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HJ 1002-2018: Water quality - Determination of butyl xanthate - Liquid chromatography/triple quadrupole tandem mass spectrometry
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Water quality - Determination of butyl xanthate - Liquid chromatography/triple quadrupole tandem mass spectrometry
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HJ 1002-2018
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Basic data | Standard ID | HJ 1002-2018 (HJ1002-2018) | | Description (Translated English) | Water quality - Determination of butyl xanthate - Liquid chromatography/triple quadrupole tandem mass spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 13,179 | | Date of Issue | 2018-12-26 | | Date of Implementation | 2019-06-01 | | Regulation (derived from) | Ministry of Ecology and Environment Announcement No. 73 of 2018 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1002-2018: Water quality - Determination of butyl xanthate - Liquid chromatography/triple quadrupole tandem mass spectrometry
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Water quality - Determination of butyl xanthate - Liquid chromatography/triple quadrupole tandem mass spectrometry
National Environmental Protection Standard of the People's Republic
Determination of butyl xanthate in water - liquid chromatography - triple quadrupole mass spectrometry
Published on.2018-12-26
2019-06-01 Implementation
Ministry 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... 2
7 Analysis steps...3
8 Calculation and representation of results...5
9 Precision and Accuracy...7
10 Quality Assurance and Quality Control...7
11 Waste treatment...7
Appendix A (informative) The precision and accuracy of the method...8
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 the Prevention and Control of Water Pollution, to protect the ecological environment,
To ensure human health, standardize the determination method of butylxanthine in water, and formulate this standard.
This standard specifies liquid chromatography-triple quadrupole tandem mass spectrometry for the determination of butylxanthogen in surface water, groundwater, domestic sewage and industrial wastewater.
Appendix A of this standard is an informative annex.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring and the Department of Regulations and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Dalian Environmental Monitoring Center.
This standard is verified by. Liaoning Provincial Environmental Monitoring Experimental Center, Chengdu Environmental Monitoring Center Station, Petrochemical Park Monitoring Station,
Sichuan Environmental Monitoring Station, Chongqing Ecological Environment Monitoring Center, Liaoning Marine Fisheries Research Institute and Jiangsu Environmental Monitoring Center.
This standard is approved by the Ministry of Ecology and Environment on December 26,.2018.
This standard has been implemented since June 1,.2019.
This standard is explained by the Ministry of Ecology and Environment. 1
Determination of butyl xanthate in water - liquid chromatography - triple quadrupole mass spectrometry
Warning. The acetonitrile and butyl xanthate used in the experiment are toxic and harmful compounds.
Avoid contact with skin and clothing during the experiment. The solution preparation process should be carried out in a fume hood.
1 Scope of application
This standard specifies liquid chromatography-triple quadrupole tandem mass spectrometry for the determination of butyl xanthogen in water.
This standard applies to the determination of butyl xanthogen in surface water, groundwater, domestic sewage and industrial wastewater.
The target of this standard is butyl xanthogen, excluding other xanthogens.
When the injection volume is 10.0 μl, the detection limit of butyl xanthogen measured in this standard is 0.2 μg/L, and the lower limit of determination is 0.8 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 directly injected after filtration, separated by liquid chromatography column, and examined by mass spectrometry under multiple reaction monitoring (MRM) conditions.
Butyl xanthic acid was measured and quantified by internal standard method according to retention time and characteristic ion characterization.
4 reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. The experimental water was pure water containing no target.
4.1 Acetonitrile (CH3CN). Pure by liquid chromatography.
4.2 Ammonia (NH3·H2O). Excellent grade.
4.3 Butyl xanthate. Potassium butyl xanthate (C5H9OS2K) or sodium butylxanthate (C5H9OS2Na), purity ≥95%.
4.4 Formic acid (HCOOH). Excellent grade.
4.5 Sodium hydroxide (NaOH).
4.6 Sodium hydroxide solution. ρ(NaOH) = 0.4 g/ml.
Weigh 4 g of sodium hydroxide (4.5) dissolved in water and dilute to 10 ml.
4.7 Ammonia solution 1. 1 1.
4.8 Ammonia solution 2. 2
Take a certain amount of ammonia (4.2) dissolved in water, adjust the pH ≈ 9.5, use within 8 h.
