g of ammonium acetate (4.6), dissolve in water, and dilute to 1 L.
4.14 Acetic acid solution. 3 97.
Measure 3 ml of glacial acetic acid (4.2) and 97 ml of water, mix and set aside.
4.15 sodium hydroxide solution. c (NaOH) = 1 mol/L.
Weigh 4 g of sodium hydroxide (4.4), dissolve in water, and dilute to 100 ml.
4.16 Ammonia solution in methanol. 5 95.
Measure 5 ml of ammonia (4.3) and 95 ml of methanol (4.8), mix and set aside.
4.17 Standard stock solution of benzidine. ρ = 1000 μg/ml.
Weigh 0.050 g (accurate to 0.1 mg) of benzidine (4.7) in a 50 ml brown volumetric flask and dissolve with methanol (4.8)
Dissolve and dilute to volume, transfer to a screw brown reagent bottle lined with Teflon pad. This solution is at 4 ° C
It can be stored for 1 year under cold storage and protected from light. Commercially available certified standard solutions can also be purchased directly.
4.18 benzidine standard intermediate. ρ = 100 μg/ml.
Accurately remove 1.00 ml of benzidine standard stock solution (4.17) in a 10 ml brown volumetric flask and dilute with methanol (4.8)
Release the volume to the marking line. This solution is stored at 4 ° C or less and can be stored for 1 year in the dark.
4.19 Standard solution of benzidine used I. ρ = 10.0 μg/ml.
Accurately transfer 1.00 ml of benzidine standard intermediate (4.18) in a 10 ml brown volumetric flask with aqueous methanol (4.12)
Dilute to volume. This solution is stored at 4 ° C or less and can be stored for 3 months in the dark. Allow to room temperature and mix before use.
4.20 Standard solution of benzidine used II. ρ = 1.00 μg/ml.
Accurately transfer 1.00 ml of benzidine standard solution I (4.19) in a 10 ml brown volumetric flask with methanol
(4.12) Dilute to volume. Available now.
4.21 Solid phase extraction column. mixed cation exchange solid phase extraction column, the filler is benzene sulfonated polystyrene-divinyl
Benzene resin, 150 mg/6 ml, or other equivalent extraction column.
4.22 Filter. 0.45 μm PTFE membrane.
4.23 Nitrogen. purity ≥ 99.99%.
5 instruments and equipment
5.1 High Performance Liquid Chromatograph. with fluorescence detector.
5.2 Column. C18 reversed-phase column with a particle size of 5 μm, a column length of 15 cm and an internal diameter of 4.6 mm, or other equivalent
Column.
5.3 Vials. 500 ml brown thin-mouthed glass bottles with ground plugs or brown threaded glass bottles with Teflon liners.
5.4 Microinjectors. 10 μl, 50 μl and 100 μl.
5.5 Nitrogen blowing instrument.
5.6 Ultrasonic cleaner. The output power is above 180 W and the operating frequency is 40 kHz.
5.7 Solid phase extraction unit.
5.8 Common instruments and equipment used in general laboratories.
6 samples
6.1 Sample collection and preservation
Sample collection was performed in accordance with the relevant regulations of HJ/T 91 and HJ/T 164. Add to the vial (5.3) before sampling
Sodium thiosulfate (4.5) was added and 40 mg was added per 500 ml of sample. When sampling, the sample should be filled with the sample bottle, leaving no liquid
On the space. If the pH of the sample is not between 6 and 9, adjust with hydrochloric acid solution (4.11) or sodium hydroxide solution (4.15).
pH to 6-9. The collected samples should be stored at 4 ° C or less, stored in the dark, and extracted within 5 days. The extracted eluate at 4 ° C
The following refrigerated and protected from light, the analysis was completed within 4 days.
6.2 Preparation of samples
6.2.1 Activation of solid phase extraction column
The solid phase extraction column (4.21) was fixed on a solid phase extraction unit (5.7) with 5 ml of methanol (4.8) for about 2 ml/min.
The flow rate is passed through a solid phase extraction column. Before the filler is exposed to air, 5 ml of water is added to the column until the water is about 2 ml.
Stop activation.
6.2.2 Enrichment, purification and concentration
Measure 150 ml of the sample in a 250 ml Erlenmeyer flask and pass the activated solid phase extraction column at a flow rate of approximately 2 ml/min.
(6.2.1) After the sample is completely enriched, add 5 ml of acetic acid solution (4.14). After the acetic acid solution is completely discharged, add 8 ml.
The methanol (4.8) was rinsed, and after the methanol completely flowed out, the vacuum pump was used for 5 minutes. Use 7 ml ammonia solution in methanol (4.16)
Elution was carried out and the eluate was collected into a concentrate bottle. The flask was then placed on a nitrogen blower (5.5) and concentrated to 1 ml at 60 °C.
The volume was adjusted to 2.0 ml with water, mixed and filtered through a filter (4.22) into a brown sample vial for testing.
Note. For samples with a suspended solids concentration of more than 12 mg/L, the sample can be adjusted to a pH of about 3 with a hydrochloric acid solution (4.11).
The sonic cleaner (5.6) was sonicated for 10 min and filtered through a filter (4.22) infiltrated with ethanol (4.9). The filtrate is dissolved in sodium hydroxide
The liquid (4.15) was adjusted to pH 6-9 and subjected to solid phase extraction.
6.3 Preparation of blank samples
The test sample was used to replace the sample, and the preparation of the blank sample was carried out in the same manner as in the preparation of the sample (6.2).
7 Analysis steps
7.1 Chromatographic Reference Conditions
Mobile phase A. acetonitrile (4.10), mobile phase B. ammonium acetate solution (4.13); elution procedure is isocratic elution, flow
Phase A/mobile phase B=20/80 (V/V), flow rate. 1.0 ml/min; column temperature. 40 ° C; excitation wavelength. 292 nm, detection
Wavelength. 395 nm; injection volume. 40.0 μl.
