HJ 1074-2019Water quality--Determination of four organic tin compounds including tributyltin--Liquid chromatography/inductively coupled plasma mass spectrometry (English PDF)
水质 三丁基锡等4种有机锡化合物的测定 液相色谱-电感耦合等离子体质谱法
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Issued by
Ministry of Ecology and Environment
Level / Type
National · Mandatory
Issue date
January 1, 1970
Implementation date
June 30, 2020
Scope
HJ 1074-2019 is the English-translated version of 水质 三丁基锡等4种有机锡化合物的测定 液相色谱-电感耦合等离子体质谱法.
HJ 1074-2019 — This standard specifies the liquid chromatography-inductively coupled plasma quality for the determination of four organotin compounds such as tributyltin in water.
Spectrum method. This standard applies to dibutyltin, tributyltin, dibutyltin in surface water, groundwater, seawater, domestic sewage and industrial wastewater.
Determination of phenyltin and triphenyltin.
When the liquid-liquid extraction method is used, the sampling volume is 1000 ml, the concentration volume is 1.0 ml, and the injection volume is 20.0 µl, the method the detection limit is 0.004 µg/L to 0.005 µg/L, and the lower detection limit is 0.016 µg/L to 0.020 µg/L. When the direct injection method is used, when the injection volume is 20.0 µl, the detection limit of the method is 3 µg/L to 6 µg/L, and the lower detection limit is 12 µg/L to 24 µg/L. See attached Record A.
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Document preview — HJ 1074-2019
National Standard of the People's Republic of China
- ICS
- 13.060
- Classification
- Z 16
Issued by: Ministry of Ecology and Environment
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 Methodology
- 4 Reagents and materials
- 5 Instruments and equipment
- 6 Sample
- 7 Analysis steps
- 8 Calculation and Representation of Results
- 9 Precision and accuracy
- 10 Quality Assurance and Quality Control
- 11 Waste disposal
- 12 Notes
- Appendix A (Normative) Method detection limit and determination limit
- Appendix B (Informative) Precision and accuracy of the method
Foreword
In order to implement the "Environmental Protection Law of the People's Republic of China" Republic of the Marine Environmental Protection Law, protects the ecological environment, protects human health, and regulates four kinds of organotinization such as tributyltin in water Method for determination of compounds, formulated this standard.
This standard specifies four kinds of organotinization such as tributyltin in surface water, groundwater, seawater, domestic sewage and industrial wastewater.
Chromatography-inductively coupled plasma mass spectrometry.
Appendix A of this standard is a normative appendix, and Appendix B 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. Dalian Ecological Environment Monitoring Center, Liaoning Province.
Verification units of this standard. National Environmental Analysis and Testing Center, National Marine Environmental Monitoring Center, Shenyang Ecological Environment, Liaoning Province Environmental Monitoring Center, Fushun Environmental Monitoring Center Station, Dalian Food Inspection Institute and Dalian Product Quality Testing Research Institute.
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 4 organotin compounds including tributyltin Liquid chromatography-inductively coupled plasma mass spectrometry Warning. The reagents and standard solutions used in this method are corrosive and toxic. The 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 the liquid chromatography-inductively coupled plasma quality for the determination of four organotin compounds such as tributyltin in water.
Spectrum method.
This standard applies to dibutyltin, tributyltin, dibutyltin in surface water, groundwater, seawater, domestic sewage and industrial wastewater.
Determination of phenyltin and triphenyltin.
When the liquid-liquid extraction method is used, the sampling volume is 1000 ml, the concentration volume is 1.0 ml, and the injection volume is 20.0 µl, the method the detection limit is 0.004 µg/L to 0.005 µg/L, and the lower detection limit is 0.016 µg/L to 0.020 µg/L. When the direct injection method is used, when the injection volume is 20.0 µl, the detection limit of the method is 3 µg/L to 6 µg/L, and the lower detection limit is 12 µg/L to 24 µg/L. See attached Record A.