4.9 Formic acid solution. 1 1.
4.10 Standard stock solution of butylxanthogen. ρ(C4H9OCSSH) = 100 mg/L.
Weigh butyl xanthate (0.0330 g potassium butyl xanthate or 0.0302 g butyl xanthate) (4.3), add a small amount
Dissolve in water, transfer to a 250 ml brown volumetric flask (5.4), add water to the standard line, and add 3 drops of sodium hydroxide solution (4.6)
Shake well, make the pH 9~10, and add water to make up. Transfer the solution to a brown glass reagent bottle, and store the stock solution at 4 ° C or less.
Stored in the dark, it can be stored for 20 days. Commercially available certified standard solutions can also be purchased directly.
4.11 Standard use solution of butyl xanthogen. ρ(C4H9OCSSH) = 1.00 mg/L.
Pipette 1.00 ml of butyl xanthogen standard stock solution (4.10) into a 100 ml brown volumetric flask with ammonia solution 2
(4.8) Constant volume. Available now.
4.12 Internal standard stock solution. ρ(C8H6Cl2O3-13C6)=100 mg/L.
Directly purchase certified 2,4-dichlorophenoxyacetic acid-13C6 standard solution. The internal standard stock solution is stored in the refrigerator at 4 ° C or less and stored in the dark.
Can be saved for one year. Or save it by referring to the manufacturer's product description.
4.13 Internal standard use solution. ρ=1.0 mg/L.
Dilute the internal standard stock solution (4.12) to 1.0 mg/L with water. Now available.
4.14 Membrane. 0.22 μm pore size, hydrophilic polypropylene, glass fiber, hydrophilic polytetrafluoroethylene or other equivalent materials.
4.15 Nitrogen. Purity ≥ 99.9%.
5 instruments and equipment
5.1 High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometer. High performance liquid chromatography with gradient elution and mass spectrometer equipped with electrospray ionization source (ESI).
5.2 Column. C18 column or other equivalent column with a column length of 50 mm, an inner diameter of 2.1 mm, and a packing particle size of 1.7 μm.
Note. Since the mobile phase has a pH of 9.5, a column suitable for mobile phase pH ≥ 10 should be used.
5.3 Brown vial. 2.0 ml.
5.4 Brown volumetric flask. 250 ml.
5.5 Sampling bottle. 40 ml brown glass bottle, screw cap (with Teflon coated gasket).
5.6 Microinjectors. 10 μl, 50 μl, 100 μl and 1 ml.
5.7 Common instruments and equipment used in general laboratories.
6 samples
6.1 Sample collection and preservation
Samples were taken in accordance with the relevant regulations of HJ/T 91 and HJ/T 164.
When collecting samples, slowly pour the sample into the sample bottle (5.5) near the full bottle, with ammonia solution 1 (4.7) or formic acid solution (4.9)
Adjust the pH of the sample to 9~10, add the sample to the full bottle, and mix. The samples were stored in the dark at 4 ° C or less and stored within 48 h.
6.2 Preparation of samples
The sample was filtered through a filter (4.14), 1.0 ml was placed in a brown vial (5.3), and 10.0 μl of internal standard solution was added.
(4.13), mix and test.
Note. The sample is returned to room temperature and the pH is measured. If the pH of the sample changes, re-use ammonia 1 (4.7) or formic acid (4.9) to adjust the pH to 9-10.
6.3 Preparation of blank samples
The test water was used instead of the sample, and a laboratory blank sample was prepared in the same manner as in the preparation of the sample (6.2).
7 Analysis steps
7.1 Measurement conditions
7.1.1 Liquid Chromatograph Reference Conditions
Mobile phase. mobile phase A is acetonitrile (4.1), mobile phase B is aqueous ammonia solution 2 (4.8), gradient elution procedure is shown in Table 1;
Column temperature. 40 ° C;
Injection volume. 10.0 μl;
Flow rate. 0.2 ml/min.
Table 1 Liquid chromatography mobile phase gradient elution procedure
7.1.2 Mass Spectrometer Reference Conditions
Ionization mode. negative ion mode (ESI-);
Ionization voltage. 3000 V;
Ion source heating gas temperature. 120 ° C;
Detection method. Multiple reaction monitoring (MRM), the specific conditions are shown in Table 2.
Table 2 Multiple reaction monitoring conditions of target compounds
7.1.3 Tuning
Perform mass spectrometer mass and resolution tuning according to the instrument instructions, and test after the instrument performance is normal...
7.2 Calibration
7.2.1 Establishment of the standard curve
Take a standard amount of butyl xanthogen (4.11) in ammonia solution 2 (4.8) to prepare a standard of 5 concentration points.
