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HJ 1210-2021 English PDF

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HJ 1210-2021: Soil and sediment - Determination of 13 aniline compounds and 2 benzidine compounds - Liquid chromatography-triple quadrupole mass spectrometry
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HJ 1210-2021English559 Add to Cart 5 days [Need to translate] Soil and sediment - Determination of 13 aniline compounds and 2 benzidine compounds - Liquid chromatography-triple quadrupole mass spectrometry Valid HJ 1210-2021

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Basic data

Standard ID HJ 1210-2021 (HJ1210-2021)
Description (Translated English) Soil and sediment - Determination of 13 aniline compounds and 2 benzidine compounds - Liquid chromatography-triple quadrupole mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 24,22
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1210-2021: Soil and sediment - Determination of 13 aniline compounds and 2 benzidine compounds - Liquid chromatography-triple quadrupole mass spectrometry


---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.
(Determination of 13 anilines and 2 benzidines in soils and sediments by liquid chromatography-triple quadrupole mass spectrometry) National Ecological Environment Standard of the People's Republic of China Soil and sediment 13 anilines and 2 biphenyls Determination of Amines by Liquid Chromatography - Triple Quadrupole rod mass spectrometry Soil and sediment-Determination of 13 aniline compounds and 2 benzidine compounds-Liquid chromatography-triple quadrupole mass spectrometry This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment. Published on 2021-11-15 2022-06-01 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Principles of the method...1 4 Interference and cancellation...1 5 Reagents and materials...2 6 Instruments and equipment...3 7 Samples...3 8 Analysis steps...4 9 Result calculation and representation...7 10 Accuracy...8 11 Quality Assurance and Quality Control...9 12 Waste Disposal...10 Appendix A (normative appendix) detection limit and lower limit of determination of the method...11 Appendix B (Normative Appendix) Quantitative Mode...12 Appendix C (Informative Appendix) Mass Spectrometry Reference Conditions...13 Appendix D (informative) Accuracy of the method...15 Determination of 13 anilines and 2 benzidine compounds in soil and sediment liquid chromatography-triple quadrupole mass spectrometry Warning. The standard substance used in the experiment has high toxicity or carcinogenicity. The solution preparation and sample preparation process should be in a fume hood When operating, wear protective equipment as required to avoid inhalation into the respiratory tract or contact with skin and clothing.

1 Scope of application

This standard specifies the liquid chromatography-triple quadrupole mass spectrometry method for the determination of anilines and benzidine compounds in soil and sediments. This standard applies to benzidine, aniline, 4-methylaniline, 2-methoxyaniline, 3-methylaniline, 2-methylbenzene in soil and sediment Amine, 2,4-dimethylaniline, 4-nitroaniline, 3-nitroaniline, 4-chloroaniline, 2-naphthylamine, 2,6-dimethylaniline, 3-chloroaniline, 3,3 '- Determination of dichlorobenzidine and N-nitroso diphenylamine in total of 13 anilines and 2 benzidine compounds. When the sampling volume is 5.0 g and the constant volume is 1.0 ml, the method detection limits for 13 anilines and 2 benzidine compounds are 2 μg/kg～4 μg/kg, the lower limit of determination is 8 μg/kg～16 μg/kg. See Appendix A for details.

2 Normative references

This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. GB 17378.3 Marine Monitoring Specification Part 3.Sample Collection, Storage and Transportation GB 17378.5 Marine Monitoring Specification Part 5.Sediment Analysis HJ/T 166 Technical Specification for Soil Environment Monitoring HJ 494 Water Quality Sampling Technical Guide HJ 613 Gravimetric Method for Determination of Soil Dry Matter and Moisture

3 Principles of the method

Aniline and benzidine target compounds in soil or sediment are extracted under alkaline conditions, purified, concentrated and fixed to volume, and then used in liquid Phase chromatography-triple quadrupole mass spectrometer separation and detection. According to retention time and characteristic ion identification, internal standard method for quantification.

4 Interference and cancellation

When there is matrix effect interference in the sample, it can be reduced by cleaning the sample, optimizing the chromatographic conditions, reducing the sample volume or injection volume, etc. Low or eliminate interference.