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 442 Specifications for Environmental Monitoring in Coastal Waters HJ 493 Technical regulations for the storage and management of water samples HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring
3 Method principle
The organotin compounds in the samples were enriched by liquid-liquid extraction or directly injected, and then separated by liquid chromatography columns, inductively coupled.
Determination by plasma mass spectrometer. Qualitative according to retention time, quantified by external standard method.
4 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 Distilled water.
4.1 Acetonitrile (CH3CN). pure liquid chromatography.
4.2 Acetic acid (CH3COOH). excellent grade pure.
4.3 Triethylamine (C6H15N). Excellent grade pure.
4.4 Methanol (CH3OH). pure by liquid chromatography.
4.5 Acetone (CH3COCH3). pure liquid chromatography.
4.6 Dichloromethane (CH2Cl2). pesticide residue level.
4.7 Sodium chloride (NaCl). excellent grade pure.
Burn at 400 ° C for 2 h, and store in a desiccator after cooling.
4.8 Hydrochloric acid. rho (HCl) = 1.19 g/ml, excellent purity.
4.9 Hydrochloric acid solution. 1 1.
Measure 50.0 ml of hydrochloric acid (4.8) and dilute to 100 ml with experimental water.
4.10 Hydrochloric acid solution. 1 19.
Measure 50.0 ml of hydrochloric acid (4.8) and dilute to 1000 ml with experimental water.
4.11 Hydrochloric acid solution. 1 99.
Measure 1.0 ml of hydrochloric acid (4.8) and dilute to 100 ml with experimental water.
4.12 anhydrous sodium sulfate (Na2SO4).
Burn at 400 ° C for 4 h, and store in a desiccator after cooling.
4.13 Organic tin (dibutyltin, tributyltin, diphenyltin, and triphenyltin) standard stock solution. rho = 1000 mg/L.
Weigh accurately 13.05 mg (accurate to 0.01 mg) of dibutyltin chloride (C8H18Cl2Sn) and 11.22 mg of tributyl Tin chloride (C12H27ClSn), 12.60 mg of diphenyltin chloride (C12H10Cl2Sn), 11.01 mg of triphenyltin chloride (C18H15ClSn) standard material, dissolved in methanol (4.4) or acetone (4.5), and made up to 10.00 ml. Stock solution per liter it contains 1000 mg of dibutyltin, tributyltin, diphenyltin and triphenyltin. Can be stored frozen at -18 ° C or less 1 year. Certified standard solutions can also be purchased directly.
Note. Other organotin standard materials such as organotin acetate can also be purchased to prepare standard stock solutions.
4.14 Standard solution for organotin (dibutyltin, tributyltin, diphenyltin and triphenyltin). rho = 10.0 mg/L.
Measure 1.00 ml of organic tin (dibutyltin, tributyltin, diphenyltin, and triphenyltin) standard stock solution (4.13) Make up to 100 ml with acetonitrile (4.1). It can be stored at -18 °C for 20 days.
4.15 Mobile phase.
Measure 65.0 ml of acetonitrile (4.1), 12.0 ml of acetic acid (4.2), and 0.05 ml of triethylamine (4.3) in 100 ml.
In a brown glass volumetric flask, make up to 100 ml with experimental water.
4.16 PTFE microporous membrane. 0.22 µm.
4.17 Argon. purity is not less than 99.99%.
4.18 External gas. 80% argon and 20% oxygen mixed gas (V/V), the purity of argon and oxygen is not less than 99.99%.
5 Instruments and equipment
Unless otherwise specified, all Class A glass measuring instruments are used in accordance with national standards for analysis.
5.1 Inductively coupled plasma mass spectrometer. equipped with external gas control unit, atomizer with organic waste pipe, platinum sampling Cone, platinum interception cone and organic rectangular tube.
5.2 Liquid chromatography.
5.3 Chromatographic column. C18 column with a particle size of 5.0 µm, a column length of 250 mm, and an inner diameter of 4.6 mm, or other equivalent chromatography column.