The series, butyl xanthogen concentrations of 1.00 μg/L, 5.00 μg/L, 10.0 μg/L, 50.0 μg/L and 100 μg/L, respectively,
Add 10.0 μl of internal standard solution (4.13) per ml of standard series solution to make the internal standard mass concentration 10.0 μg/L.
Available in brown vials (5.3).
The standard series solution is injected sequentially in the order of decreasing concentration to the mass of butyl xanthogen in the standard series solution.
The concentration is the abscissa, the peak area (or peak height) of butyl xanthate and the peak area (or peak height) ratio of the internal standard and the internal standard
The product of the concentration is plotted on the ordinate and a standard curve is established. Or calculate the average relative response factor RRF of butyl xanthate according to formula (1) and formula (2).
7.2.2 Standard sample spectrum
Figure 1 Total ion chromatogram of internal standard and butyl xanthate
7.3 Sample determination
The measurement of the sample (6.2) was carried out in the same manner as in the establishment of the standard curve (7.2.1).
Note. If the concentration of butylxanthate in the sample exceeds the highest point of the calibration curve, dilute with ammonia solution 2 (4.8) and measure.
7.4 Blank test
The blank sample (6.3) was measured in the same manner as in the sample measurement (7.3).
8 Calculation and representation of results
8.1 Qualitative analysis
Characterize the retention time of the sample and the relative abundance of the qualitative ion/quantitative ion.
The relative abundance of the qualitative ion/quantitative ion in the sample (Ksam) and the corresponding qualitative ion in the standard solution close to the concentration
/ Quantitative ion relative abundance (Kstd) is compared, the resulting deviation is within the maximum allowable deviation range specified in Table 3, then it can be judged
Butyl xanthogen was present in the sample. Ksam and Kstd are calculated according to formula (3) and formula (4), respectively.
Table 3 Maximum allowable deviation of relative ion abundance
8.3.2 Average relative response factor method
When butyl xanthic acid is quantified by the average relative response factor method, the mass concentration of butyl xanthogen in the sample is ρx
Calculated according to formula (6).
8.4 Result representation
When the measurement result is less than 100 μg/L, one digit after the decimal point is retained, and when the measurement result is greater than or equal to 100 μg/L,
Keep 3 significant digits. 7
9 Precision and accuracy
9.1 precision
6 laboratories added 1.0 ug/L, 10.0 μg/L and 50.0 μg/L of surface water to butyl xanthogen, respectively.
The tailings leaching wastewater with a concentration of 20.0 μg/L, 100 μg/L and 500 μg/L and the influent of the sewage treatment plant were tested repeatedly.
The relative standard deviation of the experimental room ranges from 1.5% to 11%, and the relative standard deviation between laboratories ranges from 0.5% to 7.3%.
The repeatability range is from 0.3 μg/L to 32 μg/L, and the reproducibility range is from 0.3 μg/L to 32 μg/L. See Appendix A.
9.2 Accuracy
6 laboratories added 1.0 ug/L, 10.0 μg/L and 50.0 μg/L of surface water to butyl xanthogen, respectively.
The tailings leaching wastewater with a concentration of 20.0 μg/L, 100 μg/L and 500 μg/L and the influent of the sewage treatment plant were tested repeatedly.
The recoveries ranged from 77.2% to 113%. See Appendix A.
10 Quality Assurance and Quality Control
10.1 Blank test
At least one blank test shall be performed for each batch of samples (≤20/batch), and the test results shall not exceed the detection limit of the method.
10.2 Calibration
The correlation coefficient of the standard curve is r≥0.995, or the relative standard deviation of the relative response factor (RRF) should be ±20%.
Between each batch (≤20/batch), a curve intermediate check point is determined, and the measured result is corresponding to the standard curve.
The relative error should be between ±20%.
10.3 Parallel samples
At least one parallel double sample should be determined for each batch of samples (≤20/batch), and the relative deviation of the parallel double sample results should be between ±20%.
10.4 Matrix addition
At least one matrix spiked sample shall be determined for each batch of samples (≤20 cells/batch), and the spiked recovery range shall be between 70% and 120%.
11 Waste treatment
The waste liquid generated in the experiment should be collected in a centralized manner, and the corresponding identification should be carried out, and a qualified unit should be entrusted to handle it. 8
Appendix A
(informative appendix)
Method precision and accuracy
Six laboratories tested different concentrations of samples. The results of precision and accuracy are shown in Table A.1 and Table A.2.
Table A.1 Precision of the method
Table A.2 Method accuracy
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