5 Reagents and Materials

Unless otherwise stated, analytical reagents that meet national standards are used in the analysis, and the experimental water is freshly prepared and does not contain target compounds. of pure water. 5.1 Dichloromethane (CH2Cl2). chromatographically pure. 5.2 n-hexane (C6H14). chromatographically pure. 5.3 Acetone (CH3COCH3). chromatographically pure. 5.4 Methanol (CH3OH). chromatographically pure. 5.5 Formic acid (HCOOH). chromatographically pure. 5.6 Sodium thiosulfate pentahydrate (Na2S2O3 5H2O). 5.7 Ammonia (NH3·H2O). w(NH3·H2O)=25%～28%. 5.8 n-hexane-acetone mixed solvent. Mix with n-hexane (5.2) and acetone (5.3) in a 1.1 volume ratio. 5.9 Formic acid-methanol solution. Pipette 100 μl of formic acid (5.5) into 1000 ml of methanol (5.4). 5.10 Formic acid aqueous solution. Pipette 100 μl of formic acid (5.5) into 1000 ml of water. 5.11 Standard stock solution of aniline and benzidine compounds. ρ=100 mg/L～200 mg/L. It can be prepared with standard material, the purity of the standard material is more than 99%, dissolved in methanol (5.4), frozen below -18 ℃, sealed and protected from light Save it for 3 months. You can also directly purchase certified standard solutions and store them with reference to the product instructions. 5.12 Standard intermediate solution for aniline and benzidine compounds. ρ=5.00 mg/L～10.0 mg/L. Dilute the standard stock solution (5.11) of aniline and benzidine compounds with methanol (5.4), the concentration of 3-nitroaniline is 10.0 mg/L, its The concentration of the remaining compounds was 5.00 mg/L. The intermediate solution should be frozen, sealed, and protected from light below -18 ℃, and N-nitroso diphenylamine can be stored for 1 months, the remaining compounds can be stored for 3 months. 5.13 Internal standard stock solution. ρ=1000 mg/L. Recommended internal standards are benzidine-d8, aniline-d5, 3,3'-dichlorobenzidine-d6 and N-nitrosodiphenylamine-d6, and isotopic substitutions are also available For other aniline compounds, see Appendix B. It can be prepared with standard material, the purity of the standard material is more than 99%, dissolved in methanol (5.4), Freeze, seal, and protect from light below -18 °C for 3 months. The standard solution can also be purchased directly and stored with reference to the product manual. 5.14 Internal standard intermediate solution. ρ=20.0 mg/L. Dilute the internal standard stock solution (5.13) with methanol (5.4), and the concentration of each internal standard is 20.0 mg/L. The intermediate solution is frozen below -18 ℃, Sealed and protected from light, N-nitrosodiphenylamine-d6 can be stored for 1 month, and other internal standards can be stored for 3 months. 5.15 Internal standard solution I. ρ=2.00 mg/L. Dilute the internal standard intermediate solution (5.14) with methanol (5.4), the concentration of each internal standard is 2.00 mg/L. The solution should be frozen below -18 ℃, Sealed and protected from light, it can be stored for 1 month. 5.16 Internal standard solution II. ρ=50.0 μg/L. Dilute the internal standard intermediate solution (5.14) with water, and add an appropriate amount of methanol (5.4), the concentration of each internal standard is 50.0 μg/L, and the methanol The product ratio is 25%, and it is ready for immediate use. 5.17 Standard solution for aniline and benzidine compounds. ρ=1.00 mg/L～2.00 mg/L. Dilute the standard intermediate solution (5.12) of aniline and benzidine compounds with water, and add an appropriate amount of internal standard solution I (5.15) and methanol (5.4), the concentration of 3-nitroaniline was 2.00 mg/L, the concentration of other compounds was 1.00 mg/L, the concentration of internal standard was 50.0 μg/L, and the The volume ratio of alcohol is 25%, and it is prepared for immediate use. 5.18 Quartz sand. particle size of 0.150 mm to 0.450 mm (100 mesh to 40 mesh). Bake at 400 °C for 4 h in a muffle furnace, and store in a ground glass bottle after cooling. 5.19 Solid phase extraction column. the packing is C18, 1 g/6 ml, or other equivalent solid phase extraction column suitable for non-polar to moderately polar compounds. 5.20 Syringe filter. The filter membrane is made of hydrophilic polytetrafluoroethylene with a pore size of 0.22 μm. 5.21 Nitrogen. purity ≥99.99%.

6 Instruments and equipment

6.1 Vials. Amber glass straight wall jars with Teflon liner, 500 ml. 6.2 Liquid chromatography-triple quadrupole mass spectrometer. liquid chromatography has the function of gradient elution, and mass spectrometer is charged with electrospray ionization source (ESI source). triple quadrupole mass spectrometer. 6.3 Chromatographic column. a C18 reversed-phase chromatographic column with a particle size of 1.8 μm, a column length of 50 mm and an inner diameter of 4.6 mm or other chromatographic columns with similar performance column. 6.4 Ultrasonic cleaner. 40 kHz, power ≥ 100 W. 6.5 Refrigerated centrifuge. the rotation speed is ≥6000 r/min. 6.6 Concentration device. nitrogen blowing concentrator, rotary evaporator or other equipment with equivalent performance. 6.7 Solid phase extraction device. automatic or manual, the flow rate can be adjusted. 6.8 Vortex mixer. 6.9 Freeze Dryers. 6.10 Stoppered centrifuge tube. glass or polypropylene, 30 ml. 6.11 Aluminum foil ziplock bag. 6.12 Common laboratory instruments and equipment.