5.4 Concentrating device. Rotary evaporation device, KD concentrator, nitrogen blower or other equivalent equipment.
5.5 Separating funnel. 2 L.
5.6 Brown sample bottle. 2.0 ml.
5.7 General laboratory instruments and equipment.
6 Samples
6.1 Collection and storage of samples
Sampling and sampling according to the relevant regulations of HJ 91.1, HJ/T 91, HJ/T 164, HJ 442 and HJ 493 set.
Collect a 2.5 L sample in a brown glass bottle, add an appropriate amount of hydrochloric acid solution (4.9), and adjust the sample pH <= 2. Protect the sample from light, Refrigerated transportation and storage below 4 °C. When using the extraction method, the sample extraction needs to be completed within 24 hours, and the extraction solution can be stored for 7 days;
When using the direct injection method, the samples should be analyzed within 24 hours.
6.2 Preparation of test specimens
6.2.1 Liquid-liquid extraction
6.2.1.1 Extraction
Return the sample to room temperature and confirm that the sample pH is <=2. Measure 1000 ml (reduce sample volume when sample concentration is high) in a separatory funnel (5.5), add the sample to 30 g of sodium chloride (4.7) and shake. Add 60 ml of dichloromethane (4.6), After shaking for 5 min, the layers were allowed to stand still. The organic phase was collected and extracted twice with 60 ml of dichloromethane (4.6). The extracts were combined, Dehydrated over anhydrous sodium sulfate (4.12) and concentrated.
Note 1. If the emulsification is serious during the extraction process, demulsification can be performed by methods including agitation, centrifugation, glass wool filtration, and freezing.
Note 2. The amount of sodium chloride (4.7) can be appropriately reduced in seawater samples.
6.2.1.2 Concentration and solvent conversion
Concentrate the extract with a concentration device (5.4) to about 0.5 ml, add 1 ml of acetonitrile (4.1) and mix well.
Reduce to about 0.5 ml, and then add acetonitrile (4.1) twice to concentrate. Finally, make up to 1.0 ml with mobile phase (4.15). Jingju the tetrafluoroethylene microporous membrane (4.16) was filtered and placed in a brown sample bottle (5.6) for testing.
Note. The solvent evaporation during the concentration process has a greater impact on the recovery of the target.
6.2.2 Direct injection method
The sample was returned to room temperature, and the pH of the sample was adjusted to <= 2 with a hydrochloric acid solution (4.9). Take 1.0 ml sample with PTFE Filter through a microporous membrane (4.16), collect the filtrate in a brown sample bottle (5.6), and take 1.0 ml of acetonitrile (4.1) to wash the the filter membrane and washing solution were combined in a brown sample bottle (5.6) and tested.
6.3 Preparation of blank samples
Replace the sample with experimental water, and prepare a blank sample by following the same procedure as in sample preparation (6.2).
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Reference conditions for liquid chromatography
Mobile phase. V (acetonitrile). V (water). V (acetic acid) = 65. 23. 12, containing 0.05% triethylamine Column temperature. 18 °C ~ 30 °C.
Flow rate. 0.8 ml/min.
Injection volume. 20.0 µl.
7.1.2 Reference conditions for inductively coupled plasma mass spectrometry
See Table 1 for reference conditions for inductively coupled plasma mass spectrometry (ICP-MS).
Table 1 ICP-MS working conditions and parameters
Parameter value
RF power 1600 W
Sampling depth (distance between rectangular tube and sample cone) 9.0 mm Plasma/cooling gas (argon) 15.0 L · min-1 Auxiliary gas (argon) 0.00 L · min-1 Carrier gas (argon) 0.55 L · min-1 External gas (argon-oxygen mixed gas) 0.25 L · min-1 Sampling cone diameter 1.0 mm Intercepting cone diameter 0.4 mm Sampling mode time resolution Acquisition time 1200 s Detection element 116Sn, 118Sn, 120Sn
7.2 Establishment of standard curve
7.2.1 Preparation of standard series
7.2.1.1 Standard series preparation by liquid-liquid extraction
Use organic tin (dibutyltin, tributyltin, diphenyltin, and triphenyltin) standard liquid (4.14) as a mobile phase (4.15) Standard systems diluted to 10.0 µg/L, 20.0 µg/L, 50.0 µg/L, 100 µg/L, 150 µg/L,.200 µg/L Column, stored in a brown vial (5.6).