7.2 Establishment of calibration curve
Take appropriate amount of benzidine standard use solution I (4.19) or benzidine standard use solution II (4.20), with methanol water
Dilute the solution (4.12) to prepare a standard series of at least 5 concentration points. The mass concentration of benzidine is 2.00 μg/L,
5.00 μg/L, 10.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L (this is the reference concentration). According to the chromatographic reference strip
(7.1), the standard series solution is injected sequentially from low to high concentration, and the mass concentration (μg/L) of benzidine is
On the abscissa, the corresponding peak area or peak height is plotted on the ordinate to establish a calibration curve.
7.3 Determination of samples
The measurement of the sample (6.2.2) was carried out under the same conditions as the establishment of the calibration curve (7.2).
7.4 Blank test
The blank sample (6.3) was measured under the same conditions as the measurement (7.3) of the sample.
8 Calculation and representation of results
8.1 Qualitative analysis
Qualitative according to the retention time of the target compound in the sample and the target compound in the standard series, different wavelengths can be used
The fluorescence intensity below is more qualitatively defined and, if necessary, confirmed by high performance liquid chromatography-triple quadrupole mass spectrometry.
The standard chromatogram of benzidine is shown in Figure 1 under the chromatographic reference conditions (7.1) recommended in this standard.
Figure 1 Standard chromatogram of benzidine (ρ = 50.0 μg/L)
0.00
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 min 0.00
mAU
8.2 Quantitative analysis
The mass concentration of benzidine in the sample ρ (μg/L), calculated according to formula (1).
DVρ
= 11 (1)
Where. ρ--the mass concentration of benzidine in the sample, μg/L;
1-1-- mass concentration of benzidine in the sample obtained from the calibration curve, μg/L;
V1--sample volumetric volume, ml;
V--sampling volume, ml;
D--dilution factor.
8.3 Result representation
When the measurement result is less than 1 μg/L, the three decimal places are retained; when the measurement result is greater than or equal to 1 μg/L, the retention is retained.
Three valid figures.
9 Precision and accuracy
9.1 precision
6 laboratories were applied to surface water samples with a concentration of benzidine spiked at 0.027 μg/L, 0.267 μg/L and 1.06 μg/L.
6 repeated measurements. the relative standard deviations in the laboratory were 1.9% to 7.2%, 1.7% to 7.5%, and 1.7% to 6.3%, respectively;
The relative standard deviations between laboratories were 8.8%, 5.5%, and 7.5%, respectively; the repeatability limits were 0.003 μg/L, 0.032 μg/L, and
0.11 μg/L; reproducibility limits are 0.006 μg/L, 0.047 μg/L and 0.23 μg/L.
Six replicates of 6 samples of domestic wastewater containing benzidine spiked at 0.267 μg/L were tested in 6 laboratories. experiment
The indoor relative standard deviation is 3.4% to 6.6%; the relative standard deviation between laboratories is 6.6%; the repeatability limit is 0.038 μg/L;
The reproducibility limit was 0.057 μg/L.
Industrial wastewater samples with an average concentration of 0.462 μg/L of biphenylamine and a spiked concentration of 0.500 μg/L in 6 laboratories
Six repeated measurements before and after the spike were performed. the relative standard deviations in the laboratory were 1.4% to 7.0% and 1.1% to 5.3%, respectively;
The relative standard deviations between laboratories were 8.1% and 4.5%, respectively; the repeatability limits were 0.062 μg/L and 0.095 μg/L; reproducibility
The limits are 0.12 μg/L and 0.15 μg/L.
9.2 Accuracy
6 laboratories were applied to surface water samples with a concentration of benzidine spiked at 0.027 μg/L, 0.267 μg/L and 1.06 μg/L.
Six times of repeated spike analysis showed that the recoveries ranged from 73.9% to 95.1%, 80.6% to 98.4%, and 84.0%, respectively.
97.0%; the final recoveries were 88.0% ± 15.8%, 88.2% ± 12.4% and 91.0% ± 10.0%.
6 laboratories performed six repeated spikes on the domestic sewage samples with a concentration of 0.267 μg/L of benzidine.
The recovery rate of the spiked standard ranged from 83.8% to 100%; the final value of the spiked recovery was 90.3%±11.2%.
Industrial wastewater samples with an average concentration of 0.462 μg/L of biphenylamine and a spiked concentration of 0.500 μg/L in 6 laboratories
Six times of repeated spike analysis were carried out. the recoveries ranged from 86.6% to 102%; the final value of the spiked recovery was
93.7% ± 10.6%.
10 Quality Assurance and Quality Control
10.1 Blank test
At least one laboratory blank should be made for every 20 samples or batches (≤20 samples/batch) and the results should be below the square
Law detection limit.
10.2 Calibration
The correlation coefficient of the calibration curve should be ≥0.999. One should be determined for every 20 samples or batches (≤20 samples/batch)
For the standard solution of the intermediate concentration point of the calibration curve, the relative error between the measurement result and the concentration of the curve at this point should be within ±15%.
10.3 Parallel samples
At least one parallel sample should be measured for every 20 samples or batches (≤20 samples/batch). The relative deviation of the parallel samples should be
≤20%.
10.4 Matrix addition
At least one matrix spiked sample shall be determined for every 20 samples or batches (≤20 samples/batch), and the spiked recovery rate shall be
Between 70% and 120%.
11 Waste treatment
The organic waste liquid produced in the experiment shall be collected, stored in a centralized manner, and properly marked, and entrusted with qualified units.
Line processing.
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