7 samples

7.1 Sample Collection and Storage Soil samples were collected according to relevant requirements of HJ/T 166, water sediment samples were collected according to relevant requirements of HJ 494, and marine sediment samples were collected according to relevant requirements of HJ 494. The samples were collected in accordance with the relevant requirements of GB 17378.3.Samples should be stored in clean sample vials (6.1) after collection and should be avoided during transportation. Light, sealed, refrigerated, and shipped back to the laboratory for analysis as soon as possible. If the analysis cannot be done temporarily, 4-chloroaniline, 4-nitroaniline and 3-nitroaniline can be selected Keep refrigerated below 4 ℃ or cryopreserved below -18 ℃, other target compounds should be stored frozen below -18 ℃, see Table 1 for details. cryopreservation In order to avoid breaking the glass bottle during storage, transfer the sample to an aluminum foil ziplock bag (6.11) for airtight storage. 7.2 Preparation of samples Use a freeze dryer (6.9) to dehydrate and dry the samples, grind and sieve the freeze-dried samples, and homogenize them to a size of about 0.25 mm. particle. Prepared samples are stored in pre-cleaned sample vials (6.1) and analyzed as soon as possible according to the sample storage time. 7.3 Determination of moisture The dry matter content of soil samples was determined according to HJ 613, and the moisture content of sediment samples was determined according to GB 17378.5. 7.4 Preparation of test specimens 7.4.1 Extraction Weigh 5 g (accurate to 0.01 g) of the sample (7.2) into a stoppered centrifuge tube (6.10), add 1 g of sodium thiosulfate pentahydrate (5.6), Add 50.0 μl of the internal standard intermediate solution (5.14) and 10.0 ml of n-hexane-acetone mixed solvent (5.8) in turn, seal it with a vortex mixer (6.8) Mix well. After ultrasonic extraction for 30 min (place an ice box in the water tank to ensure that the temperature of the water bath is always lower than 25 °C), refrigerated centrifugation at 6000 r/min After 10 min, the supernatant was filtered through a hydrophilic polytetrafluoroethylene needle filter (5.20), and the filtrate was to be purified. Note. If the pH value of the sample is not between 7 and 10, use formic acid (5.5) or ammonia water (5.7) to adjust the pH value to 7 to 10, and then perform extraction. 7.4.2 Purification Fix the C18 solid phase extraction cartridge (5.19) on the solid phase extraction device (6.7). Rinse the cartridge with 5 ml of dichloromethane (5.1), Then use 5 ml methanol (5.4) to equilibrate the extraction column, close the flow control valve after the extraction column is full, soak for 5 minutes, slowly open the control valve, Discard the effluent. Before the solvent is drained, transfer 2.00 ml of the filtered sample extract (7.4.1) to the column and discard the effluent. exist Before the solvent is drained, close the control valve, add 5 ml of methanol (5.4), slowly open the control valve after 5 min, and receive the eluent until it flows out completely. 7.4.3 Concentration At room temperature, turn on nitrogen until there are slight fluctuations on the surface of the solvent (avoid vortex formation). Concentrate the purified eluent (7.4.2) with nitrogen blowing At least 0.8 ml, dilute to 1.0 ml with methanol (5.4), and transfer to a 2 ml brown sample bottle. Refrigerate below 4 °C, and complete the analysis within 7 days. Or freeze below -18 °C, and complete the analysis within 28 days. 7.4.4 Preparation of test solutions Accurately pipette 250 μl of the concentrated purified eluent (7.4.3), make up to 1.0 ml with water, mix well, use a syringe filter (5.20) After filtration, it was transferred to a 2 ml brown sample bottle for analysis on the machine. Note. If the concentration of the target compound in the sample exceeds the highest point of the standard curve, reduce the sampling amount and prepare the sample again. 7.5 Preparation of blank samples Using quartz sand (5.18) in place of the actual sample, prepare a blank sample in the same manner as in the preparation of the sample (7.4).