7.2.1.2 Standard series preparation by direct injection method
Dissolve organic tin (dibutyltin, tributyltin, diphenyltin, and triphenyltin) standard solution (4.14) with hydrochloric acid Solution (4.11) diluted to 10.0 µg/L, 20.0 µg/L, 50.0 µg/L, 100 µg/L, 150 µg/L,.200 µg/L Series, stored in brown vials (5.6).
7.2.2 Establishment of standard curve
Measured in accordance with the instrument reference conditions (7.1), taking the target concentration as the abscissa and the corresponding response value as the vertical Coordinates to establish a standard curve.
7.3 Determination of sample
Measure 20.0 µl sample and follow the same procedure as the standard curve.
7.4 Blank test
Measure 20.0 µl blank sample and follow the same procedure as for sample analysis (7.3).
8 Results calculation and representation
8.1 Qualitative analysis
Characterized by retention time. See Figure 1 for the standard chromatograms of the four organotins.
1-diphenyltin; 2-dibutyltin; 3-triphenyltin; 4-tributyltin.
Figure 1 Standard chromatograms of four organotin
8.2 Calculation of results
8.2.1 Extraction method
The mass concentration of organic tin in the sample is calculated according to formula (1).
Vrho
rho i
In the formula. i-mass concentration of organic tin in the sample, µg/L;
i--mass concentration of organotin in the sample calculated from the standard curve, µg/L;
V--constant volume of sample, ml;
V0--sample volume, ml.
8.2.2 Direct injection method
The mass concentration of organic tin in the sample is calculated according to formula (2).
2xx= Dii (2)
In the formula. i-mass concentration of organic tin in the sample, µg/L;
i--mass concentration of organotin in the sample calculated from the standard curve, µg/L;
D--Sample dilution.
8.3 Representation of results
The number of decimal places in the measurement result is consistent with the detection limit of the method. A maximum of three significant digits are retained.
9 Precision and accuracy
9.1 Precision
Six laboratories spiked four types of organotin with 0.100 µg/L of surface water, 0.020 µg/L of groundwater and 0.020 µg/L seawater samples were extracted 6 times by extraction method. the relative standard deviations in the laboratory were 1.6% to 5.1%, 2.4% to 9.9%, and 2.5% to 9.8%. The relative standard deviations between laboratories are 2.0% to 3.5%, 3.1% to 7.8% and 4.6% to 13%, with repeatability limits of 0.007 µg/L to 0.010 µg/L, 0.003 µg/L to 0.004 µg/L and 0.003 µg/L to 0.005 µg/L, with reproducibility limits ranging from 0.008 µg/L to 0.011 µg/L, 0.003 µg/L to 0.005 µg/L and 0.003 µg/L to 0.008 µg/L.
Six laboratories spiked samples of domestic sewage and.200 µg/L industrial wastewater with concentrations of 100 µg/L Six repeated determinations using direct injection. Relative standard deviations in the laboratory ranged from 0.8% to 5.5% and 0.9% ~ 4.6%, the relative standard deviations between the laboratories are 3.2% ~ 12% and 1.3% ~ 9.4%, and the repeatability limit range 4 µg/L to 8 µg/L and 10 µg/L to 15 µg/L, respectively, with reproducibility limits ranging from 10 µg/L to 37 µg/L and 15 µg/L to 47 µg/L.
See Appendix B for specific precision data.
9.2 Accuracy
Six laboratories spiked four types of organotin with 0.100 µg/L of surface water, 0.020 µg/L of groundwater and 0.020 µg/L of seawater was measured by extraction method. the spiked recoveries ranged from 74.6% to 90.3% and 68.5% to 93.0% and 69.0% ~ 109%, the final values of the spiked recovery rates are 77.5% ± 4.8% ~ 86.1% ± 5.0%, 78.8% ± 12.4% ~ 85.9% ± 8.4% and 77.3% ± 7.2% ~ 90.3% ± 24.2%.
Six laboratories sampled 4 kinds of organic tin with a concentration of 100 µg/L of domestic sewage and.200 µg/L of industrial waste water.
Measured by direct injection method. recovery range of standard addition is 80.4% ~ 106% and 80.5% ~ 102%, recovery of standard addition the final value range of the rate is 86.4% ± 5.6% ~ 93.7% ± 13.2% and 86.4% ± 16.6% ~ 94.3% ± 7.0%.
See Appendix B for specific accuracy data.
10 Quality Assurance and Quality Control
10.1 Blank test
At least one blank test is performed for every 20 samples or batches of samples (<=20 samples/batch).
Out of limits.
10.2 Calibration
The correlation coefficient of the standard curve r >= 0.990, measured in one curve every 20 samples or batch samples (<= 20 samples/batch) for the inter-check point, the relative error between the measurement result and the concentration of the corresponding point of the standard curve should be within ± 20%.
10.3 Parallel samples
Every 20 samples or each batch of samples (<= 20 samples/batch), at least one parallel double sample shall be measured.
The deviation should be <=20%.
10.4 Matrix Spiking
Measure at least one matrix spiked sample for every 20 samples or batches (<=20/batch), and its spike recovery range it should be between 60% and 120%.
11 Waste treatment
The waste generated during the experiment should be collected in a centralized manner, be labeled accordingly, and be entrusted to a qualified unit for processing.
12 Notes
12.1 When the signal background of the instrument is high, the acetonitrile and the reagents used to prepare the mobile phase should be checked and replaced if necessary.
12.2 All glassware should be soaked in hydrochloric acid solution (4.10) for more than 24 hours before use.
Appendix A
(Normative appendix) Method detection limit and determination limit the detection limits and lower detection limits for each target compound in the extraction method are shown in Table A.1.
Table A.1 Extraction detection limits and determination limits
No. Compound name Detection limit (µg/L) Lower detection limit (µg/L)
1 Diphenyltin 0.004 0.016
2 Dibutyltin 0.005 0.020
3 Triphenyltin 0.004 0.016
4 Tributyltin 0.004 0.016 the detection limits and lower detection limits of each target compound for the direct injection method are shown in Table A.2.
Table A.2 Detection limit and determination limit of direct injection method
No. Compound name Detection limit (µg/L) Lower detection limit (µg/L)
1 Diphenyltin 4 16
2 Dibutyltin 6 24
3 Triphenyltin 3 12
4 Tributyltin 3 12
Appendix B
(Informative appendix) Method precision and accuracy B.1 Extraction method the results of the extraction precision are summarized in Table B.1.
Table B.1 Precision of extraction method
Serial number
Compound
name
sample
Types of
concentration
(Mg/L)
Relative standards in the laboratory Quasi deviation range (%) Interlaboratory relative standard Quasi deviation range (%) Repeatability limit r (Mg/L) Reproducibility limit R (Mg/L) Diphenyl Kissi Surface water 0.100 2.4 ~ 5.1 3.1 0.010 0.011 Groundwater 0.020 3.4 ~ 9.9 7.8 0.003 0.005 Seawater 0.020 4.8 ~ 8.5 4.6 0.003 0.003 Erding Kissi Surface water 0.100 2.4 ~ 4.9 2.9 0.009 0.010 Groundwater 0.020 2.9 ~ 9.9 4.9 0.004 0.004 Seawater 0.020 7.5 ~ 9.8 13 0.005 0.008 Triphenyl Kissi Surface water 0.100 1.6 ~ 3.7 3.5 0.007 0.011 Groundwater 0.020 2.4 ~ 8.8 5.9 0.003 0.004 Seawater 0.020 2.5 ~ 9.4 8.7 0.004 0.006 Sanding Kissi Surface water 0.100 1.9 ~ 3.7 2.0 0.007 0.008 Groundwater 0.020 3.6 ~ 8.6 3.1 0.003 0.003 Seawater 0.020 3.9 ~ 7.9 9.3 0.003 0.005 the accuracy results of the extraction method are summarized in Table B.2.