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 Liquid chromatography reference conditions Mobile phase A. formic acid-methanol solution (5.9), mobile phase B. formic acid aqueous solution (5.10), gradient elution procedure is shown in Table 2; flow rate. 8.1.2 Reference conditions for mass spectrometry Ion source. Electrospray ion source (ESI), positive ion mode. Monitoring method. multiple reaction monitoring (MRM). See Appendix C for the remaining conditions. 8.1.3 Instrument tuning There are certain differences in the tuning parameters of instruments from different manufacturers. Calibration of instrument mass and resolution to ensure that the instrument is in the best test state. 8.2 Calibration 8.2.1 Establishment of standard curve Dilute the standard solution (5.17) for aniline and benzidine compounds with internal standard solution II (5.16), and prepare at least 6 concentrations of standard solution. quasi-series (see Table 3 for reference mass concentration), stored in a brown sample bottle for testing. According to the reference conditions of the instrument (8.1), analyze the standard series of solutions from low concentration to high concentration in turn. The mass concentration of the target compound is the abscissa, the ratio of the peak area (or peak height) of the target compound to the peak area (or peak height) of the corresponding internal standard The product with the concentration of the internal standard is the ordinate, and a standard curve is established. 8 μg/kg, 31 μg/kg～65 μg/kg and 38 μg/kg～109 μg/kg; reproducibility limits are 10 μg/kg～28 μg/kg, 104 μg/kg～ 314 μg/kg and 153 μg/kg to 446 μg/kg. Six laboratories performed six replicates of a uniform sample of loam and marine sediment spiked at 20 μg/kg (as aniline) Determination (quantification using 4 internal standards). the relative standard deviations within the laboratory are 1.0% to 15% and 0.80% to 14%, respectively; The standard deviations were 5.8% to 19% and 6.1% to 19%, respectively; the repeatability limits were 2 μg/kg to 10 μg/kg and 3 μg/kg to 9 μg/kg, respectively; The limit of detection is 8 μg/kg～31 μg/kg and 9 μg/kg～28 μg/kg, respectively. The 6 laboratories respectively tested the river sediment samples with a spiked concentration of.200 μg/kg (calculated as aniline) and a spiked concentration of 360 μg/kg (calculated as aniline). 6 repeated determinations (using 4 internal standards for quantification) of sand samples with aniline meter). the relative standard deviation in the laboratory is 0.80%～ 15% and 1.2%-11%; the relative standard deviations between laboratories are 6.7%-20% and 7.6%-18%, respectively; the repeatability limits are 26 μg/kg～ 74 μg/kg and 46 μg/kg to 128 μg/kg; reproducibility limits were 93 μg/kg to 269 μg/kg and 170 μg/kg to 500 μg/kg, respectively. For precision data see Table D.1 in Appendix D. 10.2 Correctness 6 laboratories measured the quartz sand samples spiked with concentration of 20 μg/kg,.200 μg/kg, 360 μg/kg (calculated as aniline) respectively (4 kinds of internal standards were used for quantification). The recovery rates of standard additions ranged from 72.0% to 127%, 73.0% to 128%, and 71.4% to 123%, respectively; The final yields were 86.7%±15.5%～109%±24.6%, 89.6%±23.0%～109%±15.2% and 87.2%±20.6%～ 110%±13.7%. Six laboratories measured uniform samples of loam and marine sediments spiked at a concentration of 20 μg/kg (as aniline) (using 4 kinds of internal standard quantification). the recovery rates of the standard additions ranged from 72.5% to 124% and 69.2% to 119%, respectively; the final values of the standard addition recoveries were 85.1%, respectively. ±18.3%～106%±23.8% and 83.8%±14.5%～104%±18.5%. The 6 laboratories respectively tested the river sediment samples with a spiked concentration of.200 μg/kg (calculated as aniline) and a spiked concentration of 360 μg/kg (calculated as aniline). aniline meter) for the determination of sand samples (quantified by using 4 internal standards). the recovery rates of the standard additions ranged from 70.2% to 122% and 72.4% to 72.4%. The final recovery rate of standard addition was 88.6%±25.5%～104%±31.7% and 87.2%±22.5%～108%±19.4%, respectively. For accuracy data see Table D.2 in Appendix D. 11 Quality Assurance and Quality Control 11.1 Blank test At least one laboratory blank should be determined for every 20 samples or batches (less than 20 samples), and the results should be below the method detection limit. 11.2 Calibration A standard curve should be established for each batch of samples, and the correlation coefficient should be greater than or equal to 0.995, otherwise the standard curve should be redrawn. Every 20 samples or each batch (less than 20 samples) should be determined at an intermediate concentration point of the standard curve, and the determination result should be consistent with the standard value. The error is within ±20%, otherwise the standard curve should be redrawn. 11.3 Parallel samples At least one parallel sample is determined for every 20 samples or each batch (less than 20 samples), and the relative deviation of the parallel samples should be within ±35%. 11.4 Blank Marking Every 20 samples or every batch (less than 20 samples) at least one blank spiked sample is determined, and the spiked recovery rate should be 65% to 130% between. 11.5 Matrix spikes For every 20 samples or batches (less than 20 samples) at least one matrix spiked sample is determined, the spiked recovery of soil samples should be within Between 65% and 130%, the spiked recovery of sediment samples should be between 60% and 140%. 12 Waste Disposal The waste liquid generated in the experiment should be collected by classification, stored in a centralized manner, and marked accordingly, and entrust a qualified unit to deal with it according to law.

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