Table B.2 Extraction accuracy
Compound
name
sample
Types of
Actual sample concentration Degree (µg/L) Spiked samples Concentration (µg/L) Spike recovery range(%) (%) P ) (% (%)2 SP+/-Diphenyl Kissi Surface water ND 0.100 74.6 ~ 80.6 77.5 2.4 77.5 ± 4.8 Groundwater ND 0.020 68.5 ~ 86.0 78.8 6.2 78.8 ± 12.4 Seawater ND 0.020 73.5 ~ 82.0 77.3 3.6 77.3 ± 7.2 Erding Kissi Surface water ND 0.100 83.1 ~ 90.3 86.1 2.5 86.1 ± 5.0 Groundwater ND 0.020 78.5 ~ 90.0 85.9 4.2 85.9 ± 8.4 Seawater ND 0.020 71.5 ~ 109 90.3 12 90.3 ± 24 Triphenyl Kissi Surface water ND 0.100 82.3 ~ 90.3 86.0 3.0 86.0 ± 6.0 Groundwater ND 0.020 79.5 ~ 93.0 83.7 5.0 83.7 ± 10.0 Seawater ND 0.020 76.5 ~ 97.0 88.2 7.6 88.2 ± 15.2 Sanding Kissi Surface water ND 0.100 77.9 ~ 82.2 80.2 1.6 80.2 ± 3.2 Groundwater ND 0.020 79.5 ~ 86.5 84.8 2.7 84.8 ± 5.4 Seawater ND 0.020 69.0 ~ 89.0 80.6 7.5 80.6 ± 15.0 B.2 Direct injection method See Table B.3 for the summary results of direct injection method precision.
Table B.3 Precision of direct injection method
Serial number
Compound
name
sample
Types of
concentration
(Mg/L)
Relative standards in the laboratory Quasi deviation range (%) Interlaboratory relative standard Quasi deviation range (%) Repeatability limit (Mg/L) Limit of reproducibility (Mg/L) Diphenyl Kissi Domestic sewage 100 1.6 ~ 4.7 12 8 37 Industrial wastewater.200 1.5 ~ 3.9 9.4 13 47 Erding Kissi Domestic sewage 100 1.0 ~ 2.1 7.6 4 20 Industrial wastewater.200 0.9 ~ 2.8 3.7 10 21 Triphenyl Kissi Domestic sewage 100 0.8 ~ 3.9 7.1 6 19 Industrial wastewater.200 1.7 ~ 4.4 4.4 15 26 Sanding Kissi Domestic sewage 100 1.5 ~ 5.5 3.2 7 10 Industrial wastewater.200 1.4 ~ 4.6 1.3 15 15 the accuracy results of direct injection are summarized in Table B.4.
Table B.4 Accuracy of direct injection method
Compound
name
sample
Types of
Actual sample
Concentration (µg/L) Spiked sample Degree (µg/L) Spike recovery range(%) (%) P ) (% (%)2 SP+/-Diphenyl Kissi Domestic sewage ND 100 80.4 ~ 106 92.3 11 92.3 ± 22 Industrial wastewater ND.200 80.5 ~ 102 86.4 8.3 86.4 ± 16.6 Erding Kissi Domestic sewage ND 100 86.5 ~ 103 92.8 7.3 92.8 ± 14.6 Industrial wastewater ND.200 90.0 ~ 100 94.3 3.5 94.3 ± 7.0 Triphenyl Kissi Domestic sewage ND 100 86.4 ~ 106 93.7 6.6 93.7 ± 13.2 Industrial wastewater ND.200 85.0 ~ 95.5 88.5 3.9 88.5 ± 7.8 Sanding Kissi Domestic sewage ND 100 81.5 ~ 89.7 86.4 2.8 86.4 ± 5.6 Industrial wastewater ND.200 89.0 ~ 92.5 91.3 1.2 91.3 ± 2.4
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